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LABORATOIRE NATIONAL DES CHAMPS MAGNÉTIQUES INTENSESANNUAL REPORT2009


<strong>Laboratoire</strong> <strong>National</strong> <strong>des</strong> <strong>Champs</strong> MagnétiquesInt<strong>en</strong>sesGr<strong>en</strong>oble–ToulouseC<strong>en</strong>tre <strong>National</strong> de la Recherche Sci<strong>en</strong>tifiquehttp://lncmi.cnrs.fr/Annual Report2009LNCMI is formally associated with the “Université Joseph Fourier”, Gr<strong>en</strong>oble, the “UniversitéPaul Sabatier”, Toulouse and the “Institut <strong>National</strong> <strong>des</strong> Sci<strong>en</strong>ces Appliquées”, Toulouse.Editors: Fabi<strong>en</strong>ne Duc, Rachel Graziotti and Duncan Maude


TABLE OF CONTENTSPreface 1Carbon Allotropes 3Investigation of the dynamic alignm<strong>en</strong>t of single walled carbon nanotubes in pulsed high magnetic fields . . 5Charge transport mechanisms in arrays of multi-walled carbon nanotubes . . . . . . . . . . . . . . . . . . 6Propagative Landau states and Fermi level pinning in carbon nanotubes . . . . . . . . . . . . . . . . . . . 7Aharonov-Bohm modulation of the high <strong>en</strong>ergy subbands in carbon nanotubes . . . . . . . . . . . . . . . . 8Edge fingerprints and magneto-conductance in graph<strong>en</strong>e nanoribbons . . . . . . . . . . . . . . . . . . . . 9Using Landau quantization to suppress Auger scattering in graph<strong>en</strong>e . . . . . . . . . . . . . . . . . . . . . 10Observation of the half-integer quantum Hall effect in epitaxial graph<strong>en</strong>e . . . . . . . . . . . . . . . . . . . 11Integer quantum Hall effect in epitaxial graph<strong>en</strong>e . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12Improving graph<strong>en</strong>e’s cleanliness for high field magneto-transport . . . . . . . . . . . . . . . . . . . . . . 13Metal-insulator transition for filling factor ν = −2 to ν = 0 in graph<strong>en</strong>e . . . . . . . . . . . . . . . . . . . 14How perfect can graph<strong>en</strong>e be? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15Effect of a magnetic field on the two-phonon Raman scattering in graph<strong>en</strong>e . . . . . . . . . . . . . . . . . 16Tuning the electron-phonon coupling in graph<strong>en</strong>e with magnetic fields . . . . . . . . . . . . . . . . . . . . 17Thermal conductivity of graph<strong>en</strong>e in Corbino membrane geometry . . . . . . . . . . . . . . . . . . . . . . 18Electric field doping of few-layer graph<strong>en</strong>e . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19Low temperature magneto-transport in natural graphite . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20Magnetotransport to extract the spin gap for charged excitations in graphite . . . . . . . . . . . . . . . . . 21Magneto-transmission spectroscopy of graphite in high magnetic fields . . . . . . . . . . . . . . . . . . . . 22Graphite from the viewpoint of Landau level spectroscopy: An effective graph<strong>en</strong>e bilayer and monolayer . . 23Magneto-transmission of multi-layer epitaxial graph<strong>en</strong>e and bulk graphite: A comparison . . . . . . . . . . 24Two-Dim<strong>en</strong>sional Electron Gas 25The surprisingly fragile quantum Hall ferromagnet at filling factor ν = 1 . . . . . . . . . . . . . . . . . . . 27Dispersive line shape of the resistively detected NMR on either side of filling factor ν = 1 . . . . . . . . . . 28Spin splitting <strong>en</strong>hancem<strong>en</strong>t of fully populated Landau levels . . . . . . . . . . . . . . . . . . . . . . . . . 29Spin polarisation of a disordered GaAs 2D electron gas in a strong in-plane magnetic field . . . . . . . . . 30High-order fractional microwave induced resistance oscillations . . . . . . . . . . . . . . . . . . . . . . . 31Crossover betwe<strong>en</strong> distinct mechanisms of microwave photoconductivity in double quantum wells . . . . . 32Emerg<strong>en</strong>t fractional quantum Hall effect in a triple quantum well . . . . . . . . . . . . . . . . . . . . . . . 33Re<strong>en</strong>trant fractional quantum Hall states in a triple quantum well . . . . . . . . . . . . . . . . . . . . . . . 34Magneto-intersubband oscillations in multilayer electron systems . . . . . . . . . . . . . . . . . . . . . . . 35


Interfer<strong>en</strong>ce of fractional microwave induced resistance oscillations with magneto-intersubband oscillationsin a bilayer system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36Microwave photoconductivity in multilayer systems: triple quantum wells . . . . . . . . . . . . . . . . . . 37Hole cyclotron resonance in a two-dim<strong>en</strong>sional semimetal . . . . . . . . . . . . . . . . . . . . . . . . . . . 38Electron-Phonon Interactions in a single modulation doped Ga 0.24 In 0.76 As/InP Quantum Well . . . . . . . . 39Temperature effect on Coulomb pseudogap in electron tunneling betwe<strong>en</strong> Landau-quantized twodim<strong>en</strong>sionalgases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40Semiconductors and Nanostructures 41On the trigonal field acting at the Cr 3+ ( 2 E states) in Ruby . . . . . . . . . . . . . . . . . . . . . . . . . . 43Mobility spectrum analysis in InN:Mg . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44Cyclotron effective mass measurem<strong>en</strong>ts in Indium Nitride . . . . . . . . . . . . . . . . . . . . . . . . . . . 45Oscillatory magneto-absorption under pressure in Indium Sel<strong>en</strong>ide . . . . . . . . . . . . . . . . . . . . . . 46Magnetoresistance in β-FeSi 2 on n-type Si substrates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47Two-dim<strong>en</strong>sional weak localization in polycrystalline granular SnO 2 films . . . . . . . . . . . . . . . . . . 48Magnetoresistance mobility extraction in FinFET triple gate devices . . . . . . . . . . . . . . . . . . . . . 49Spin polarization of carriers in a GaAs/GaAlAs resonant tunneling diode . . . . . . . . . . . . . . . . . . . 50Spectroscopy and optical manipulation of a single Mn spin in a CdTe-based quantum dot in high magneticfield . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51InP/GaP self-assembled quantum dots under extreme conditions . . . . . . . . . . . . . . . . . . . . . . . 52Metals, Superconductors and Strongly Correlated Systems 53Thermo-electric study of Fermi surface reconstruction in YBa 2 Cu 3 O y . . . . . . . . . . . . . . . . . . . . 55Anomalous criticality in high-T c cuprates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of the superconducting <strong>en</strong>ergy gap in Bi 2 Sr 2 CaCu 2 O 8+δ . . . . . . . . . . . . . 57Magnetoresistance anisotropy and AMRO in the electron doped superconducting cuprate Nd 2−x Ce x CuO 4 . 58Transport measurem<strong>en</strong>ts of H c2 and its anisotropy in FeSe 1−x Te x single crystals . . . . . . . . . . . . . . . 59Coexist<strong>en</strong>ce of magnetic order and superconductivity in iron pnicti<strong>des</strong> . . . . . . . . . . . . . . . . . . . . 60High-field metamagnetism in the antiferromagnet CeRh 2 Si 2 . . . . . . . . . . . . . . . . . . . . . . . . . 61Field Evolution of Coexisting Superconducting and Magnetic Orders in CeCoIn 5 . . . . . . . . . . . . . . 62Fermi surface study of the hidd<strong>en</strong> order state in URu 2 Si 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . 63High field resistivity measurem<strong>en</strong>ts on single crystalline UPt 2 Si 2 . . . . . . . . . . . . . . . . . . . . . . . 64Evolution of the Fermi surface of BaFe 2 (As 1−x P x ) 2 on <strong>en</strong>tering the superconducting dome . . . . . . . . . 65Angular dep<strong>en</strong>d<strong>en</strong>ce of the Nernst effect in elem<strong>en</strong>tal bismuth . . . . . . . . . . . . . . . . . . . . . . . . 66Magnetic field-induced electronic instability in bismuth . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67Magnetic oscillations in a linear chain of comp<strong>en</strong>sated orbits . . . . . . . . . . . . . . . . . . . . . . . . . 68


Coexist<strong>en</strong>ce of closed orbit and quantum interferometer with the same cross section in the organic metalβ”-(BEDT-TTF) 4 (H 3 O)[Fe(C 2 O 4 ) 3 ]·C 6 H 4 Cl 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69Metal-non-metal transition in the charge transfer salt (BEDT-TTF) 8 [Hg 4 Br 12 (C 6 H 5 Br) 2 ] . . . . . . . . . . 70Magnetic torque experim<strong>en</strong>ts on the magnetic-field-induced organic superconductor λ-(BETS) 2 FeCl 4 . . . 71Temperature and magnetic field dep<strong>en</strong>d<strong>en</strong>ce of domain wall width and period of Condon domain structurein Ag . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72Intrinsic diamagnetic l<strong>en</strong>gth scales of Condon domain phase in Be . . . . . . . . . . . . . . . . . . . . . . 73Magnetic Systems 75Y b 3+ → Er 3+ up-conversion luminesc<strong>en</strong>ce under high pressure and pulsed magnetic fields . . . . . . . . . 77Nd 3+ crystal-field studies of weakly doped Nd 1−x Ca x MnO 3 . . . . . . . . . . . . . . . . . . . . . . . . . 78Magnetotransport in a disordered Zn 1-x Mn x GeAs 2 alloy . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79Anomalous Hall effect in (Ge,Mn)Te-(Sn,Mn)Te spin-glasslike crystals . . . . . . . . . . . . . . . . . . . 80High field torque magnetometry on a molecular Dysprosium triangle . . . . . . . . . . . . . . . . . . . . . 81NMR evid<strong>en</strong>ce for long zero-quantum coher<strong>en</strong>ce in antiferromagnetic molecular wheels NaFe 6 and LiFe 6 . 82Nuclear magnetic resonance determination of spin-superlattice structure of magnetization plateaus inSrCu 2 (BO 3 ) 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83Magnetic structure of the half magnetization plateau phase in CdCr 2 O 4 . . . . . . . . . . . . . . . . . . . . 84Structural analysis with pulse-l<strong>en</strong>gth exposures up to 30 Tesla at ID06, ESRF . . . . . . . . . . . . . . . . 85Magnetization at low temperatures and high magnetic fields on LuFe 2 O 4 . . . . . . . . . . . . . . . . . . . 86Enhancem<strong>en</strong>t magnetic mom<strong>en</strong>t in the single phase nanostructure Gd 3 Fe 5 O 12 . . . . . . . . . . . . . . . . 87Effect of the M/Co substitution on magnetocrystalline anisotropy and magnetization in SmCo 5−x M x compounds(M=Ga; Al) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88Investigation of the intrinsic magnetic properties of the ThCo 4 B compound . . . . . . . . . . . . . . . . . 89Magnetic properties of Y 0.7 Er 0.3 Fe 2 (H, D) 4.2 compounds up to 35 T . . . . . . . . . . . . . . . . . . . . 90Field-induced transitions in RECo 0.50 Mn 0.50 O 3 (RE = Dy, Eu) . . . . . . . . . . . . . . . . . . . . . . . . 91High magnetic field study in chromium-based Mn 1−x Cd x Cr 2 S 4 thiospinels . . . . . . . . . . . . . . . . . . 92Magnetic properties of ErCo x Mn 1−x O 3 perovskites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93Ferromagnetic domains in nanosized erbium perovskites . . . . . . . . . . . . . . . . . . . . . . . . . . . 94Biology, Chemistry and Soft Matter 95Concerted spin crossover and symmetry breaking yield three thermally- and one light-induced crystallographicphases of a novel molecular material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97Magnetostructural correlations in Tetrairon(III) single-molecule magnets . . . . . . . . . . . . . . . . . . . 98Applied Superconductivity 99Magnetic field behaviour of ex-situ processed MgB 2 multifilam<strong>en</strong>tary wires . . . . . . . . . . . . . . . . . 101Superconductivity of C and TiC doped multi-filam<strong>en</strong>tary MgB 2 wires . . . . . . . . . . . . . . . . . . . . 102


Phthalocyanine doping to improve critical curr<strong>en</strong>t d<strong>en</strong>sities in MgB 2 tapes . . . . . . . . . . . . . . . . . . 103Critical curr<strong>en</strong>t measurem<strong>en</strong>ts on Bi-2212 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104Magneto-Sci<strong>en</strong>ce 105Changes in the microstructure resulting from a high cooling rate in Fe-xC-Mn alloys in strong magnetic field 107Study of the influ<strong>en</strong>ce of magnetic forces on the mass transfer of paramagnetic particles in electrochemistry 108Large Alfvén Waves in liquid sodium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109Magnetohydrodynamic effect on electrodeposition of nickel alloys-catalysts for hydrog<strong>en</strong> evolution . . . . 110Diffusion behavior of Al/Cu diffusion interface under a high magnetic field . . . . . . . . . . . . . . . . . 111Magnet Developm<strong>en</strong>t and Instrum<strong>en</strong>tation 113High field helix developm<strong>en</strong>t . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115Magnets for neutron and x-ray scattering and absorption experim<strong>en</strong>ts . . . . . . . . . . . . . . . . . . . . . 116A new cooling loop for thermo-hydraulic magnet studies . . . . . . . . . . . . . . . . . . . . . . . . . . . 117Pulsed <strong>en</strong>ergy supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118Pulsed high-field coils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119High str<strong>en</strong>gth conductors for pulsed magnets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120Megagauss magnetic field g<strong>en</strong>eration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121SEISM: A 60 GHz electron cyclotron resonance (ECR) ion source prototype . . . . . . . . . . . . . . . . . 122Towards developing a high T c superconducting magnet . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123Status report of the 42+ Tesla hybrid magnet project . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124Measuring the vacuum magnetic birefring<strong>en</strong>ce . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125Special purpose NMR probe for spectroscopy of quadrupolar nuclei at 30 T . . . . . . . . . . . . . . . . . 126New rotating sample holder for broad-band quasi-optical HF-EPR spectroscopy . . . . . . . . . . . . . . . 127A new magnetometer for use in dc magnetic fields in excess of 28 T. . . . . . . . . . . . . . . . . . . . . . 128Proposals for Magnet Time – Projects Carried Out in 2009 129PhD Theses 2009 141List of Publications 2009 142Contributors of the LNCMI to the Pres<strong>en</strong>t Report 147Collaborating External Laboratories 148


2009PrefaceDear Reader,You have before you the first annual report of the <strong>Laboratoire</strong> <strong>National</strong> <strong>des</strong> <strong>Champs</strong> Magnétiques Int<strong>en</strong>ses (LNCMI),created on the 1st of January 2009 through the merger of the <strong>Laboratoire</strong> <strong>des</strong> <strong>Champs</strong> Magnétiques Int<strong>en</strong>ses (Gr<strong>en</strong>oble)and the <strong>Laboratoire</strong> <strong>National</strong> <strong>des</strong> <strong>Champs</strong> Magnétiques Pulsés (Toulouse). The LNCMI is a “Unité Propre de Recherche”of the C<strong>en</strong>tre <strong>National</strong> de la Recherche Sci<strong>en</strong>tifique (UPR3228) and is part of the Fr<strong>en</strong>ch “Très Grands Equipem<strong>en</strong>ts”.The laboratory is associated with the Université Joseph Fourier de Gr<strong>en</strong>oble, the Université Paul Sabatier de Toulouseand the Institut <strong>National</strong> <strong>des</strong> Sci<strong>en</strong>ces Appliquées de Toulouse. Its activities are also supported by the EC FP7 “Largeinfrastructures” program, where it is the coordinator of the EuroMagNET2 Integrating Activity.This report int<strong>en</strong>ds to provide a complete overview of the in-house and collaborative sci<strong>en</strong>tific and technical activities in2009 of the LNCMI.The 24MW power supply of the Gr<strong>en</strong>oble site, dedicated to the g<strong>en</strong>eration of static fields, allows either to operate simultaneouslytwo resistive 10MW magnets or to operate one 24 MW magnet. The highest field g<strong>en</strong>erated at the LNCMI-G is35 T in a 34 mm bore diameter. A hybrid magnet, capable of g<strong>en</strong>erating 43 T is curr<strong>en</strong>tly under construction.The 14 MJ capacitor bank g<strong>en</strong>erator of the Toulouse site, dedicated to the g<strong>en</strong>eration of pulsed fields, allows to g<strong>en</strong>eratefields up to 80 T. An installation to g<strong>en</strong>erate <strong>des</strong>tructive pulsed fields up to 300 T is nearing its completion.This report and the list of publications show the importance and the interest of results obtained in magnetic fields, eitheron the basis of in-house research or as a result of a close collaboration with several research groups from many differ<strong>en</strong>tcountries.In addition, the LNCMI is proud to contribute to the training of young sci<strong>en</strong>tists by giving them the opportunity to preparetheir thesis work and/or to participate to European research activities.Finally, a word of thanks to the sci<strong>en</strong>tific, technical and administrative staff of the laboratory (altogether 90 people),our post docs and PhD stud<strong>en</strong>ts (almost 30) and the numerous visitors (over 200 this year) for their contributions to theimprovem<strong>en</strong>t of the installation and for the quality of their work.Geert Rikk<strong>en</strong>December 20091


2009Carbon Allotropes3


2009 CARBON ALLOTROPESInvestigation of the dynamic alignm<strong>en</strong>t of single walled carbon nanotubesin high pulsed magnetic fieldsThe differ<strong>en</strong>t carbon allotropes have attracted r<strong>en</strong>ewed att<strong>en</strong>tionin rec<strong>en</strong>t years with the successful fabrication of thelower dim<strong>en</strong>sional forms of graphite e.g. fuller<strong>en</strong>es, carbonnanotubes, graph<strong>en</strong>e and graph<strong>en</strong>e nano-ribbons. Carbonnanotubes are unique nano-objects with highly anisotropicelectrical, magnetic and optical properties. Over the lastfew years our understanding of the physics of carbon nanotubeshas made considerable progress and the detailedcompreh<strong>en</strong>sion of the complex physical properties of carbonnanotubes has significantly increased. Dep<strong>en</strong>ding onthe diameter, and the helical arrangem<strong>en</strong>t of the hexagonallyarranged carbon atoms, carbon nanotubes can be eithermetallic or semiconducting.In this work we have investigated the magnetic propertiesof single walled carbon nanotubes. Semiconducting nanotubesare diamagnetic both along and perp<strong>en</strong>dicular totheir long axis, however, the magnitude of the perp<strong>en</strong>dicularsusceptibility is higher. Metallic nanotubes are paramagneticalong their long axis and diamagnetic perp<strong>en</strong>dicularto it. This constrains both types of single walled carbonnanotubes to align parallel to a magnetic field. The samplesinvestigated here are composed of individually susp<strong>en</strong>dedsingle walled carbon nanotubes in an aqueous solution. Theaim is to study the dynamic alignm<strong>en</strong>t of the single walledcarbon nanotubes during the application of a pulsed magneticfields via the absorption of polarized light.differ<strong>en</strong>ce betwe<strong>en</strong> the measured and the simulated l<strong>en</strong>gthdistribution.Further measurem<strong>en</strong>ts with l<strong>en</strong>gth sorted samples are beingundertak<strong>en</strong>. The ultimate aim is to id<strong>en</strong>tify the role ofthe single walled carbon nanotubes in the dynamic processand determine the influ<strong>en</strong>ce of the chirality on the magneticanisotropy.Figure 1: The time and field dep<strong>en</strong>d<strong>en</strong>t alignm<strong>en</strong>t of a carbonnanotubes susp<strong>en</strong>ded in aqueous solution.To measure the alignm<strong>en</strong>t of single walled carbon nanotubeswe make use of the fact that nanotubes absorb lightonly if it is polarized parallel to the axis of the nanotube.We thus refer to linear dichroism spectroscopy: The absorptionratio betwe<strong>en</strong> light polarized parallel and perp<strong>en</strong>dicularto the applied magnetic field directly reflects the degree ofalignm<strong>en</strong>t of the <strong>en</strong>semble on nanotubes under the influ<strong>en</strong>ceof this magnetic field. Measuring the integrated absorptionspectra of a white light source at differ<strong>en</strong>t times during themagnetic field pulse allows us to determine the time dep<strong>en</strong>d<strong>en</strong>talignm<strong>en</strong>t of the single walled carbon nanotubes(figure 1).Our data can be understood with the aid of a theoreticalmodel based on rotational diffusion of rigid rods [Shaveret al., ACS Nano 3,1 131 (2009)]. A typical result of thesimulation is shown in figure 2. The l<strong>en</strong>gth distribution ofthe single walled carbon nanotubes in the sample was determinedusing an atomic force microscope. The simulationwhich best <strong>des</strong>cribes our experim<strong>en</strong>tal data shows a slightFigure 2: Time dep<strong>en</strong>d<strong>en</strong>t alignm<strong>en</strong>t and best match fit (red).Insert: The matching l<strong>en</strong>gth distribution (red) is larger than themeasured distribution (blue).N. Ubrig, S. George, O. PortugallJ. Kono, M. Pasquali (Rice University)5


CARBON ALLOTROPES 2009Charge transport mechanisms in arrays of multi-walled carbon nanotubesUnlike the case of individual nano-objects, in these arraysthe inter-tube barriers and defects play an ess<strong>en</strong>tial role inthe electrical transport properties of the carbon nanotubesarrays. In this work, we demonstrate the role of the surfacedefects of the nano tube by its spins. In thin layersof multi-walled carbon nanotubes (MWCNT) the variationof the resistance as a function of temperature range [4-60K] follows a Mott’s law of two dim<strong>en</strong>sional (2D) VariableRange Hopping (VRH). Figure 3(a) shows the relative magnetoresistance(MR), ∆R/R 0 , in the temperature range inwhich the VRH is observed.where Ω B = 4DeBh≪ 1/τ ϕ , τ ϕ being the phase coher<strong>en</strong>cetime, and ψ the digamma function. The obtained curvesfollows the 2D WL model, which demonstrates the role ofthe surface defects of the nano tubes by its spins.The minimum position of negative magneto-resistance(NMR) shifts to higher fields as the temperature rises. Bothlow-field NMR due to changing of phase betwe<strong>en</strong> alternatehopping paths <strong>en</strong>closing a magnetic flux (quantum interfer<strong>en</strong>ce)and high-field positive magneto-resistance (PMR)due to electronic orbit shrinkage are predicted for systemswith hopping conductivity mechanism; ie MR = NMP +PMR. In this model, the amplitude of the NMR declinesas the temperature is rising. However, in our samples, acontrario, the NMR amplitude increases as the temperatureincreases in the temperature range in which VRH canbe responsible of the charge transport mechanism. Fromthe other side negative MR is inher<strong>en</strong>t for the systemswhere conductivity can be <strong>des</strong>cribed in the frame of weaklocalisation(WL) theory [Lee and Ramakrishnan, Rev.Mod. Phys. 57, 287 (1985)]. Therefore, we made the assumptionthat MR data are the sum of the positive and negativecontribution due to MR effects in the VRH and WLregimes, respectively. We find that high-field positive partof MR can be approximated in frame of Kamimura modelfor spin-dep<strong>en</strong>d<strong>en</strong>t VRH conductivity (due to the surfacedefects of the nano tubes) [Modern problems in cond<strong>en</strong>sedmatter sci<strong>en</strong>ces Chap. 7, Vol. 10, Efros A.L. & Pollak M.ed., North Holland 1985]:∆GG = −A KKHKK 2 − (1)H2where H KK is the characteristic field for spin alignm<strong>en</strong>t,A KK the saturation value of the magneto-conductance. Usingthis formula and values of parameters H KK and A KK obtainedfrom the approximation data of high field MR data,we calculated the positive magneto-conductance for lowfieldregion (figure 3(b)).H 2The pure negative contribution to MR according our assumptionis calculated by subtracting positive MR from theexperim<strong>en</strong>tal data and shown in figure 3(c). These data canbe fitted reasonably well by the equation for 2D WL:∆G = e2Πh α[Ψ(1 2 + 1Ω B τ ϕ+ ln(Ω B τ ϕ )] (2)Figure 3: (a) Relative magnetoresistance in the temperaturerange in which 2D VRH is observed. (b) Kamimura’s model forPMR (spin dep<strong>en</strong>d<strong>en</strong>t VRH). (c) NMR obtained by subtraction ofthe calculated PMR from the experim<strong>en</strong>tal results.T.A. Dauzh<strong>en</strong>ka, J. GalibertV.K. Ks<strong>en</strong>evich (Belarus State University, Dept Phys. SC & nanoelectronics, BY-Minsk), D. Seliuta (SC Institute LI-Vilnius), V.A. Samuilov (Garcia c<strong>en</strong>ter Polymers at Engineered Interfaces, Stony Brook Univ. NY)6


2009 CARBON ALLOTROPESPropagative Landau states and Fermi level pinning in carbon nanotubesCarbon nanotubes (CNT), isolated graph<strong>en</strong>e sheets andgraph<strong>en</strong>e nano-ribbons (GNR) have revealed remarkableelectronic properties. The massless dispersion bands atthe charge neutrality point (CNP) drive spectacular ph<strong>en</strong>om<strong>en</strong>alike an anomalously low backscattering and relatedlong mean free path in metallic nanotubes, or thehuge charge carriers mobility in graph<strong>en</strong>e layers. CNTand GNR also have in common a large magnetic field dep<strong>en</strong>d<strong>en</strong>ceof their 1-D subbands. In graph<strong>en</strong>e, the highmagnetic field behavior of Dirac fermions has be<strong>en</strong> shownto induce an half-integer quantum Hall effect. In singleand multi-walled carbon nanotubes (MWCNT), whileAharonov-Bohm ph<strong>en</strong>om<strong>en</strong>a were investigated in-depth foraxial magnetic fields, the exploration of Landau states inpres<strong>en</strong>ce of high transversal magnetic fields has be<strong>en</strong> facingoverwhelming technical chall<strong>en</strong>ges. On the theoreticalside, a drastic change of the 1-D dispersion bands hasbe<strong>en</strong> predicted once the cyclotron radius equals the tuberadius. The calculations show that the resulting magneticbands remain dispersive along the tube axis at large k wavevectorssuggesting an inhomog<strong>en</strong>eous chiral curr<strong>en</strong>t flowingat the flanks of the tube. At low k-vectors, a Landau levelsspectrum is derived with the √ nB magneto-fingerprintof graph<strong>en</strong>e, whatever the CNT chirality. Notwithstanding,an experim<strong>en</strong>tal spectroscopy of Landau states in CNTshas not yet be<strong>en</strong> achieved and the longitudinal magnetoconductancein the quantum regime remains unexplored.In this work, MWCNTs of diameters in the range of 10 nmto 20 nm are selected to reach the high magnetic fieldregime under 60 T, corresponding to a dim<strong>en</strong>sionless parameterν = r/l B larger than 1 (r is the tube’s radius andl B = √ /eB, the magnetic l<strong>en</strong>gth). In the following, wefocus on two MWCNTs whose external shells, mainly contributingto the conductance, have be<strong>en</strong> id<strong>en</strong>tified respectively,as behaving as semiconducting and metallic shells,in the light of their Aharonov-Bohm magneto-fingerprints[Nanot et al., C. R. Physique 10, 268 (2009)].The contribution of propagative Landau states to magnetotransportin semiconducting and metallic MWCNTshells is experim<strong>en</strong>tally unveiled [Nanot et al., submitted].For semiconducting shells, the occurr<strong>en</strong>ce of a zero<strong>en</strong>ergyLandau state associated with the <strong>en</strong>ergy gap closureis found to g<strong>en</strong>erate strongly delocalized states closeto the Dirac point, <strong>des</strong>pite the pres<strong>en</strong>ce of disorder andlow dim<strong>en</strong>sionality, and irrespective of the electrostaticdoping str<strong>en</strong>gth. For doped metallic shells, the magnetoconductancealso exhibits an upshift of the massive 1Dbandsin agreem<strong>en</strong>t with the formation of Landau states.At the CNP, the re-introduction of the backscattering inthe metallic bands, clearly evid<strong>en</strong>ces the onset of the zero<strong>en</strong>ergyLandau state (figure 4). Ev<strong>en</strong> more spectacular isthe pinning of the Fermi level at the CNP in high field(figure 5). These remarkable features are supported byLandauer-Büttiker simulations of the magnetoconductanceof weakly disordered semiconducting and metallic CNTs.Figure 4: High magnetic field perp<strong>en</strong>dicular magneto-conductanceobtained at 100 K on a individually connected MWCNT forvarious Fermi <strong>en</strong>ergies. The drastic decrease of the conductanceabove 25 T results from the re-introduction of the back-scatteringalong with the onset of the first Landau level at zero <strong>en</strong>ergy.Figure 5: Landauer-Büttiker simulation of the perp<strong>en</strong>dicularmagneto-conductance on a (10,10) NTC in pres<strong>en</strong>ce of weak disorderfor various magnetic field dep<strong>en</strong>d<strong>en</strong>t electrostatic pot<strong>en</strong>tials.The mag<strong>en</strong>ta curve with cross marks is the calculated magneto–conductance at a fixed Fermi <strong>en</strong>ergy. In inset, the magnetic fielddep<strong>en</strong>d<strong>en</strong>ce of the electrostatic pot<strong>en</strong>tial illustrating the so calledpinning of the Fermi <strong>en</strong>ergy at the charge neutrality point.S. Nanot, W. Escoffier, J-M Broto, B. Raquet,S. Roche, R. Avriller (Commissariat à l’Energie Atomique, INAC, SP2M, Gr<strong>en</strong>oble)7


CARBON ALLOTROPES 2009Aharonov-Bohm modulation of the high <strong>en</strong>ergy subbands in carbon nanotubesIn this work, we demonstrate the usefulness of combiningthe nano-probing of individual carbon nanotubes and verylarge magnetic fields. We show that the magneto-fingerprintin the conductance under a parallel magnetic field is an unequivocalsignature of a metallic or a semiconducting behaviorof the external shell from which the locations of thediffer<strong>en</strong>t 1-D subbands are deduced.Under 60 T threading the carbon nanotube along its axis,the electronic d<strong>en</strong>sity of states undergoes quantum-fluxmodulations yielding to a giant Aharonov-Bohm oscillationof the conductance, orders of magnitude larger thanthe standard Aharonov-Bohm effect in metallic rings orcylinders. Here, we study the sub-bands modulation bythe Aharonov-Bohm flux within a large diameter MWCNT(d = 18 nm) with a distance L T = 150 nm betwe<strong>en</strong> contacts(atomic force microscope (AFM) observation). Inthis case, we expect to observe more than 3 modulationperiods within 55 T. Meanwhile, a thin oxide thickness(t ox = 40 nm) is used to <strong>en</strong>hance the gate effici<strong>en</strong>cy and allowshigher doped regime. As shown in figure 6, the pulsedfield magneto-conductance exhibits three periods and a π-dephasing of the modulation wh<strong>en</strong> changing the gate voltage.The period of 17 T corresponds to a quantum fluxthreading a 17.3 nm diameter cylinder, in consist<strong>en</strong>ce withthe AFM estimation.Figure 6: Left: Experim<strong>en</strong>tal magneto-conductance measuredon an 18 nm diameter MWCNT (AFM estimate) at 100 K, for variousback-gate voltages. Curves are shifted for clarity. Right: Calculationof the magneto-conductance for a (219,0) nanotube withdiffer<strong>en</strong>t locations of the Fermi <strong>en</strong>ergies. Comparison betwe<strong>en</strong> theexperim<strong>en</strong>tal and calculated curves yields a direct assignm<strong>en</strong>t ofthe locations of the CNP and the vHs.The data are directly compared to the conductance calculationfor a metallic (219,0) nanotube in the frame of theLandauer-Buttiker formalism (figure 6) at 100 K. We assumea ballistic regime and, for a first qualitative approach,Schottky barriers are neglected. Without any fitting parameter,the agreem<strong>en</strong>t betwe<strong>en</strong> the experim<strong>en</strong>tal curves andthe modelling based on the band structure modulation, ev<strong>en</strong>in the highly doped states where several bands are carryingthe curr<strong>en</strong>t, is convincing. Wh<strong>en</strong> changing the gate voltagefrom +10 to −10 V, successive weak<strong>en</strong>ing and π-phasechange of the magneto-conductance are experim<strong>en</strong>tally observed.Interestingly, the holes and electrons <strong>en</strong>ergies canbe deduced at any gate voltage without any analytical estimationby directly comparing the (magnetic) phase andrelative amplitude of the effect to the calculated curves. Infact, while the magnetic flux induces successive gap op<strong>en</strong>ingand closing, sub-bands at higher <strong>en</strong>ergies are split andshifted to lower (E − i )(or higher, E + i ) <strong>en</strong>ergies dep<strong>en</strong>dingon their clockwise (respectively counter-clockwise) movem<strong>en</strong>twith respect to the applied magnetic field. As a consequ<strong>en</strong>ce,at a giv<strong>en</strong> <strong>en</strong>ergy, the number of sub-bands carryingthe curr<strong>en</strong>t is modulated. Wh<strong>en</strong> the Fermi <strong>en</strong>ergy isbetwe<strong>en</strong> the CNP and E 1 /2 (0 and 35 meV in our case, redcurves figure 6), the number of sub-bands passes from 2 to0 during the first half-period and th<strong>en</strong> rises back to 2 duringthe second half-period. The magneto-conductance is firstlynegative and th<strong>en</strong> positive. At the same time, the magnitudeof the oscillations decreases as the Fermi <strong>en</strong>ergy increases,and vanishes at E F = E 1 /2 where the number of sub-bandsis magnetic field indep<strong>en</strong>d<strong>en</strong>t (gre<strong>en</strong> and cyan curves). Betwe<strong>en</strong>E 1 /2 and E 1 (35 and 70 meV, black curve), the firstvan Hove singularity splitting to lower <strong>en</strong>ergies induces firstan increase of the number of sub-bands from 2 to 4 beforeΦ 0 /2 and th<strong>en</strong> returns to 2 betwe<strong>en</strong> Φ 0 /2 and Φ 0 . Thiscorresponds to a π-dephasing compared to the magnetoconductanceat low <strong>en</strong>ergies. A new vanishing, followed bya new dephasing, is consist<strong>en</strong>tly observed wh<strong>en</strong> the Fermi<strong>en</strong>ergy reaches and goes beyond the first vHs at E 1 (mag<strong>en</strong>taand blue curves).Finally, we conclude that the magneto-fingerprints of theAharonov-Bohm effect is an unique tool to both id<strong>en</strong>tify themetallic or semiconducting behavior of the external shelland to assign the location of its charge neutrality point andthe van Hove singularities.S. Nanot, W. Escoffier, J-M Broto, B. Raquet,A. Magrez, L. Forro ()8


2009 CARBON ALLOTROPESEdge fingerprints and magneto-conductance in graph<strong>en</strong>e nanoribbonsThe control of the curr<strong>en</strong>t flow in gated graph<strong>en</strong>e nanoribbons(GNR) constitutes a fascinating chall<strong>en</strong>ge for the futureof carbon-based electronic devices. The combinationof the extraordinary electronic properties of the Diracfermions in graph<strong>en</strong>e, like their outstanding mobility atroom temperature, with a sizeable <strong>en</strong>ergy gap, op<strong>en</strong>s a routeto outperform the ultimate scaling of silicon field effecttransistors [Wang et al, Phys. Rev. Lett. 100 206803(2008)]. However, the lateral confinem<strong>en</strong>t goes along witha problematic decay of the mobility. Low temperaturetransport measurem<strong>en</strong>ts performed on nano-lithographedGNR also unveil a ubiquitous <strong>en</strong>ergy gap, irrespective ofthe edges ori<strong>en</strong>tation and exceeding the expected confinem<strong>en</strong>tgap.Drawing a parallel betwe<strong>en</strong> GNR and carbon nanotubes(CNT) is certainly tempting. The pres<strong>en</strong>ce of edges in GNRimposes Dirichlet boundary conditions and results in a lossof one conducting channel at the Charge Neutrality Point(CNP), compared to armchair CNT.obtained on high quality GNR is sorely lacking. Applyinga large transverse magnetic field is also a suitable tool toboth explore the expected 1D-electronic band structure andthe disorder induced localization.In this work, we pres<strong>en</strong>t evid<strong>en</strong>ce of 1D-subbands signatureson the electronic transport on an 11 nm wide GNR.Comparison to band structures calculations of a set ofGNRs in a width window of 11±0.3 nm allows an assignationof the carbon atoms arrangem<strong>en</strong>t at the edges and th<strong>en</strong>umber of dimers (figure 7).The application of a 60 T perp<strong>en</strong>dicular magnetic field inducesa drastic increase of the conductance, whose magnitudedep<strong>en</strong>ds on the doping level (figure 8(left). At zero<strong>en</strong>ergy, we demonstrate that the large positive magnetoconductanceoriginates from the onset of the first Landaustate accompanying the closing of the <strong>en</strong>ergy gap (figure8(right). Landauer-Buttiker simulations of the conductanceof GNR including bulk and edge disorder (and curr<strong>en</strong>tlyin progress) demonstrate that the magnetoconductanceresults from a subtle combination of magnetic bandformations and quantum interfer<strong>en</strong>ce effects in pres<strong>en</strong>ce ofdisorder.Figure 7: Conductance versus back-gate voltage at 80 K measuredon the 11 nm wide GNR for two V bias , 50 mV and 1 mV(respectively red and blue curve). Superimposed is the calculatedd<strong>en</strong>sity of states (black curve) as a function of V g , for four distinctGNRs : (a,b,c) aGNR, N = 90,91,92 and (d) zGNR, N = 52.Non-perfect edges are also source of short range pot<strong>en</strong>tialdisorder responsible for inter-valley backscattering. Drasticconsequ<strong>en</strong>ces on the electronic transport have be<strong>en</strong> theoreticalanticipated with the formation of a mobility gap at zero<strong>en</strong>ergy, ev<strong>en</strong> in the pres<strong>en</strong>ce of an ultra-smooth edge roughness.However, a direct comparison with experim<strong>en</strong>tal dataFigure 8: (Left) Magnetoconductance measured on the 11 nmwide GNR for various back gate voltages at 80 K. For comparison,the black dashed curve is the magnetoconductance measuredon a 90 nm GNR varying from 0.6 to 0.4G 0 under 55 T. (Right)Magnetoconductance at the CNP measured at 80,50 and 20 K.The black dashed curves are the simulated magnetoconductanceassuming a thermally activated regime and a magnetic field inducedclosing of the <strong>en</strong>ergy gap along with the onset of the firstLandau level at zero <strong>en</strong>ergy.J-M Poumirol, W. Escoffier, M. Goiran, J-M Broto, B. RaquetS. Roche, A. Cresti (Commissariat à l’Energie Atomique, INAC, SP2M, Gr<strong>en</strong>oble), X. Wang, H. Dai (Physics departm<strong>en</strong>tand Chemistry Laboratory, Stanford, US)9


CARBON ALLOTROPES 2009Using Landau quantization to suppress Auger scattering in graph<strong>en</strong>eCarrier-carrier scattering due to the Coulomb interactionis the dominant process which governs the dynamics ofhot carriers in solids at very short time scales. Thisis true for conv<strong>en</strong>tional (semiconductor) two-dim<strong>en</strong>sionalsystems, ev<strong>en</strong> wh<strong>en</strong> their <strong>en</strong>ergy bands are quantized intodiscrete Landau levels by the application of a magneticfield. This is because Auger-type scattering processes betwe<strong>en</strong>equidistant Landau levels, formed from bands withparabolic dispersions, are extremely effici<strong>en</strong>t. Indeed,Auger scattering has long be<strong>en</strong> considered as the main obstaclefor the fabrication of tunable far-infrared laser basedon inter-Landau level emission. However, the application ofa magnetic field should considerably influ<strong>en</strong>ce the electronelectronscattering process in strongly non parabolic electronicsystems such as graph<strong>en</strong>e.Here we investigate the dynamics of the non-equilibriumcarriers in graph<strong>en</strong>e measured using a deg<strong>en</strong>erate pumpprobetechnique which directly probes the occupancy ofstates well above the Fermi level. The differ<strong>en</strong>tial transmission∆T /T as a function of delay betwe<strong>en</strong> the pumpand probe pulses, is pres<strong>en</strong>ted in figure 9(a-d) for magneticfields in the range 0 − 6 T. Two characteristic relaxationtimes are observed, a fast process (∼ 50 fs) which broad<strong>en</strong>sthe photo-created distribution and a slower process (∼ 4 ps)due to thermalization. At low temperature (T = 18 K), themagnetic field has a considerable influ<strong>en</strong>ce on both the fastand slow relaxation processes.This can be se<strong>en</strong> more clearly in figure 10 which plotsln(∆T /T ) versus delay time to highlight the expon<strong>en</strong>tialcharacter of the relaxation. The characteristic time of thedecay (τ r ) can be extracted from the slope of such a plot.For the slow relaxation at zero magnetic field there is littlediffer<strong>en</strong>ce betwe<strong>en</strong> the high and low temperature datawith a relaxation time of τ r ∼ 4 ps at both 18 K and 250 K.The relaxation becomes slower by a factor of 3–4, changingfrom τ r ∼ 4 ps at B = 0 T to τ r ∼ 12–14 ps for magneticfields above 3 T. For the fast decay, without magnetic fieldthere is little differ<strong>en</strong>ce betwe<strong>en</strong> the high and low temperaturedata with a relaxation time of τ r ∼ 55 fs at 18 K andτ r ∼ 70 fs at 250 K. However, at low temperatures, the applicationof a mo<strong>des</strong>t magnetic field ∼ 3–6 T doubles therelaxation time to τ r ∼ 110 fs, providing direct experim<strong>en</strong>talevid<strong>en</strong>ce that the electron-electron scattering is significantlyless effective in the pres<strong>en</strong>ce of Landau quantization.This slow down, which is common for both the slowand fast relaxation processes, can be se<strong>en</strong> as a proof that inboth cases the electron–electron scattering or thermalizationof the hot plasma with the cold electrons is reduced inthe pres<strong>en</strong>ce of Landau quantization which limits the possible<strong>en</strong>ergy of the initial and final states.This is interpreted as a reduction of electron-electron(Auger) scattering due to the unusual Landau quantizationof Dirac fermions in graph<strong>en</strong>e. Our measurem<strong>en</strong>ts, whichprobe Landau levels with a high index (n ≈ 100), suggestthat for lower Landau levels, Auger processes may be completelysuppressed. This makes graph<strong>en</strong>e a promising systemfor the implem<strong>en</strong>tation of the long ago proposed tunablefar infrared Landau level laser [Plochocka et al. Phys.Rev. B 80, 245415 (2009)].Figure 9: The differ<strong>en</strong>tial transmission ∆T /T as a function of thedelay betwe<strong>en</strong> the pump and probe pulses measured at a temperatureof (a-b) 250 K and (c-d) 18 K for magnetic fields in the range0 − 6 T.Figure 10: (a-b) Natural log of the differ<strong>en</strong>tial transmission as afunction of a delay betwe<strong>en</strong> pump and probe pulses measured formagnetic fields (0 − 6 T) at 18K. The B = 0 T data measured at250 K is plotted using op<strong>en</strong> circles. The relaxation times τ r extractedfrom linear fits are indicated. The inset of (a) shows thecalculated <strong>en</strong>ergy mismatch for Auger processes for carriers in th<strong>en</strong> = 10 and n = 100 Landau level versus change in Landau levelindex mP. Plochocka, P. Kossacki, M. PotemskiA. Golnik, T. Kazimierczuk (Institute of Experim<strong>en</strong>tal Physics, University of Warsaw), C. Berger, W. A. de Heer (GeorgiaTech., Atlanta, USA)10


2009 CARBON ALLOTROPESObservation of the half-integer quantum Hall effect in epitaxial graph<strong>en</strong>eGraph<strong>en</strong>e, a monolayer of sp 2 -bond carbon atoms, has rec<strong>en</strong>tlyattracted considerable interest due to its extraordinaryelectronic properties such as high charge carrier mobilitiesand a novel quantum Hall signature. These properties,that were first observed in exfoliated graph<strong>en</strong>e, are adirect consequ<strong>en</strong>ce of: (i) the linear band structure and (ii)the pseudo-spin, arising from the two sub-lattices. However,we use an epitaxial process to grow graph<strong>en</strong>e monolayerson the Si-face of a semi-insulating silicon carbi<strong>des</strong>ubstrate. The epitaxy and the sample fabrication is <strong>des</strong>cribedin [Emtsev et al. Nature Materials 8, 203 (2009)].As we can grow epitaxial graph<strong>en</strong>e with a high and reproduciblequality (transport properties vary only about30% from sample to sample [figure 11(a) and (b)]) wewant to address an important question; are the quasirelativisticproperties of free-standing graph<strong>en</strong>e also pres<strong>en</strong>tin graph<strong>en</strong>e on SiC? Theory predicts distinct magnetotransportproperties for monolayer, bi-layer and multi-layergraph<strong>en</strong>e that are nicely reproduced in exfoliated samples.In order to clarify if these predictions also hold for epitaxialgraph<strong>en</strong>e, we have measured magneto-transport up to 28 Tin two differ<strong>en</strong>t systems.The as prepared Hall bars show Shubnikov-de Haas (SdH)oscillations in the resistance R xx and emerging plateausin the Hall resistance R xy [see figure 12(a)]. The valuesof these plateaus, that are precursors to the quantumHall effect (QHE), follow the scheme of monolayergraph<strong>en</strong>e: R xy = e 2 /((4n + 2)h) where n is an integer. Ifthe SdH extrema n are plotted against the inverse field1/B a linear dep<strong>en</strong>d<strong>en</strong>ce can be recognized [see inset infigure 12(b)]. The axis intercepts of 0 (1/2) for minima(maxima) yield a Berry phase of π as predicted for singlelayer graph<strong>en</strong>e and confirmed in exfoliated samples.To probe the most interesting point of the band structure,the charge neutrality point, we evaporated ≈ 5 Å oftetrafluorotetracyanoquinodimethane (F4-TCNQ). This resultsin a reduced carrier d<strong>en</strong>sity of n ≈ 5 × 10 11 cm −2 . Insuch a sample the half-integer QHE is visible [figure 12(b)].An evaluation of the SdH oscillations (barely visible below4 T) with the above m<strong>en</strong>tioned procedure further confirmsthe picture of unperturbed graph<strong>en</strong>e.We conclude that the close contact to the SiC substrate doesnot change the magneto-transport properties noticeable andepitaxial graph<strong>en</strong>e reproduces the unique features observedin exfoliated graph<strong>en</strong>e, while remaining a system which iscertainly more suitable for large scale production.Figure 11: (a) Histograms of the charge carrier d<strong>en</strong>sity n, and (b)mobility µ, of samples with differ<strong>en</strong>t geometries and sizes from5 mm to 400 nm. Some Hall bars are patterned on atomicallyflat terraces of the SiC substrate and therefore consist of perfectmonolayer graph<strong>en</strong>e. (c) The step edges are clearly visible in theelectron micrograph.Figure 12: (a) R xx and R xy in a Hall bar on a single substrate terrace[cf. figure 11(c)]. SdH oscillations and plateaus in the Hallresistance are clearly visible. (b) The same quantities in a samplegated close to charge neutrality with F4-TCNQ. Half-integerQHE is visible above 7 T. The inset shows the evaluation of theSdH oscillations [op<strong>en</strong> (closed) symbols: minima (maxima)]. Thelines are best fits to the data [black: Hall bar on a single substrateterrace, red: Hall bar covering several substrat terraces,blue: F4-TCNQ covered (plotted against 0.1/B for clarity)] thatyield a Berry phase of π as expected for monolayer graph<strong>en</strong>e.D.K. MaudeJ. Jobst, D. Waldmann, H.B. Weber (Applied Physics Departm<strong>en</strong>t, University of Erlang<strong>en</strong>-Nürnberg)11


CARBON ALLOTROPES 2009Integer quantum Hall effect in epitaxial graph<strong>en</strong>eIn graph<strong>en</strong>e, a single sheet of hexagonally arranged carbonatoms, electrons behave as Dirac fermions while stillexhibiting the quantum Hall effect wh<strong>en</strong> subjected to a normalmagnetic field. Epitaxial graph<strong>en</strong>e grown on SiC showsmost of the properties of single layer graph<strong>en</strong>e (e.g. Landaulevel quantization), nevertheless, the quantum Hall effectremains elusive in this material. Very rec<strong>en</strong>tly, the productionof high mobility (∼20 000 cm 2 /Vs) single-layergraph<strong>en</strong>e on the C-face of SiC single crystalline wafershas <strong>en</strong>able the observation of quantum Hall plateaus atthe predicted values for graph<strong>en</strong>e ( σ xy = νe 2 /h, with ν =4(N + 1/2) where N is the Landau level index, unambiguouslydemonstrating the graph<strong>en</strong>e like nature of epitaxialgraph<strong>en</strong>e [Wu et al. Appl. Phys. Lett. 95, 223108 (2009)].single terrace) or over steps, to investigate the influ<strong>en</strong>ce ofsubstrate and defects on well-characterized samples. Conversely,these studies will bring insights on the pot<strong>en</strong>tialof epitaxial graph<strong>en</strong>e as a scalable platform for graph<strong>en</strong>ebasedelectronics, with pot<strong>en</strong>tial applications in metrologyat room temperature.In this work, we ext<strong>en</strong>d this observation to magnetic fieldsup to 32 T where we observe the quantum Hall effect atfilling factor 1. This quantum Hall state is shown to be particularrobust against temperature in the epitaxial graph<strong>en</strong>esamples investigated here.In figure 13, the ν = 1 quantum Hall effect can be id<strong>en</strong>tifiedby a true zero-resistance state in the longitudinal resistivityρ xx . At the lowest temperatures a minimum is se<strong>en</strong> in ρ xxaround B ∼ 7.3T, probably related to the emerg<strong>en</strong>ce of a gapat ν = 4. In this temperature range, ρ xx also exhibits sharpreproducible features coexisting with the quantum Hall effect,which are t<strong>en</strong>tatively assigned to mesoscopic effects.Due to the spin and pseudo-spin degrees of freedom of electronsin graph<strong>en</strong>e, the Landau levels are four-fold deg<strong>en</strong>erateand the quantum Hall effect is thus observed for fillingfactors ν = 4(N + 1/2) (where N is the Landau level index)wh<strong>en</strong> this deg<strong>en</strong>eracy is not lifted. The origin (spinor pseudo-spin) of the observed ν =1 (and ν =4) quantumHall states is curr<strong>en</strong>tly the subject of debate [Z. Jiang et al.Phys. Rev. Lett. 99, 106802 (2007)].The temperature robustness of the quantum Hall effect observedin exfoliated graph<strong>en</strong>e [K. S. Novoselov et al. Sci<strong>en</strong>ce315, 1379 (2007)] is also pres<strong>en</strong>t in epitaxial graph<strong>en</strong>e.In figure 14, the longitudinal R xx and Hall resistance R xy areplotted as a function of the magnetic field. The R xy quantizationat ν = 2 persists spectacularly up to room temperature.This behaviour, which primarily emanates from thevery large value of the cyclotron gap in graph<strong>en</strong>e, also reflectsthe weak temperature dep<strong>en</strong>dance of the Landau levelbroad<strong>en</strong>ing.The observation of the quantum Hall effect in epitaxialgraph<strong>en</strong>e op<strong>en</strong>s new av<strong>en</strong>ues for graph<strong>en</strong>e physics: epitaxialgraph<strong>en</strong>e for the first time offers the possibility to studygraph<strong>en</strong>e layers on a atomically flat surface (device on aFigure 13: Longitudinale magnetoresistivity at T ∼ 20mK temperature.The filling factors corresponding to the observed QHstates are indicated.Figure 14: Temperature robustness of the quantum Hall effect.Longitudinale magnetoresistivity ρ xx at T = 4K (dashed line, rightscale). Hall resistance R xy as a function of the magnetic field fordiffer<strong>en</strong>t temperatures: T = 4K (thick line), and T = 300K (thinline).B.A. Piot, C. Faugeras, M. Potemski, D.K. MaudeC. Berger, W. A. de Heer (School of Physics, Georgia Institute of Technology, Atlanta, USA)12


2009 CARBON ALLOTROPESImproving graph<strong>en</strong>e’s cleanliness for high field magneto-transportPulsed magnetic field magneto-transport on exfoliatedgraph<strong>en</strong>e has be<strong>en</strong> performed over the last few years andpreliminary results have shown anomalous Integer QuantumHall effect in disordered samples. The use of veryhigh magnetic field is required to investigate on the fundam<strong>en</strong>talelectronic states of 2D graph<strong>en</strong>e, where Landaulevel deg<strong>en</strong>eracy is expected to be lifted by the field. Forev<strong>en</strong> stronger magnetic field, the system ev<strong>en</strong>tually evolvesinto the fractional quantum Hall effect regime [Bolotin etal. Nature 462, 196 (2009)]. However, to make these investigationspossible, clean graph<strong>en</strong>e devices (that is freeof defects or impurities and displaying very high mobility)are necessary. Actually, graph<strong>en</strong>e devices are inescapablyheavily contaminated through the fabrication and contactingprocesses, as well as by direct exposure to air. Therefore,effici<strong>en</strong>t cleaning procedures have to be found in orderto recover the intrinsic properties of graph<strong>en</strong>e.Figure 16: Resistance of the graph<strong>en</strong>e sample as a function ofgate voltage after several annealing processes.Figure 15: (a) Example of home-made graph<strong>en</strong>e device mountedon a pulsed-field fri<strong>en</strong>dly sample holder (b) Optical microscopeimage of the c<strong>en</strong>tral part of the device.Successive cleaning processes have be<strong>en</strong> initiated in thelaboratory. Samples are first annealed at 250 ◦ C in secondaryvacuum. Investigations have shown that this processdrastically improves the quality of the samples which,however, quickly degra<strong>des</strong> wh<strong>en</strong> exposed to air. The devicesare th<strong>en</strong> connected inside the experim<strong>en</strong>tal measurem<strong>en</strong>tsetup and annealed at 90 ◦ C under vacuum. This secondannealing helps in recovering high quality samples. Finally,electrical annealing [Moser et al. Appl. Phys. Lett.91, 163513 (2007)] is performed just before the magnetotransportmeasurem<strong>en</strong>ts take place. All the aforem<strong>en</strong>tionedprocedures require specific know-how and oft<strong>en</strong> lead tosample’s <strong>des</strong>truction if not properly performed. These necessarytests (which are both time and sample consuming)have be<strong>en</strong> done with home-made graph<strong>en</strong>e samples (see figure15). Micro-mechanical cleaving of graphite (to obtaingraph<strong>en</strong>e on a substrate) followed by electron-beam lithography,etching and metal deposition have be<strong>en</strong> performedusing clean-room facilities at LAAS (CNRS).Figure 16 illustrates the influ<strong>en</strong>ce of two of the above m<strong>en</strong>tionedcleaning methods on a graph<strong>en</strong>e sample. The resistanceis measured as a function of gate voltage before andafter annealing. The position of the resistance maximum aswell as the HWFM can be used to estimate the cleanlinessof the device. Further improvem<strong>en</strong>ts have be<strong>en</strong> achievedon similar home-made devices and high magnetic field experim<strong>en</strong>tsare now under progress. These annealing methodshave also be<strong>en</strong> successfully tested on another graph<strong>en</strong>esample (provided by the University of Manchester) and adirect comparison of the results could be made betwe<strong>en</strong> thedisordered and clean regime. In the close vicinity of thecharge neutrality point, in the disordered case, transport isdominated by the formation of electron and hole puddlesin the sample over a large <strong>en</strong>ergy range. Accordingly themean Hall resistance is weak (contribution of electrons andholes to the Hall resistance cancel each other) and displayslarge fluctuations. Actually, disorder prev<strong>en</strong>ts the occurr<strong>en</strong>ceof Landau level deg<strong>en</strong>eracy lifting which could notbe observed in magnetic field as high as 60 T. A weak annealingof the device drastically changed its transport properties;at very high magnetic field the Hall resistance increases(contrary to the disordered case) although withoutdisplaying a new quantized resistance plateau. This effecttogether with the diverg<strong>en</strong>ce of the longitudinal resistanceat very high magnetic field are interpreted as a first sign ofLandau level deg<strong>en</strong>eracy lifting. Further experim<strong>en</strong>ts withimproved annealing processes are curr<strong>en</strong>tly in progress toaddress the clean high field magneto-transport regime ingraph<strong>en</strong>e.J.M. Poumirol, R. Ribeiro, A. Kumar, W. Escoffier13


CARBON ALLOTROPES 2009Metal-insulator transition for filling factor ν = −2 to ν = 0 in graph<strong>en</strong>eIn the framework of the scaling theory of the integer quantumHall effect (IQHE), plateau-plateau (PP) and plateauinsulatortransitions (PI) are interpreted as quantum phasetransitions with an associated universal critical expon<strong>en</strong>tκ. The underlying physics is the Anderson localizationdelocalization.We investigate the quantum Hall effect(QHE) in a graph<strong>en</strong>e sample at high magnetic fields, discoveringa metal-insulator (MI) quantum phase transitionpassing from filling factor ν = −2 to ν = 0. The analysisof the temperature dep<strong>en</strong>d<strong>en</strong>ce of the longitudinal resistancegives the value κ = 0.57 for the critical expon<strong>en</strong>tof the MI (i.e PI) transition. This value is the same asthat found experim<strong>en</strong>tally on the PI transitions in semiconductorsin quantum Hall regime [D. Shahar et al., SolidState Comm. 107, 19 (1998)] while is diverse from thePP transition expon<strong>en</strong>t κ = 0.42 [A.J.M. Giesbers et al.arXiv:0908.0461v1]).For this purpose we have used graph<strong>en</strong>e onto a Si waferwith a 300 nm SiO 2 top layer. It was processed depositing50Å Ti /500Å Au contacts in a Hall-bar geometry by usinge-beam nanolithography. The sample was annealed in-situprior to insertion into the cryostat at 100C for 90 minutesin a low pressure He exchange gas atmosphere. The insetwas placed in a 4 He bath cryostat while four probe measurem<strong>en</strong>tswere carried out using standard ac lock-in techniqueswith excitation curr<strong>en</strong>ts of 1−10 nA and frequ<strong>en</strong>ciesof 1.3 − 13 Hz. The Dirac point appeared at V Dirac = −3V. In Fig.17 we show the longitudinal (R xx ) and Hall (R xy )resistances as a function of the magnetic field from 1.4to 4 K, with V gate = −8V. The hole d<strong>en</strong>sity was n 2D =4.1×10 11 cm −2 and the mobility µ = 1.3×10 4 cm 2 V −1 s −1 .R xx grows expon<strong>en</strong>tially and appears to exhibit a T indep<strong>en</strong>d<strong>en</strong>tcritical point at B c = 16.7T, while R xy closely followsthe ν = 0 quantized value, deep into the insulating phase.Unfortunately, the diverging behavior of R xx seriously hindersthe determination of R xy , as ev<strong>en</strong> a small Hall-contactmisalignm<strong>en</strong>t will result in a dominant contribution fromR xx this is why we show in the inset the R xy for +B and −Bin solid lines and R a xy = 1 2 [R xy(B)−R xy (−B)] in dashed line.The experim<strong>en</strong>tal characterization of quantum Hall PP andPI quantum phase transitions, relies on the behavior of thesystem as a function of T for magnetic fields suffici<strong>en</strong>tlyclose to the transition point. In the vicinity of the criticalpoint (B c in our case) the longitudinal resistance is expectedto follow the empirical law:R xx = exp[−∆ν/ν 0 (T )], (3)with ∆ν = 1/B − 1/B c and B c = 16.7T (ν here should notbe confused with the Landau level filling factor). Fittingto Eq.(3) the experim<strong>en</strong>tal R xx measured in function of Twe can obtain the associated critical expon<strong>en</strong>t κ by usingν −10∝ T −κ . [D.C. Tsui, Rev. Mod. Phys. 71, 891-895(1999)]. In Fig(18) we plot the R xx as a function of ∆ν with∆ν = 1/B - 1/B c T. Using the scaling procedure we obtainν 0 and a critical expon<strong>en</strong>t κ = 0.57 (shown in the upper insert).We believe that this MI transition belongs to the sameuniversality class as the conv<strong>en</strong>tional PI transition from thelast quantum Hall liquid to the quantum Hall insulator.Figure 17: Longitudinal (R xx ) and Hall (R xy ) resistances as afunction of B for T = 1.4, 2, 3 and 4K with a V gate = −8V.Figure 18: Longitudinal resistance (R xx ) as a function of ∆ν. Inthe lower inset we show log(R xx ) as a function of B while in theupper the linear fit to obtain κD.K. MaudeM. Amado and E. Diez (Laboratorio de bajas temperaturas, Universidad de Salamanca, Spain), D. López-Romero (CT-ISOM, Universidad Politécnica de Madrid, Spain) J.M. Caridad, F. Rossella and V. Bellani (Universitá degli studi diPavia, Italy)14


2009 CARBON ALLOTROPESHow perfect can graph<strong>en</strong>e be?We have id<strong>en</strong>tified the cyclotron resonance (CR) responseof purest graph<strong>en</strong>e ever investigated, which can be found innature on the surface of bulk graphite, in form of decoupledlayers from the substrate material, and which have be<strong>en</strong> rec<strong>en</strong>tlydiscovered in scanning tunnelling experim<strong>en</strong>ts [G.Li et al., Phys. Rev. Lett. 103, 176804 (2009)]. Probingsuch flakes in the THz range at very low magnetic fields, wedemonstrate a superior electronic quality of these ultra lowd<strong>en</strong>sity layers (n 0 ≈ 3×10 9 cm −2 ) expressed by the carriermobility in excess of 10 7 cm 2 /(V.s) or scattering time ofτ ≈ 20 ps. These values significantly exceed those reportedin any kind of manmade graph<strong>en</strong>e samples.The cyclotron resonance of electrons in these graph<strong>en</strong>eflakes has be<strong>en</strong> measured in a high-frequ<strong>en</strong>cy electron paramagneticresonance setup in double-pass transmission configuration,using the magnetic-field-modulation technique.A flake of natural graphite was placed in the variable temperatureinsert of the superconducting sol<strong>en</strong>oid and viaquasi-optics exposed to the linearly polarized microwaveradiation emitted by a Gun diode.A typical example of our experim<strong>en</strong>tal finding is illustratedin figure 19a, where the derivative of the magnetoabsorptionspectrum of decoupled graph<strong>en</strong>e on the surfaceof a natural graphite specim<strong>en</strong> at T = 25 K, measured asa function of the magnetic field at a fixed microwave frequ<strong>en</strong>cy.The interpretation is schematically illustrated inpart (b). The observed spectral lines are assigned to cyclotronresonance transitions betwe<strong>en</strong> adjac<strong>en</strong>t Landau levelswith <strong>en</strong>ergies: E n = sign(n)˜c √ 2eB|n|, characteristicof massless Dirac fermions in graph<strong>en</strong>e sheets with an effectiveFermi velocity ˜c. This velocity is the only adjustableparameter required to match the <strong>en</strong>ergies of theobserved and calculated CR transitions and reaches ˜c =(1.00 ± 0.02) × 10 6 m.s −1 .Since the well-defined Landau level quantization in ourgraph<strong>en</strong>e flakes is spotted down to |B| = 1 mT we obtainvia the semi-classical quantization condition µB > 1 thecarrier mobility µ > 10 7 cm 2 /(V.s), almost two orders ofmagnitude higher in comparison to any other reported values.The scattering time τ ≈ 20 ps derived from the typicalCR width in our spectra also significantly exceeds valuesreported in any kind of graph<strong>en</strong>e samples. This scatteringtime gives an indep<strong>en</strong>d<strong>en</strong>t estimation for the mobilityµ = eτ ˜c 2 /E F ≈ 3 × 10 7 cm 2 /(V.s) in good agreem<strong>en</strong>twith the estimate above. Interestingly, bearing in mindthis exceptional quality, one may conclude that Landaulevel quantization should survive in studied graph<strong>en</strong>e layersdown to the field of B = (/(E 1 · τ)) 2 ≈ 1 µT. H<strong>en</strong>ce,the magnetic field of the Earth of ∼ 50 µT is no longer negligiblysmall. Instead, the <strong>en</strong>ergy gap up to ∆ ≈ 0.3 meVshould appear at the Dirac point, dep<strong>en</strong>ding on the sampleori<strong>en</strong>tation.Figure 19: (Derivative of) a typical magneto-absorptionspectrum measured at T = 25 K and microwave frequ<strong>en</strong>cyω = 1.171 meV (a) in comparison with the Landau level fanchart (b), where the observed CR transitions are shown by arrows.The occupation of individual levels is giv<strong>en</strong> by the Fermi-Diracdistribution plotted in the part (c). For simplicity, we consideredonly n-type doping with E F = 6.5 meV. The dashed lines showpositions of resonances assuming ˜c = 1.00 × 10 6 m.s −1 .Moreover, the estimated mobility should not decrease withtemperature, as no broad<strong>en</strong>ing of CRs is observed up toT = 50 K, wh<strong>en</strong> CR int<strong>en</strong>sities become comparable withthe noise. This extremely high value of mobility combinestwo effects: the long scattering time τ and a very small effectivemass m = E F / ˜c 2 ≈ 2 × 10 −4 m 0 E F [meV]. Remarkably,the same scattering time in a moderate d<strong>en</strong>sity sample(n 0 = 10 11 cm −2 ), would imply the mobility still remaininghigh, around µ ≈ 5×10 6 cm 2 /(V.s), and comparable to bestmobilities of two-dim<strong>en</strong>sional electron gas in GaAs structuresat these d<strong>en</strong>sities.To conclude, our measurem<strong>en</strong>t significantly shifts the curr<strong>en</strong>tlimits of intrinsic mobility in graph<strong>en</strong>e and poses aquest for further developm<strong>en</strong>t in the technology of its fabrication.For details see, P. Neugebauer et al., Phys. Rev. Lett. 103,136403 (2009).P. Neugebauer, M. Orlita, C. Faugeras, A.-L. Barra, M. Potemski15


CARBON ALLOTROPES 2009Effect of a magnetic field on the two-phonon Raman scattering in graph<strong>en</strong>eAmong the differ<strong>en</strong>t features that can be observed in theRaman scattering spectrum of graph<strong>en</strong>e or graphite, theso-called 2D band feature is of particular interest. It is afully resonant second order Raman scattering process anddirectly involves the electronic band structure. Its observationas a single Lor<strong>en</strong>tzian shaped contribution is a uniquefingerprint of the monolayer character of a graph<strong>en</strong>e specim<strong>en</strong>or of the decoupled nature of the graphitic planes inmultilayer epitaxial graph<strong>en</strong>e samples. As a fully resonantsecond order Raman scattering process, it shows a dispersionwith excitation laser <strong>en</strong>ergy which was used to tracethe phonon band structure of differ<strong>en</strong>t carbon allotropes.We have measured the evolution of the 2D band feature ofa multilayer epitaxial graph<strong>en</strong>e sample as a function of themagnetic field with the experim<strong>en</strong>tal set-up and in the sameconfiguration as is <strong>des</strong>cribed in the preceding report. As canbe se<strong>en</strong> with the black dots in the left part of figure 20, fromB=0 to 33 T we observe first a quadratic and th<strong>en</strong> a linearcontinuous red shift of the <strong>en</strong>ergy of this feature (8 cm −1 )together with a broad<strong>en</strong>ing of 20%.As can be se<strong>en</strong> in the schematics in the right part of figure20, in the semi-classical real-space picture of the Ramanprocess, the incid<strong>en</strong>t photon creates an electron and thehole with opposite mom<strong>en</strong>ta at an arbitrary location withinthe laser spot. They subsequ<strong>en</strong>tly propagate along the classicaltrajectories, and emit phonons. If they meet at someother location, again with opposite mom<strong>en</strong>ta, they can recombineradiatively producing a scattered photon. In theabs<strong>en</strong>ce of magnetic field, the trajectories are straight lines,so that in order to meet at the same point with opposite mom<strong>en</strong>taand contribute to the Raman signal, during phononemission the electron and the hole must necessarily be scatteredbackwards. This fixes the phonon mom<strong>en</strong>tum q(measured from the K or K ′ point) as q = p + p ′ , wherep = ω L /(2c∗) and p ′ = (ω L − 2ω ph )/(2c∗) are theelectronic mom<strong>en</strong>ta (also measured from the Dirac points)before and after the phonon emission, ω L and ω ph are respectivelythe excitation laser and the phonon frequ<strong>en</strong>cies,and c∗ is the electron velocity.In a magnetic field, the electron and hole trajectories ar<strong>en</strong>o longer straight lines but, because of the Lor<strong>en</strong>tz forcethat acts on charged particles in a magnetic field, they correspondto Larmor circles. As a result, (i) phonons withsmaller mom<strong>en</strong>ta, q = pcosϕ + p ′ cosϕ ′ , can be emitted,and (ii) since each phonon can be emitted at an arbitraryinstant in time, the l<strong>en</strong>gth of the arc <strong>des</strong>cribing the electrontrajectory is random [not exceeding the electron meanfree path c ∗ /(2γ), where γ is the electron scattering rate],and so are the angles ϕ,ϕ ′ . Tuning the magnetic field is,in this s<strong>en</strong>se, equival<strong>en</strong>t to changing the resonant conditionsof the Raman scattering process at a fixed excitationwavel<strong>en</strong>gth and allows spanning part of the phonon bandstructure closer to the K point. Fact (i) results in an overallred shift of the Raman peak, while fact (ii) introduces anadditional spread in q, and contributes significantly to thebroad<strong>en</strong>ing of the peak as observed through Raman scatteringmeasurem<strong>en</strong>ts.The solid red lines in figure 20 are the result of a calculationof the maximum Raman scattering int<strong>en</strong>sities as a functionof magnetic field following our model calculating the Ramanmatrix elem<strong>en</strong>t with an applied magnetic field and withthe assumption that Landau levels at the excitation laser <strong>en</strong>ergyare not separated (non-quantizing magnetic fields forhigh <strong>en</strong>ergy charge carriers). Experim<strong>en</strong>tal results are wellreproduced with only two adjustable parameters, the electronscattering rate deduced to be γ = 27 meV and σ, abroad<strong>en</strong>ing parameter introduced to take into account scatteringmechanisms other than electronic scattering and responsiblefor half of the observed total broad<strong>en</strong>ing. Thisfield induced 2D band feature evolution is not typical forgraph<strong>en</strong>e and should also be observed in graphite.Figure 20: Left: Black dots are the 2D band feature Raman shiftand line width as a function of the magnetic field and solid redlines are calculated with our model. Right: Real space schematicsof the second order Raman scattering process responsible for the2D band at B=0T and B≠0T. The lightning is the excitation laserwith <strong>en</strong>ergy E L , black arrows repres<strong>en</strong>t the electron and hole trajectorieswith mom<strong>en</strong>tum p (-p) before the phonon emission andp’ (-p’) after, dashed gre<strong>en</strong> arrows are the K point optical phononswith mom<strong>en</strong>tum q and <strong>en</strong>ergy E(q), the flash is the emission of theRaman photon.C. Faugeras, P. Kossacki, M. Amado, M. PotemskiD. Basko (LPMMC-CNRS, Gr<strong>en</strong>oble, France), M. Sprinkle, C. Berger, W.A. de Heer (Georgia Institute of Technology,Atlanta, USA)16


2009 CARBON ALLOTROPESTuning the electron-phonon coupling in graph<strong>en</strong>e with magnetic fieldsLattice vibrations in solids, phonons, can be effectivelymodified via their coupling to electronic excitations givingrise to many ph<strong>en</strong>om<strong>en</strong>a such as the Köhn anomaly in metals,differ<strong>en</strong>t phonon mo<strong>des</strong> observed in semiconducting orin metallic carbon nanotubes or coupled phonon-plasmonmo<strong>des</strong> in doped polar semiconductors.In graph<strong>en</strong>e which is not a polar material, the zone c<strong>en</strong>terE 2g optical phonons, the so-called G-band, effici<strong>en</strong>tlycouple to low <strong>en</strong>ergy, direct electronic transitions (∆ k = 0)through the deformation pot<strong>en</strong>tial interaction. Low <strong>en</strong>ergydirect electronic transitions exist in graph<strong>en</strong>e thanks to itspeculiar band structure in which the conduction and theval<strong>en</strong>ce bands touch at the Dirac point (gapless material)and exhibit a linear dispersion. These transitions r<strong>en</strong>ormalizethe E 2g phonons <strong>en</strong>ergy observed for instance throughRaman scattering experim<strong>en</strong>ts. As a consequ<strong>en</strong>ce, a modificationof the electronic excitation spectrum can modifythe E 2g phonon <strong>en</strong>ergy, a situation unique for a cond<strong>en</strong>sedmatter system and not <strong>en</strong>countered in traditionalsemiconductor-based systems for which a band gap of <strong>en</strong>ergymuch larger than the phonon <strong>en</strong>ergy is pres<strong>en</strong>t and imposesa low <strong>en</strong>ergy onset for such direct electronic transitions.A method to severely alter the electronic excitation spectrumis to apply a magnetic field perp<strong>en</strong>dicular to thegraph<strong>en</strong>e plane. Under such conditions, the electronic excitationspectrum characteristic for graph<strong>en</strong>e which is continuousat zero magnetic field, becomes discrete and composedof a series of optical transitions among Landau levelsas observed through magneto-infrared experim<strong>en</strong>ts. In multilayerepitaxial graph<strong>en</strong>e samples grown on the carbon faceof a SiC substrate, the electronic scattering rate is extremelylow and Landau levels are well separated at magnetic fieldsas low as 40 mT. We have performed high field magneto-Raman scattering experim<strong>en</strong>ts with such high quality samplesin the back scattering configuration to observe possiblemodifications of the E 2g phonon <strong>en</strong>ergy.The observed Raman scattering signal arising from thislong wavel<strong>en</strong>gth phonon is composed of two distinct contributions,a field indep<strong>en</strong>d<strong>en</strong>t contribution and a magnetooscillatorycompon<strong>en</strong>t which field evolution is pres<strong>en</strong>ted infigure 21 as a false color plot. We observe a well definedseries of avoided crossings each time an optical transition istuned in resonance with the E 2g phonon <strong>en</strong>ergy. Wh<strong>en</strong> allpossible electronic transitions are far from the E 2g phonon<strong>en</strong>ergy, the effective interaction is very weak as revealed bythe minimum line width of ∼ 7 cm −1 of the Raman scatteringsignal of the E 2g phonon, imposed in these conditionsby scattering mechanisms other than the electron-phononscattering.This effect had be<strong>en</strong> nicely anticipated theoretically [Ando,J. Phys. Soc. Jpn. 76, 024712 (2007)] and the pink linesin figure 21 are the results of this calculation for a neutralgraph<strong>en</strong>e system with a dim<strong>en</strong>sionless electron-phononcoupling constant λ = 4.5 × 10 −3 and a broad<strong>en</strong>ing parametercharacteristic for electronic transitions δ = 90cm −1 .This experim<strong>en</strong>t allows to directly extract the str<strong>en</strong>gth ofthe electron-phonon interaction and gives an insight into therich physics of electron-phonon coupling in graph<strong>en</strong>e.Figure 21: Energy color map and evolution of the Half Widthat Half Maximum (HWHM) of the magneto-oscillatory compon<strong>en</strong>tof Raman scattering spectra of E 2g (G band) phonons asa function of the square root of the magnetic field measured atT = 4.2 K under λ = 720.7 nm laser excitation. The extractedpeak position and line width of this contribution are shown withfull dots. Their size is proportional to the line amplitude. Solidlines T k repres<strong>en</strong>t the <strong>en</strong>ergies of the series of inter Landau leveltransitions:L k;(k−1) → L k+1;(k) which couple to E 2g phonon (c* =1.02 × 10 6 m.s −1 is assumed). The solid pink lines are the resultsof the model <strong>des</strong>cribing the magneto-phonon resonance ingraph<strong>en</strong>e.C. Faugeras, M. Amado, P. Kossacki, M. Orlita, M. PotemskiM. Sprinkle, C. Berger, W.A. de Heer (Georgia Institute of Technology, Atlanta, USA)17


CARBON ALLOTROPES 2009Thermal conductivity of graph<strong>en</strong>e in Corbino membrane geometrySystems of fewer than three dim<strong>en</strong>sions are consideredto be very effici<strong>en</strong>t heat spreaders as their intrinsic thermalconductivity may ev<strong>en</strong>tually diverge for infinite specim<strong>en</strong>s,following a power or logarithmic law for one- ortwo-dim<strong>en</strong>sional systems, respectively. This conjecture isnow being confronted with experim<strong>en</strong>tations on graph<strong>en</strong>e -a single sheet of graphite, the closest archetype of a twodim<strong>en</strong>sionalcrystal. Carbon crystallites such as diamondand graphite are known as exceptional heat conductors andan extremely effici<strong>en</strong>t thermal conductivity has be<strong>en</strong> alsoreported for graph<strong>en</strong>e [Balandin et al., NanoLett 8, 902,(2008)]. This conclusion calls, however, for confirmationbecause the experim<strong>en</strong>tal methods applied to draw it ar<strong>en</strong>ot fully straightforward. A precise (contactless) temperaturereadout, an accurate sample geometry and an exactestimation of the absorbed laser power are among subtle issueswhich may significantly influ<strong>en</strong>ce the appar<strong>en</strong>t valuesof the extracted 3D thermal conductivity coeffici<strong>en</strong>t.We have performed a study of the thermal properties of alarge area graph<strong>en</strong>e membrane which fully covers a 44 µmdiameter pinhole made in the 2 mm thick plate of copper(see photograph in the inset of figure 22). With the use ofsilver epoxy, the edges of the membrane (which ext<strong>en</strong>d outsidethe pinhole) are thermally short circuited to the copperplate which serves in our experim<strong>en</strong>ts as a room temperatureheat sink. The groundwork of our experim<strong>en</strong>ts consistsin using laser excitation to locally g<strong>en</strong>erate heat and measuringthe Raman scattering spectra to extract the actualtemperature of the membrane within the laser spot fromthe int<strong>en</strong>sity ratio of Stokes to anti-Stokes Raman scatteringsignals. Our Corbino-like experim<strong>en</strong>tal configurationtogether with the direct temperature readout largely simplifiesthe data analysis. We pres<strong>en</strong>t in figure 22 typicalStokes and anti-Stokes Raman scattering spectra measuredat differ<strong>en</strong>t location along the radius of the membrane. Asexpected and se<strong>en</strong> in this figure, the laser excitation heatslocally the membrane, most effici<strong>en</strong>tly wh<strong>en</strong> the laser spotis in the c<strong>en</strong>ter of the membrane and significantly less wh<strong>en</strong>it is placed closer to the copper plate heat sink. After carefulcalibration of the response of the experim<strong>en</strong>tal set-up,we read the temperature directly from the int<strong>en</strong>sity ratio ofthe Stokes to anti-Stokes signals : I(ω exc−ω G )I(ω exc +ω G ) = exp( ω Gk B T ),where ω exc,G are the excitation laser and the phonon frequ<strong>en</strong>cyand T is the lattice temperature under the laser spot.Figure 22: Stokes and anti-Stokes Raman scattering spectra ofthe the G-band graph<strong>en</strong>e membrane measured under 6.2 mW oflaser excitation focused at differ<strong>en</strong>t points on the membrane (atdiffer<strong>en</strong>t distances r from the c<strong>en</strong>ter of the membrane). Note thechange in the ratio of Stokes to anti-Stokes signal, which depictsthe drop of local temperature within the laser spot (2µm in diameter)wh<strong>en</strong> approaching the edge of the membrane (in thermal contactwith room temperature sink). Inset : Photograph of the 44 µmdiameter membrane as se<strong>en</strong> through a ×100 optical objective.Wh<strong>en</strong> the laser spot is located in the c<strong>en</strong>ter of the membrane(r = 0), the heat equation <strong>des</strong>cribing our experim<strong>en</strong>t can besolved analytically and one can establish the following relation:T (0)−T edge∼ = 1.689α, relating the temperature differ<strong>en</strong>cebetwe<strong>en</strong> the c<strong>en</strong>ter and the edge of the membrane assumedto be a heat sink at room temperature, to α = P/κdπ,P being the absorbed optical power rec<strong>en</strong>tly measured to be2.3% of the total excitation power, d the thickness of thegraph<strong>en</strong>e membrane and κ its 3D thermal conductivity coeffici<strong>en</strong>t.In this particular case, the temperature deducedwith a total excitation power of 6.2 mW focused on a 2 µmdiameter spot is T = 660 K and a resulting α coeffici<strong>en</strong>t of216 K.The 3D equival<strong>en</strong>t thermal coeffici<strong>en</strong>t is κ ≈ 630 W/m·K,i.e., somewhat less th<strong>en</strong> previously claimed. The differ<strong>en</strong>cebetwe<strong>en</strong> the pres<strong>en</strong>t and previous estimations of κ is mainlydue to differ<strong>en</strong>t assumptions regarding the effici<strong>en</strong>cy of thegraph<strong>en</strong>e’s optical absorbance. Finite elem<strong>en</strong>ts computationsperformed to deduce the values for α in the case ofexcitations at other locations along the radius of the membraneconfirm the validity of our approach.C. Faugeras, M. Orlita, M. PotemskiB. Faugeras (Université de Nice, Nice, France), R.R. Nair, A.K. Geim (University of Manchester, Manchester, UnitedKingdom)18


2009 CARBON ALLOTROPESElectric field doping of few-layer graph<strong>en</strong>eThe electronic properties of few-layer graph<strong>en</strong>e have be<strong>en</strong>investigated at low temperature and high magnetic field.Few-layer graph<strong>en</strong>e systems consist of a few t<strong>en</strong>s of planesof carbon atoms stacked upon each others and exhibit acomplex electronic band structure. Regarding their transportproperties, they are natural candidates to study thecross over from 3D graphite to 2D graph<strong>en</strong>e. So far, manystudies have focused on graph<strong>en</strong>e, where a linear dispersionrelation at the K and K ′ points of the first Brillouin zoneleads to transport properties governed by massless quasiparticles.Such charge carrier dynamic makes graph<strong>en</strong>ea unique 2D system and is responsible, among other, tothe anomalous quantum Hall effect. On the other hand,graphite supports the pres<strong>en</strong>ce of differ<strong>en</strong>t groups of chargecarriers (electron-like and hole-like quasi-particles), amongwhich massless Dirac fermions have already be<strong>en</strong> reported[Luk’yanchuck et al. Phys. Rev. Lett., 93, 166402 (2004)].The experim<strong>en</strong>tal investigation of few-layer graph<strong>en</strong>e hasbe<strong>en</strong> undertak<strong>en</strong> in an attempt to determine the relative contributionsof the differ<strong>en</strong>t types of charge carriers to electronictransport, in a system where a small number of carbonlayers makes its electronic properties half-way betwe<strong>en</strong>those of graphite and graph<strong>en</strong>e.+70 V shows a monotonously increasing function with nohint of resistance maximum. We therefore infer that thesample is intrinsically p-doped and that the charge neutralitypoint is out of the experim<strong>en</strong>tal range. Contaminantsand/or defects are responsible for shifting the charge neutralitypoint away from V g = 0 V.Figure 24: 3D plot of the Hall resistance R xy as a function ofmagnetic field B and gate voltage V gFigure 23: Oscillatory part of R xx (B,V g ) after subtracting asmooth background function. For clarity, the curves are shiftedvertically by 1.5 kΩThe few-layer graph<strong>en</strong>e sample is obtained by exfoliationof bulk graphite and deposited onto a heavily dopedSi/SiO 2 substrate with 300 nm oxide thickness. Fourelectro<strong>des</strong> have be<strong>en</strong> fabricated on the sample using photolithographyso that the two-probe longitudinal and Hallresistance could be simultaneously measured during a pulseof the magnetic field. A gate voltage is applied thoughthe SiO 2 dielectric in order to continuously tune the chargecarrier d<strong>en</strong>sity. As compared to the simple plane capacitormodel usually accepted for graph<strong>en</strong>e, the few-layergraph<strong>en</strong>e system displays reduced gate effici<strong>en</strong>cy, mostprobably due to large scre<strong>en</strong>ing effects. The gate voltagedep<strong>en</strong>d<strong>en</strong>ce of the resistance in the range −70 < V g


CARBON ALLOTROPES 2009Low temperature magneto-transport in natural graphiteHistorically, graph<strong>en</strong>e forms the starting point for the Slonczewski,Weiss and McClure (SWM) band structure calculationsof graphite. In graphite, the Bernal stacked graph<strong>en</strong>elayers are weakly coupled with the form of the in-planedispersion dep<strong>en</strong>ding upon the mom<strong>en</strong>tum k z in the directionperp<strong>en</strong>dicular to the layers. The carriers occupy a regionalong the H − K − H edge of the hexagonal Brillouinzone. At the K point (k z = 0), the dispersion of the electronpocket is parabolic (massive fermions), while at the H point(k z = 0.5) the dispersion of the hole pocket is linear (masslessDirac fermions). A clear signature of Dirac fermionsat the H point of graphite has rec<strong>en</strong>tly be<strong>en</strong> reported usingfar-infrared magneto-absorption and ARPES measurem<strong>en</strong>ts.Such measurem<strong>en</strong>ts probe the very close vicinity ofthe H and K points where there is a maximum in the jointd<strong>en</strong>sity of states.Typical low temperature R xx versus magnetic field for naturalgraphite, is shown in Fig. 25(a). The quantum oscillations,superimposed on a large magneto-resistance background,can be better se<strong>en</strong> in the background removed data∆R xx plotted in Fig. 25(a-c). Quantum oscillations are observedfor both majority electrons and holes with orbitalquantum number up to almost N = 100. These oscillationsare fully consist<strong>en</strong>t with the pres<strong>en</strong>ce of majority electronand hole pockets within the three dim<strong>en</strong>sional SWM bandstructure calculations for graphite [Schneider et al. Phys.Rev. Lett. 102, 166403 (2009)]. At low magnetic fields,a perfect linear behavior in N(1/B) is observed for bothelectrons and holes. For high magnetic fields, clear deviationsfrom the linear behavior are observed for the electronfeatures (see Fig. 26(b-c)). This deviation from a periodicin 1/B behavior at high magnetic fields is due to theFermi level moving as the quantum limit is approachedin graphite. Clearly, the high field data should not beused to extract the phase of the oscillations. Instead weuse the complex Fourier transform ˆf (B) of the low magneticfield ∆R xx (1/B). The phase shift function K(ϕ,B) =Re[e −iϕ ˆf (B)] has maximum in the ϕ − B plane which canbe used to extract both the frequ<strong>en</strong>cy (B) and phase (ϕ) ofthe oscillations. K(ϕ,B) is plotted in Fig. 26(d-e) in theregions of the hole and electron features. From the maxima,the determined frequ<strong>en</strong>cy and phase are B fh = 4.51 T,ϕ h = −(0.56±0.1)π and B fe = 6.14 T, ϕ e = −(0.86±0.1)πfor the hole and electron features respectively.We therefore conclude that we have no evid<strong>en</strong>ce for theexist<strong>en</strong>ce of masseless Dirac fermions with a Berry phaseγ = 0. Transport measurem<strong>en</strong>ts are s<strong>en</strong>sitive to the d<strong>en</strong>sityof states at E F , which is modulated with increasing magneticfield, as the Landau bands cross the Fermi <strong>en</strong>ergy. Forholes, maxima in the d<strong>en</strong>sity of states correspond to Landaubands crossing E F for k z < 0.5, away from the H point,where the dispersion is no longer linear and a priori there isno reason to expect the carriers to behave as Dirac fermions.Figure 25: (a) Resistance R xx versus B measured at T = 10 mKfor natural graphite. (a-c) Background removed data ∆R xx showingquantum oscillations measured over differ<strong>en</strong>t magnetic fieldregions. The arrows indicate spin split electron and hole features.Figure 26: (a) Fourier transform of the low magnetic field∆R xx (1/B). (b-c) Orbital angular mom<strong>en</strong>tum quantum numberN, as a function of the reciprocal magnetic field positions of theelectron and hole features. (d) and (e) Contour plot of the phaseshift function K(ϕ,B) in the vicinity of the hole and electron features.Maxima in K(ϕ,B) determines the frequ<strong>en</strong>cy and phase ofthe oscillations.J. M. Schneider, M. Orlita, M. Potemski and D. K. Maude20


2009 CARBON ALLOTROPESMagnetotransport to extract the spin gap for charged excitations in graphiteIn a magnetic field the properties of graphite are remarkablywell <strong>des</strong>cribed by the Slonczewski, Weiss and Mc-Clure (SWM) band structure calculations. While orbitaleffects have be<strong>en</strong> ext<strong>en</strong>sively used to caliper the Fermi surface,the more subtle spin effects have received less att<strong>en</strong>tion.Indeed, the well docum<strong>en</strong>ted movem<strong>en</strong>t of the Fermi<strong>en</strong>ergy in a magnetic field seriously complicates the extractionthe spin gap (g-factor) from the magnetotransport data.Rec<strong>en</strong>t advances in experim<strong>en</strong>tal techniques, in particularthe vastly increased <strong>des</strong>ktop computing power available fordiagonalizing the SWM Hamiltonian, makes it timely torevisit this problem, ext<strong>en</strong>ding previous measurem<strong>en</strong>ts tohigher magnetic fields and lower temperatures.The oscillatory compon<strong>en</strong>t of longitudinal resistance ∆R xxas a function of the magnetic field from B = 0 − 28 T forvaries ori<strong>en</strong>tations betwe<strong>en</strong> θ = 0 ◦ and θ = 90 ◦ is shownin figure. 27(a). Quantum oscillations due to the majorityelectrons and holes Fermi surfaces are clearly observed.For increasing tilt angles the quantum oscillations shift as1/cos(θ) to higher magnetic field demonstrating the quasi2D nature of graphite. The experim<strong>en</strong>tally observed splitting∆B = B ↓ − B ↑ , where B ↑ and B ↓ are the magneticfield positions of the spin up and spin down features, isplotted as a function of the mean total magnetic field positionB m = (B ↓ + B ↑ )/2 for the n = 1 electron and holefeatures (figure.27(b)). The failure of ∆B to follow a simplequadratic behavior is an experim<strong>en</strong>tal signature that themovem<strong>en</strong>t of the Fermi <strong>en</strong>ergy must be tak<strong>en</strong> into accountwh<strong>en</strong> extracting the g-factor.Figure 27: (a) ∆R xx as a function of the magnetic field for differ<strong>en</strong>tangles (0 ◦ ≤ θ ≤ 90 ◦ ). (b) Magnetic field splitting ∆B as afunction of the total magnetic field B m . The thick line is calculatedfor the n = 1 electron Landau band with g s = 2.53 takinginto account the movem<strong>en</strong>t of the Fermi <strong>en</strong>ergy. The thin line isthe expected parabolic behaviour if E f is constant and requiresand unreasonably large value of g s = 6.5In order to extract the g-factor, we use the SWM band structuremodel.The effect of the in-plane magnetic field can beincorporated into the SWM model through an effective spingap ∆ s = g e f f µ B B ⊥ where the real g-factor g s = g e f f cos(θ).In graphite, E f moves with the applied perp<strong>en</strong>dicular magneticfield as carriers are transferred betwe<strong>en</strong> the electronand hole pockets. The Fermi level has to be calculated selfconsist<strong>en</strong>tlyassuming the sum of the electron and hole conc<strong>en</strong>trationsis constant, n− p = n 0 . At each angle, the effectivespin gap is found for which the SWM model gives thecorrect magnetic field position for the crossing of the spinup and spin down Landau band with the Fermi <strong>en</strong>ergy.Figure.28 shows the result for the spin gap ∆ s extractedfrom the SWM calculations as a function of the total magneticfield for the n = 1 hole and the n = 1 − 4 electronLandau bands. The spin gap is similar for both the electronand holes Landau bands at a giv<strong>en</strong> total magnetic field.∆ s increases linearly with magnetic field and a linear fit to∆ s = g s µ B B m (solid line) for both electron and hole Landaubands gives g s = 2.53 ± 0.07. The <strong>en</strong>hancem<strong>en</strong>t comparedto the electron spin resonance value can be attributedto electron-electron interactions.Figure 28: (a) Spin gap ∆ s for the electron and hole Landaubands, obtained by fitting the SWM model to ∆B, as a functionof the magnetic field. (b) The corresponding SWM g-factors foreach data point. The thick dashed line corresponds to g s = 2.53while the thin dashed lines correspond to the anisotropic electronspin resonance g-factors.J. M. Schneider, M. Orlita, M. Potemski and D. K. MaudeN. A. Goncharuk, P. Vasek, P. Svoboda and Z. Vyborny (Academy of Sci<strong>en</strong>ce, Prague)21


CARBON ALLOTROPES 2009Magneto-transmission spectroscopy of graphite in high magnetic fieldsThe rec<strong>en</strong>t discovery of relativistic-like, zero effective restmass particles in graph<strong>en</strong>e, an atomically thin layer of carbonhas caused a dramatic increase of interest in this material.Graphite, which is composed of Bernal stackedgraph<strong>en</strong>e layers, is a far more complex system and is notfully understood <strong>des</strong>pite nearly sev<strong>en</strong>ty years of research.In particular, spectroscopic studies have revealed the exist<strong>en</strong>ceof massive electrons at the K-point together with massless fermions near the H-point [Orlita et al. Phys. Rev. Lett.102, 166401 (2009)].In this work, we pres<strong>en</strong>t the results of transmission measurem<strong>en</strong>tsthrough a thin layer of graphite in magnetic fieldsup to 56 T. We explore the higher <strong>en</strong>ergy range of themagneto-transmission in the near visible light range usinga tungst<strong>en</strong> halog<strong>en</strong> lamp. Transmission measurem<strong>en</strong>tswere circular polarization resolved and spectra recordedfor both polarities of the magnetic field. Measurem<strong>en</strong>tswhere performed in dc magnetic fields up to 32 T in Gr<strong>en</strong>obleand in pulsed magnetic fields up to 56 T in Toulouse.Data has be<strong>en</strong> tak<strong>en</strong> at differ<strong>en</strong>t temperatures in the range4.2 − 300 K. A repres<strong>en</strong>tative transmission spectra as afunction of the temperature measured at 56 T is shown infigure 29. In the low temperature data we observe a splittingof the absorption lines (marked as ∆ in figure 29) whichvanishes with the increasing temperature.To id<strong>en</strong>tify the optical transitions we plot the position ofeach absorption line as a function of the magnetic field.The results are pres<strong>en</strong>ted in figure 30. The experim<strong>en</strong>talposition of each absorption line is marked by symbols. Simultaneouslythe theoretical prediction for the expected opticaltransitions in graphite are marked by lines. The dashedlines correspond to the optical transitions in the vicinity ofK point with an <strong>en</strong>ergy ∝ B, while the solid lines correspondto the optical transitions in the vicinity of H pointwith an <strong>en</strong>ergy ∝ √ B as for massless fermions in graph<strong>en</strong>e.As the electronic structure of graphite is more complex thanfor graph<strong>en</strong>e the optically allowed transitions (dipole interband) can be assigned to transitions betwe<strong>en</strong> L −m(−n) andL n(m) LLs, where m,n <strong>en</strong>umerates the Landau levels withthe following change of the LL index by 2 (marked in grey),by 0 (marked in black) and by 1 as for graph<strong>en</strong>e marked bydiffer<strong>en</strong>t colors.All of the transitions characteristic for graphite are wellreproduced by the theoretical predictions. However, forthe graph<strong>en</strong>e-like transitions and additional splitting of thelines is clearly observed. This is ev<strong>en</strong> more remarkablesince such a splitting is completely abs<strong>en</strong>t in magnetotransmissionmeasurem<strong>en</strong>ts on graph<strong>en</strong>e [Plochocka et al.Phys. Rev. Lett. 100, 87401 (2008)]. Intriguingly, polarizationresolved measurem<strong>en</strong>ts (not shown) demonstratethat the splitting is not polarization dep<strong>en</strong>d<strong>en</strong>t and therefor<strong>en</strong>ot linked to the asymmetry of the Dirac cone.Figure 29: Repres<strong>en</strong>tative differ<strong>en</strong>tial transmission spectra (theB = 0 T spectra has be<strong>en</strong> subtracted) measured at 56 T for differ<strong>en</strong>ttemperatures.Figure 30: Position of the absorption lines as a function of themagnetic field for spectra tak<strong>en</strong> at T = 4 K. The dashed and solidlines correspond to the calculated optically allowed dipole interbandtransitions in graphite.P. Plochocka, N. Ubrig, P. Kossacki, M. Orlita, O. Portugall, G.L.J.A. Rikk<strong>en</strong>22


2009 CARBON ALLOTROPESGraphite from the viewpoint of Landau level spectroscopy: An effectivegraph<strong>en</strong>e bilayer and monolayerThe unusual properties of massless Dirac fermions observedin graph<strong>en</strong>e monolayers, multi-layer epitaxialgraph<strong>en</strong>e or bulk graphite have be<strong>en</strong> ext<strong>en</strong>sively studied usingvarious optical and magneto-optical techniques. In contrast,few experim<strong>en</strong>ts have addressed the optical responseof a graph<strong>en</strong>e bilayer in spite of the considerable theoreticalinterest into this system. Here we show that some part ofthe physics of the graph<strong>en</strong>e bilayer can be, perhaps surprisingly,studied wh<strong>en</strong> investigating bulk graphite.We report on an infrared transmission study of a thin layerof bulk graphite prepared by a multiple exfoliation of anatural graphite crystal, performed in magnetic fields upto B = 34 T. All magneto-transmission spectra were tak<strong>en</strong>in the Faraday configuration with the magnetic field appliedalong the c-axis of the graphite, using technique ofthe Fourier transform spectroscopy.Two series of absorption lines whose <strong>en</strong>ergy scales as √ Band B were found in the spectra and id<strong>en</strong>tified as contributionsof massless holes at the H point (figure 31a)and massive electrons in the vicinity of the K point (figure.31b), respectively. We have shown that the infraredmagneto-absorption spectra of graphite, measured over awide range of the <strong>en</strong>ergy and magnetic field, can be interpretedin a very simple, transpar<strong>en</strong>t and elegant manner, i.e.that graphite can be viewed as an effective graph<strong>en</strong>e monolayerand bilayer. Our results thus confirm rec<strong>en</strong>t theoreticalmodel [B. Parto<strong>en</strong>s and F. M. Peeters, Phys. Rev. B75, 193402 (2007); M. Koshino and T. Ando, Phys. Rev.B 77, 115313 (2008)], which drastically simplifies the standardSlonczewski-Weiss-McClure model considering onlytwo tight-binding parameters γ 0 and γ 1 , which <strong>des</strong>cribe theintra- and inter-layer tunnelling, respectively.In this picture, the dominant contribution to the optical responseis provided by the H point, where electron statesclosely resemble graph<strong>en</strong>e but with an additional doubledeg<strong>en</strong>eracy, and by the K point, where the <strong>en</strong>ergy spectrumresembles a graph<strong>en</strong>e bilayer, but with an effective couplingof 2γ 1 , twice <strong>en</strong>hanced compared to a real bilayer system.Remarkably, using this simple graph<strong>en</strong>e monolayer plus bilayerview of graphite, we are able to correctly reproducethe magnetic field evolution of all observed inter-Landauleveltransitions using only the SWM parameters γ 0 and γ 1 ,with values which perfectly match those derived from studiesof real graph<strong>en</strong>e monolayer and bilayer systems (see figure.31).To conclude, the electronic states at K point of graphite areinterestingly found to mimic those of the graph<strong>en</strong>e bilayer,but with a doubled value of the effective mass. It should b<strong>en</strong>oted that as the validity of the model is limited in the vicinityof the Fermi level, it is not useful, for example, for theinterpretation of magneto-transport experim<strong>en</strong>ts. Nevertheless,bulk graphite remains a material of choice to studymagneto-optical ph<strong>en</strong>om<strong>en</strong>a in systems with both masslessas well as massive Dirac fermions.For details see, Orlita et al., Phys. Rev. Lett. 102, 166401(2009) and also Orlita et al., ibid 100, 136403 (2008).Figure 31: (a) Positions of the absorption lines related to theH point as a function of √ B. The solid and dashed lines repres<strong>en</strong>texpected positions of absorption lines for ˜c = 1.02 × 10 6 m/s(γ 0 = 3.2 eV). (b) Positions of absorption lines related to the Kpoint as a function of B. The solid lines show expected dipole allowedtransitions in a graph<strong>en</strong>e bilayer with an effective coupling2γ 1 for γ 0 = 3.2 eV and γ 1 = 0.375 eV. The inset schematicallyshows the observed inter-band transitions in the effective bilayer.The gray points in the part (b) have be<strong>en</strong> measured on highly ori<strong>en</strong>tedpyrolytic graphite.M. Orlita, C. Faugeras, J. M. Schneider, G. Martinez, D. K. Maude, and M. Potemski23


CARBON ALLOTROPES 2009Magneto-transmission of multi-layer epitaxial graph<strong>en</strong>e and bulk graphite:A comparisonThe fabrication of multi-layer epitaxial graph<strong>en</strong>e on thecarbon-terminated surface of SiC crystal [see e.g. W. A.de Heer et al., Solid State Commun. 143, 92 (2007)], withthe characteristic rotational stacking of graph<strong>en</strong>e sheets [J.Hass et al., Phys. Rev. Lett. 100, 125504 (2008)], naturallyinduced live discussions about differ<strong>en</strong>ces in electronicband structures of this system and well-known bulkgraphite, which has be<strong>en</strong> int<strong>en</strong>sively studied within lastsixty years.Here we report on magneto-transmission measurem<strong>en</strong>ts inthe far infrared spectral range, performed to help in understandingof electronic band structures of both these materials.In our study, we have compared magneto-optical responseof two kinds of samples: Multi-layer graph<strong>en</strong>e sample,which was epitaxially grown by thermal decompositionon the carbon-terminated surface of a 4H-SiC substrate andcontains around ∼100 graph<strong>en</strong>e layers, and a thin layer ofbulk graphite (single-crystal natural graphite), prepared bya simple exfoliation using an adhesive tape. Typical lowmagnetic-fielddata obtained in our experim<strong>en</strong>t are shownin Fig. 32.In our magneto-transmission measurem<strong>en</strong>ts, we have focusedon spectral features evolving linearly with √ B, whichrepres<strong>en</strong>t a hallmark of massless Dirac fermions pres<strong>en</strong>taround K and H points in graph<strong>en</strong>e and graphite, respectively.The magneto-optical response of both materialswas found to be surprisingly similar and practically thesame Fermi velocity has be<strong>en</strong> extracted from data, ˜c =1.02 × 10 6 m.s −1 . Nevertheless, the obtained data still allowedus to distinguish betwe<strong>en</strong> (strongly anisotropic) 3Dbulk graphite and 2D multi-layer epitaxial graph<strong>en</strong>e. The3D nature of bulk graphite was mainly demonstrated viaappearance of an additional set of absorption lines (d<strong>en</strong>otedby Greek letters in Fig. 32b) in comparison to multilayergraph<strong>en</strong>e. H<strong>en</strong>ce, whereas the results obtained onmulti-layer graph<strong>en</strong>e fully corresponded to expectations fordipole-allowed transitions in a 2D gas of massless Diracfermions, the transmission spectra tak<strong>en</strong> on bulk graphiteappeared to be more complex. The standard Slonczewski-Weiss-McClure model of the bulk graphite band structurewas found in latter case to be suffici<strong>en</strong>t to explain exist<strong>en</strong>ceof all absorption lines scaling as √ B as well and their individuallineshapes.For details see, M. Orlita et al., Solid State Commun. 149,1128 (2009).Figure 32: Transmissions spectra of multi-layer epitaxialgraph<strong>en</strong>e (a) and bulk graphite (b) for selected magnetic fields atT = 2 K. The absorption lines corresponding to dipole-allowedtransitions in graph<strong>en</strong>e are d<strong>en</strong>oted by Roman letters. Greek lettersare used for additional transitions which scale as √ B and areonly found in spectra tak<strong>en</strong> on bulk graphite. For clarity, the spectrain part (a) and (b) were shifted by amount of 0.18 and 0.10,respectively.M. Orlita, C. Faugeras, G. Martinez, D. K. Maude, J. M. Schneider, M. PotemskiM. Sprinkle, C. Berger, W. A. de Heer (Georgia Institute of Technology, Atlanta, USA)24


2009Two-Dim<strong>en</strong>sional Electron Gas25


2009 TWO-DIMENSIONAL ELECTRON GASThe surprisingly fragile quantum Hall ferromagnet at filling factor ν = 1In two dim<strong>en</strong>sions many body interactions oft<strong>en</strong> dominateover the single particle physics giving rise to novel collectiveground states. A striking example is the quantum Hallferromagnet. At filling factor ν = 1, the lowest Landau levelis half empty so that all the electrons have the same orbitalquantum number and only the spin degree of freedom remains.The ground state is predicted to be an extremelyrobust itinerant quantum Hall ferromagnet with a gap forspin excitations greatly exceeding the single particle Zeeman<strong>en</strong>ergy. On the other hand, either side of ν = 1 thesystem depolarizes more rapidly than predicted by the singleparticle picture, due to the formation of spin textures(Skyrmions or anti-Skyrmions) in the ground state.wave) excitation spectrum. This prediction, shown by thedot-dashed line largely overestimates the robustness of theν = 1 quantum Hall ferromagnet. Intriguingly, the predictedspin polarization calculated for two spin levels separatedby the bare Zeeman <strong>en</strong>ergy, gµ B B ≃ 2.1 K, plottedas a dashed line coinci<strong>des</strong> much better with our data. Ourresults suggest that the itinerant quantum Hall ferromagnetat ν = 1 is not robust, and collapses, wh<strong>en</strong>ever possible,to a lower <strong>en</strong>ergy ground state with a large number of reversedspins [Plochocka et al. Phys. Rev. Lett. 102, 126806(2009)].To measure the absorption spectrum of a single GaAs quantumwell (QW) at low temperatures we have used a structurewhich forms a half-cavity for the incoming light withthe QW located at the anti-node of the standing waveformed by the optical field. In figure 33(a) we plot the integratedint<strong>en</strong>sity of the absorption to the n = 0 Landau levelfor both circular polarizations as a function of filling factor.For both polarizations (σ + and σ − ) the absorption is nonzero over almost all the range 0 < ν < 2. This implies thatthe upper Zeeman (UZ) and lower Zeeman (UZ) levels arealmost never fully occupied. However, for the absorptionto the lower Zeeman (LZ) level a sharp minimum (zero) atν = 1 is observed.The spin polarization of the 2DEG can be obtained directlyfrom the optical dichroism shown in figure 33(b). The measuredpolarization at T = 1.6 K is comparable with previousabsorption and reflectivity measurem<strong>en</strong>ts, the spin polarizationsaturates at approximately 0.8 and the depolarizationon both si<strong>des</strong> of ν = 1 is roughly symmetric and compatiblewith the formation of spin textures (Skyrmions or anti-Skyrmions) in the ground state of size S ≈ A ≈ 3. At verylow temperature (T = 40 mK), the system does indeed fullypolarize within experim<strong>en</strong>tal error (∼ 0.97) at exactly fillingfactor ν = 1, and that this feature is extremely sharpwith a width of only δν ≈ 0.01 (figure.33(c)). The fully polarizedstate is a signature of the quantum Hall ferromagnetat filling factor ν = 1 while the sharp depolarization observedeither side of ν = 1 corresponds to ≈ 15 spin flipsper magnetic flux quanta added or removed from the system,consist<strong>en</strong>t with the formation of a lower <strong>en</strong>ergy spintexture (skyrmion or anti-skyrmion) ground state either sideof ν = 1.It is extremely surprising that a temperature of a few hundredmK is already suffici<strong>en</strong>t to suppress full spin polarization(figure.33(d)). The thermodynamics of the ν = 1quantum Hall ferromagnet should be governed by thermalactivation to the continuum of the spin-exciton (spinFigure 33: (a) Integrated int<strong>en</strong>sity (I σ ±) of the absorption tothe n = 0 Landau level measured for both σ + and σ − polarizationsas a function of filling factor. (b) optical dichroism,(I σ − − I σ +)/(I σ − + I σ +) (spin polarization). The calculated depolarizationfor finite size skyrmions/anti-skyrmions (A=S=3) and(A=S=15) is shown. (c) spin polarization around filling factorν = 1 measured at T=40, 500 mK and 1.6 K. (d) detailed temperaturedep<strong>en</strong>d<strong>en</strong>ce of the spin polarization at exactly ν = 1 (thesolid line is drawn as a guide to the eye). Brok<strong>en</strong> lines show thepredicted temperature dep<strong>en</strong>d<strong>en</strong>ce of the polarization for a spinwave excitation and for two spin levels separated by the singleparticle Zeeman <strong>en</strong>ergy.P. Plochocka, J. M. Schneider, D. K. Maude, M. PotemskiM. Rappaport, V. Umansky, I. Bar-Joseph (Weizmann Institute, Israel), J. G. Groshaus, Y. Gallais, A. Pinczuk(Columbia University, New York)27


TWO-DIMENSIONAL ELECTRON GAS 2009Dispersive line shape of the resistively detected NMR on either side of fillingfactor ν = 1The resistively detected nuclear magnetic resonance (RD-NMR) technique is a tool which allows the detection of theresonant excitation of nuclear spins using electrical measurem<strong>en</strong>t.This technique is especially well suited to probeNMR in high mobility two-dim<strong>en</strong>sional electron gases inthe quantum Hall regime, over a wide range of filling factors.The underlying effect is the hyperfine interactionwhich couples the nuclear and electronic spins. At the resonantradio-frequ<strong>en</strong>cy (RF) field, the nuclear spin magnetizationis reduced which, through the hyperfine interaction,leads to a change in the appar<strong>en</strong>t magnetic field se<strong>en</strong> bythe electron spins. The resulting variation of the electronicZeeman <strong>en</strong>ergy leads to a change in the sample resistance.Early measurem<strong>en</strong>ts performed on GaAs/AlGaAs heterostructuresrevealed anomalous RDNMR lines characterizedby a dispersive-like shape which occur on each sideof filling factor ν = 1 [Desrat et al. Phys. Rev. Lett. 88,256807 (2002)]. Such a line shape, composed of a negativeand a positive response of the resistance cannot be explainedby a simple uniform Zeeman <strong>en</strong>ergy change only.The origin of the anomalous line shape remains the subjectof debate. Two main ideas have aris<strong>en</strong> linking the line shapeto, (i)the contribution of domains with differ<strong>en</strong>t electronicpolarizations or (ii) the role of thermal effects (heating).The latter was supported by the inversion of the RDNMRdispersive lineshape observed betwe<strong>en</strong> ν = 1 and ν = 2/3which coincided with the change in sign of dR xx /dT .temperature increase leads to a negative (positive) ∆R xy onthe low (high) field side of ν = 1. For R xx a sign changeoccurs on each side of ν = 1. The magnetic fields forwhich ∆R xx has extrema are the fields previously introduced(B = 5.3, 5.525, 7.7 and 8 T) and labelled a, b, c and d,respectively. The comparison betwe<strong>en</strong> the dispersive RD-NMR shapes and the sign of dR/dT shows that the minmax(max-min) shapes always correspond to positive (negative)dR/dT . This is verified for both the longitudinal andthe Hall resistance.This result strongly suggests that thermal effects play a rolein the anomalous RDNMR lineshape and that the Zeeman<strong>en</strong>ergy change is not the unique contribution at the resonantRF field.Here we report similar measurem<strong>en</strong>ts but ext<strong>en</strong>ded to bothsi<strong>des</strong> of filling factor ν = 1 and to both longitudinal and Hallresistances. The eight bottom graphs in figure34 repres<strong>en</strong>tRDNMR lines measured either in R xx or in R xy at four differ<strong>en</strong>tincreasing magnetic fields, B = 5.3, 5.525, 7.7 and8 T, labeled a, b, c and d, respectively. Cases a and b areon the low field side of ν = 1 (i.e. betwe<strong>en</strong> ν = 4/3 and1), while cases c and d are on the high field side, towardsν = 2/3. All spectra show dispersive-like shapes but someconsist of a resistance minimum followed by a maximumwith increasing RF, or inversely a maximum followed bya minimum with increasing RF. The min-max shape is observedin R xx for cases b and c and in R xy for cases c andd.Now we turn to the temperature dep<strong>en</strong>d<strong>en</strong>ce of the R xx (B)and R xy (B) curves traced in the top graph of figure34. Onesees that a slight increase of the temperature, from T = 60mK to T = 70 mK, leads to a narrower plateau in R xy anda narrower dissipationless region in R xx . The resulting resistancechanges ∆R xx and ∆R xy are plotted in the middlegraph by dashed and solid lines respectively. We see that aFigure 34: (Top) R xx and R xy as a function of B for two differ<strong>en</strong>ttemperatures T = 60 mK (solid) and T = 70 mK (dash). (Middle)Resistance change ∆R = R 70 mK − R 60 mK vs B for the longitudinal(dash) and Hall resistances (solid). (Bottom) RDNMR spectrameasured in R xx and R xy at the magnetic fields indicated above,respectively). All spectra are plotted over a range of 100 kHz.B.A. Piot, D.K. MaudeW. Desrat (GES-UM2, Montpellier), Z. R. Wasilewski (Institute of Microstructural Sci<strong>en</strong>ces, NRC, Ottawa)28


2009 TWO DIMENSIONAL ELECTRON GASSpin splitting <strong>en</strong>hancem<strong>en</strong>t of fully populated Landau levelsThe effect known as “g-factor <strong>en</strong>hancem<strong>en</strong>t” is the promin<strong>en</strong>tmanifestation of electron-electron interactions in thestudy of a two-dim<strong>en</strong>sional electron gas (2DEG) in theregime of the integer quantum Hall effect. This effect isroutinely appar<strong>en</strong>t in magneto-transport experim<strong>en</strong>ts. Theyshow that thermal activation of charged carriers across theFermi <strong>en</strong>ergy located in betwe<strong>en</strong> spin split Landau levels(2DEG at odd filling factors) is ruled by the gap which cansignificantly surpass the so called bare gap expected fromsingle particle band structure models. As far, the effect of g-factor <strong>en</strong>hancem<strong>en</strong>t (at odd filling factors) has be<strong>en</strong> mostlyappar<strong>en</strong>t in experim<strong>en</strong>ts which probed the vicinity of theFermi level. As illustrated in figure. 35, the motivation ofour work was to check whether g-factor is also <strong>en</strong>hancedfor spin split Landau levels located deep below the Fermilevel.We have probed such states with magneto-luminesc<strong>en</strong>ceexperim<strong>en</strong>ts performed on 2DEG confined in aCdTe/CdMgTe quantum well. Focusing on the results oflow temperature experim<strong>en</strong>ts (100 mK) we investigate the<strong>en</strong>ergy positions of σ + and σ − luminesc<strong>en</strong>ce peaks relatedto fully occupied electronic 0th Landau level. The differ<strong>en</strong>ce∆ betwe<strong>en</strong> <strong>en</strong>ergies of these peaks is clearly notmonotonic with the magnetic field in contrast to the lineardep<strong>en</strong>d<strong>en</strong>ce expected wh<strong>en</strong> neglecting the effects ofelectron-electron interactions. As can be deduced fromfigure 36, we find that the oscillatory compon<strong>en</strong>t of ∆ isproportional to the spin polarization of the 2DEG. Notably,∆ = g e f f µ B B wh<strong>en</strong> spin polarization vanishes (at ev<strong>en</strong> fillingfactors). g e f f = 1.3 corresponds well to the combinedelectron-hole bare g-factor in our structure. Effects ofelectron-electron interactions are therefore concluded toaffect the spin splitting of fully occupied Landau levels locateddeep below the Fermi level and not only those in thevicinity of the Fermi <strong>en</strong>ergy.Figure 35: Scheme of Landau levels of a two-dim<strong>en</strong>sional electrongas at ev<strong>en</strong> (6) and odd (5) filling factors. Electron-electroninteraction is known to <strong>en</strong>hance the spin splitting at the Fermi<strong>en</strong>ergy if Landau level filling factor is odd. Enhanced or not<strong>en</strong>hanced spin splitting of fully occupied levels, deep below theFermi level, can be probed with polarization resolved magneto-luminesc<strong>en</strong>ceexperim<strong>en</strong>ts.Figure 36: a,b) Luminesc<strong>en</strong>ce spectra of a 2DEG confined ina 20 nm-wide modulation doped CdTe quantum well at two distinctmagnetic field corresponding to Landau level filling factor 5(a) and 4 (b). Note that spin splitting of the main peak is larger atsmaller field. c) Energy positions of the main σ + and σ − luminesc<strong>en</strong>cepeaks and their separation, ∆ as a function of the magneticfield. Note the increase of ∆ each time the Landau filling is odd.J. Kunc, K. Kowalik, F.J. Teran, P. Plochocka, D.K. Maude, M. PotemskiG. Karczewski, T. Wojtowicz (Institute of Physics, Polish Academy of Sci<strong>en</strong>ces, Warsaw, Poland)29


TWO-DIMENSIONAL ELECTRON GAS 2009Spin polarisation of a disordered GaAs 2D electron gas in a strong in-planemagnetic fieldAn in-plane magnetic field couples to the spins of a 2Dsystem, and can thus be used to probe the impact of manybody effects on the ground state of the 2D electron gas (2-DEG). For example, the longitudinale resistance under parallelmagnetic field g<strong>en</strong>erally exhibits a saturation or a kinkfor a magnetic field B = B p signaling the complete spin polarizationof the 2D system [T. Okamoto et al., Phys. Rev.Lett. 82, 3875 (1999)].pres<strong>en</strong>t in disordered systems and should under no circumstancesbe interpreted as evid<strong>en</strong>ce for a ferromagnetic instability.Using high magnetic fields up to 32 T, we report on the particularlyrich parallel field physics occurring in 2D electrongas in GaAs, revealing an interplay betwe<strong>en</strong> these spin effects,disorder, and orbital effects. The magneto resistancekink usually associated with the 2-DEG complete spin polarizationis observed up to B p ∼ 30 T, and shifts down continuouslyon more than 20 T as the electron d<strong>en</strong>sity (andconsequ<strong>en</strong>tly mobility) is lowered in the sample (see figure37(a). This reduction of B p with decreasing electrond<strong>en</strong>sity is consist<strong>en</strong>t with the predicted electron-electron interaction<strong>en</strong>hancem<strong>en</strong>t of the spin susceptibility at low d<strong>en</strong>sity,favoring the 2-DEG polarization. However, the absolutevalue of B p remains 2-3 times smaller than the one calculatedat T = 0K for a disorder-free system, and extrapolatesto B p = 0 at a relatively “high” electron d<strong>en</strong>sity, wher<strong>en</strong>o ferromagnetic states have ever be<strong>en</strong> observed. We arguethis behaviour is due to the localization of electrons whichare subsequ<strong>en</strong>tly subtracted from the total free carrier d<strong>en</strong>sity[B.A. Piot et al. Phys. Rev. B 80, 115337 (2009)]. Inthis situation the Fermi sea appears effectively smaller andless magnetic field is required to fully polarize the system.This approach is motivated by the strong mobility dropmeasured as the electron d<strong>en</strong>sity is decreased in this veryregion. The temperature dep<strong>en</strong>d<strong>en</strong>ce of B p , which dep<strong>en</strong>dson the effective size of the Fermi sea, corresponds to thepolarization of a smaller Fermi sea, and indicates that thefraction of localized states increases as the electron d<strong>en</strong>sityis reduced. From this temperature behavior, a d<strong>en</strong>sity of delocalizedelectron can be estimated, and used to re-plot theexperim<strong>en</strong>tal B p of figure 37(b) (triangles), giving a betterquantitative agreem<strong>en</strong>t with theory.In summary, the magnetic field at which complete spin polarizationoccurs is dramatically reduced both by electronlocalization and electron-electron interaction <strong>en</strong>hanced atlow carrier d<strong>en</strong>sity. The large value of the extrapolatedcarrier d<strong>en</strong>sity for full spin polarization at zero magneticfield simply reflects the large number of localized electronsFigure 37: (a) Magneto resistance for differ<strong>en</strong>t electron d<strong>en</strong>sities.(b) Field associated with the complete spin polarization B pas a function of the electron d<strong>en</strong>sity (circles and squares), and asa function of the “corrected” electron d<strong>en</strong>sity (triangles). TheoreticalT = 0 K calculations of the magnetic field for full spin polarizationincluding many-body effects: Random Phase Approximation(RPA) [Y. Zhang and S. D. Sarma, Phys. Rev. Lett. 96,196602 (2006)], and Quantum Monte Carlo Calculation (QMC)[A. L. Subasi and B. Tanatar, Phys. Rev. B 78, 155304 (2008)].B.A. Piot, D. K. MaudeU. G<strong>en</strong>nser, A. Cavanna, D. Mailly (<strong>Laboratoire</strong> de Photonique et de Nanostructures, Marcoussis, France)30


2009 TWO-DIMENSIONAL ELECTRON GASHigh-order fractional microwave induced resistance oscillationsResonant transitions of electrons betwe<strong>en</strong> Landau levels(LLs) lead to microwave-induced resistance oscillations(MIROs) whose period is governed by the ratio of the radiationfrequ<strong>en</strong>cy ω to the cyclotron frequ<strong>en</strong>cy ω c = eB/m ∗ ,where m ∗ is the effective mass of electrons. For high microwaveint<strong>en</strong>sity, the resistance has resonant features associatedwith the fractional ratios ε = ω/ω c = n/m where nand m are integers (m ≥ 2). These fractional microwaveinducedresistance oscillations (FMIROs) have be<strong>en</strong> observedup to ε=1/4 and explained by multiphoton absorptionprocesses which appear in the strongly nonlinear regime.The FMIROs are <strong>des</strong>cribed by two theoretical models: asimultaneous absorption of several photons and a stepwisesingle-photon absorption. In both cases the FMIROs correspondingto larger fractional d<strong>en</strong>ominators m (higher-orderFMIROs) appear progressively with increasing MW power.In contrast to the previous studies with low electron d<strong>en</strong>sityand ultrahigh mobility, we investigate high-d<strong>en</strong>sity electrongas with moderate mobilities. The samples are 14 nmwide GaAs quantum wells from differ<strong>en</strong>t wafers. In this reportwe focus on the results for samples with a carrier conc<strong>en</strong>trationn s = 7.8 × 10 11 cm −2 and mobility of 1.2 × 10 6cm 2 /Vs. Figure 38 first pres<strong>en</strong>ts photoresistance for twochoos<strong>en</strong> frequ<strong>en</strong>cies at 1.4 and 6.5 K at a constant MWelectric field. We observed that FMIRO features are betterpronounced wh<strong>en</strong> they are not hindered by Shubnikov-deHaas (SdH) oscillations. Second, FMIROs up to d<strong>en</strong>ominatorm=8 are visible for low frequ<strong>en</strong>cies and all FMIROs arequ<strong>en</strong>ched above 85 GHz. Power dep<strong>en</strong>d<strong>en</strong>ce for FMIROsis close to linear behavior for low MW power and amplitu<strong>des</strong>aturates with increasing MW power [S. Wiedmann etal., Phys. Rev. B 80, 035317 (2009)].observation of high-order FMIROs, see figure 39. Therefore,high-order FMIROs require another explanation.Figure 38: (left) FMIROs for 75 and 66 GHz at temperatures1.4 and 6.5 K at a constant electric field of E=6 V/cm. (right)Frequ<strong>en</strong>cy dep<strong>en</strong>d<strong>en</strong>t photoresistance: for 90 GHz, all FMIROfeatures are qu<strong>en</strong>ched.Theoretical analysis is based on both competing FMIROmodels. The simultaneous absorption model can only accountfor ε = n/2, but is negligible small for high d<strong>en</strong>ominatorm. The stepwise absorption model has constraintsfor experim<strong>en</strong>ts of FMIROs. For the observations of comm<strong>en</strong>surabilityresonances n/m associated with the singlestepwisetransitions betwe<strong>en</strong> adjac<strong>en</strong>t Landau levels (n=1)and in the regime of separated Landau levels [α


TWO-DIMENSIONAL ELECTRON GAS 2009Crossover betwe<strong>en</strong> distinct mechanisms of microwave photoconductivity indouble quantum wellsDouble quantum wells (DQWs) or bilayer electron systemsexposed to microwave (MW) irradiation exhibit a peculiarphotoresistance which can be explained by an interfer<strong>en</strong>cebetwe<strong>en</strong> magneto-intersubband (MIS) oscillationsand microwave induced resistance oscillations (MIROs).The microscopic mechanism <strong>des</strong>cribing the MIROs at lowtemperatures T is associated with a MW-g<strong>en</strong>erated nonequilibriumoscillatory compon<strong>en</strong>t of the electron distributionfunction. The corresponding contribution to magnetoresistanceis proportional to the inelastic scattering timeτ in due to electron-electron scattering and decreases withincreasing temperature according to τ in ∝ T −2 [Wiedmannet al., Phys. Rev. B 78, 121301(R) (2008)].For temperature dep<strong>en</strong>d<strong>en</strong>t measurem<strong>en</strong>ts we have choos<strong>en</strong>the frequ<strong>en</strong>cy range betwe<strong>en</strong> 55 and 140 GHz and we focushere on measurem<strong>en</strong>ts with a fixed frequ<strong>en</strong>cy (85 GHz) at aconstant MW electric field E ω , see figure 40. For these temperatures,Shubnikov-de Haas (SdH) oscillations are completelysuppressed. The amplitude of <strong>en</strong>hanced MIS peaksis not saturated yet for this electric field to <strong>en</strong>sure that weare far away from the saturated regime. The estimated electricfield is E ω ≃ 2.0 V/cm. Figure 40 pres<strong>en</strong>ts the analysisof experim<strong>en</strong>tal data for differ<strong>en</strong>t temperatures up to8 K. The temperature-dep<strong>en</strong>d<strong>en</strong>t quantum lifetime τ q andtransport time τ tr are extracted from dark magnetoresistancemeasurem<strong>en</strong>ts if T e ≃ T . The comparison of experim<strong>en</strong>talmagnetoresistance, see model in [Wiedmann et al.,Phys. Rev. B 78, 121301(R) (2008)], at constant ω andE ω shows that the theoretical temperature dep<strong>en</strong>d<strong>en</strong>ce ofinelastic scattering time τ in ∝ Te−2 fits well up to 3.5 K. Assumingthat τ in = ε F /λ in Te 2 , where λ is a numerical constantof order unity, we can find λ in ≃ 1. Note that theelectron temperature T e is at least 2.8 K (for this choos<strong>en</strong>MW electric field) because of heating of electrons due tomicrowave irradiation (see also figure 41), but for the latticetemperatures T > 3 K the heating effect is negligible,T e ≃ T . By comparing experim<strong>en</strong>t and theory, e.g. figure40(c) at T = 6.0 K for 0.1 T < B < 0.2 T, we see thatthe inverted MIS oscillations are not resolved in the theoreticalplot and we have to introduce an <strong>en</strong>hanced inelasticscattering time τ ∗ in with τ∗ in = 3.5τ in to fit the experim<strong>en</strong>talresults.The deviation starts at T c = 4 K, and for T c > 4 K we obtaina nearly constant τ ∗ in ≃ 190 ps [figure 41]. Similar saturationof τ in with increasing temperature at T ≃ 2 K has be<strong>en</strong>rec<strong>en</strong>tly observed in a one-subband system and attributed toa crossover to the displacem<strong>en</strong>t mechanism of photoresistance[Hatke et al., Phys. Rev. Lett. 102, 066804 (2009)].This explanation is not applicable to our samples becausethe quantum lifetime, according to our estimates, is stillmuch smaller than τ in at T e ∼ 4 K. Our theoretical model,based on inelastic mechanism of MW photoresistance, failsto <strong>des</strong>cribe the obtained oscillation picture for T e > 4 K andfurther theoretical studies of MW photoresistance, possiblyinvolving new mechanisms, are necessary.Figure 40: Temperature dep<strong>en</strong>d<strong>en</strong>ce at 85 GHz up to 8.0 K.Experim<strong>en</strong>tal traces (bottom, black) are fitted to the theoreticalmodel (top, red). With increasing temperature, an <strong>en</strong>hanced inelasticscattering time τ ∗ in (middle, blue) is necessary to fit experim<strong>en</strong>taltraces. SdH oscillations are suppressed for these temperatures.Figure 41: Inelastic scattering time τ ∗ in as a function of electrontemperature T e . Deviation from inelastic mechanism occurs forT e > 4 K, where T -dep<strong>en</strong>d<strong>en</strong>ce of τ in is saturated.S. Wiedmann, J.C. PortalG.M. Gusev (Instituto de Física da Universidade de São Paulo, SP, Brazil), O.E. Raichev (Institute of SemiconductorPhysics, NAS of Ukraine, Kiev, Ukraine), A.K. Bakarov (Institute of Semiconductor Physics, Novosibirsk, Russia)32


2009 TWO-DIMENSIONAL ELECTRON GASEmerg<strong>en</strong>t fractional quantum Hall effect in a triple quantum wellFractional quantum Hall (FQH) effect in a two-dim<strong>en</strong>sional(2D) electron gas is a consequ<strong>en</strong>ce of the exist<strong>en</strong>ce of incompressiblestates at certain fractional filling factors ν ofLandau levels. Bilayer and trilayer systems possess an extradegrees of freedom and this leads to the appearance ofnew FQH states which are not pres<strong>en</strong>t in single layer systems.Such correlated states occur if the interlayer electronelectroninteraction, controlled by the ratio of layer separationto the magnetic l<strong>en</strong>gth, is comparable to the intralayerinteraction. Correlated states have already be<strong>en</strong> discoveredin bilayer systems. In trilayer systems (triple quantumwells, TQWs), correlated states should also exist in acertain interval of parameters determined by the interlayerseparation, electron d<strong>en</strong>sity and the magnetic l<strong>en</strong>gth. Experim<strong>en</strong>tsin low-d<strong>en</strong>sity TQWs have not revealed the statespredicted in [MacDonald, Surf. Sci. 229, 1 (1990)]. A furtheradvance in fractional quantum Hall physics is based onnew many-body ground states in multilayer electron systemswhich are differ<strong>en</strong>t from already studied bilayer systems.In our experim<strong>en</strong>ts we use symmetrically doped GaAsTQWs with a 230 Å wide c<strong>en</strong>tral well and equal 100 Åwide lateral wells coupled by tunneling. The total electronsheet d<strong>en</strong>sity is n s = 9·10 11 cm −2 and the mobility is 4·10 5cm 2 /V s. Here we pres<strong>en</strong>t results with a barrier thicknessof 20 Å. The estimated d<strong>en</strong>sity in the c<strong>en</strong>tral well is 30%smaller than in the side wells. Experim<strong>en</strong>ts have be<strong>en</strong> carriedout in a diluation refrigerator at low temperatures downto T ≃ 50 mK.of the tunneling gap is expected. Now electron motion isconfined into a single layer and correlation of eletrons innearby layers can lead to new states. In fact, wh<strong>en</strong> the sampleis tilted to an angle Θ > 45 ◦ , three new minima occurin R xx and Hall resistance exhibits precursors of the correspondingquantized plateaus. In figure 42(b) we pres<strong>en</strong>tedthe situation where three new fractional states are developed.Within an accuracy of 2%, the plateau at B ⊥ ≃10.2 Tcorresponds to the filling factor ν=10/3. The same effectoccurs for filling factor ν=2 [Gusev et al., Phys. Rev. B 80,161302(R) (2009)].To summarize, the observation of the collapse of integerfilling factors ν=4 and ν=2 and the emerg<strong>en</strong>ce of new FQHstates with increasing in-plane magnetic field can be attributedto new correlated states in a trilayer electron systembecause these states occur wh<strong>en</strong> the in-plane magneticfield suppresses tunneling and multilayer many-body correlationsbecome possible.In order to observe many-body correlations one have toincrease the localization of electrons by applying an inplanemagnetic field. This in-plane magnetic field adds anAharanov-Bohm phase to the tunneling amplitude whichcauses oscillations of the tunnel coupling betwe<strong>en</strong> electronstates in the layers and a suppression of this coupling forlow Landau levels (LLs) [G.M. Gusev et al., Phys. Rev. B78, 155320 (2008)]. This effect, which is a single-particleph<strong>en</strong>om<strong>en</strong>on, can be se<strong>en</strong> in figure 42(a) in the plot of R xxin the tilt angle - perp<strong>en</strong>dicular magnetic field plane for thesecond LL at filling factors ν=7, 9 and 10 which vanish andreappear with increasing tilt angle. In this sample, fractionalquantum Hall states also occur with filling factorsν=17/3, 16/3 and 8/3 up to 15 T.Now, we focus on integer filling factor ν=4 where a completesuppression of the resistance is observed at Θ ≃ 40 ◦whereas the state at ν=5 remains robust with increasingtilt angle. The corresponding parallel magnetic field correspondsto the situation where the expon<strong>en</strong>tial suppressionFigure 42: (a) Longitudinal magnetoresistance in the tilt angle–mag<strong>en</strong>tic field plane for a TQW with a barrier width of 2.0 nm.Minimum for ν=4 is suppressed and three new FQH states occur.(b) Longitudinal and Hall resistance at Θ = 0 ◦ (dashed line) andΘ = 49 ◦ (solid) for T =50 mK.S. Wiedmann, J.C. PortalG.M. Gusev (Instituto de Física da Universidade de São Paulo, SP, Brazil), O.E. Raichev (Institute of SemiconductorPhysics, NAS of Ukraine, Kiev, Ukraine), A.K. Bakarov (Institute of Semiconductor Physics, Novosibirsk, Russia)33


TWO-DIMENSIONAL ELECTRON GAS 2009Re<strong>en</strong>trant fractional quantum Hall states in a triple quantum wellTriple quantum wells (TQWs) consist of three quantumwells separated by thin barriers and can be considered asthree parallel two-dim<strong>en</strong>sional (2D) electron layers coupledby tunneling. The corresponding Landau level (LL)fan diagram for TQWs consists of spin-split LLs separatedby <strong>en</strong>ergy gaps which are <strong>des</strong>cribed by the expressionω c (N + 1/2) ± ∆ Z /2 + E j , where ω c is the cyclotron <strong>en</strong>ergy,∆ Z the Zeeman <strong>en</strong>ergy, and E j ( j = 1,2,3) the <strong>en</strong>ergiesof quantization in the TQW pot<strong>en</strong>tial. Within thetight-binding model [Hanna et al., Phys. Rev. B 53, 15981(1996)] these <strong>en</strong>ergies as well as the corresponding singleelectronwave functions can be estimated. An in-plane magneticfield adds an Aharonov-Bohm phase to the tunnelingamplitude which causes oscillations of the tunnel couplingbetwe<strong>en</strong> electron states in the layers and suppresses the tunnelcoupling for low LLs. Here, we investigate fractionalquantum Hall (FQH) around total filling factor ν=5/2.An interesting behavior is observed in the region betwe<strong>en</strong>filling factors 2 and 5/2, see figure 44. Several new plateausoccur which are abs<strong>en</strong>t for B ‖ =0 T. The exact origin of theemerg<strong>en</strong>t and re<strong>en</strong>trant plateaus at fractional filling factorsis still not clear. We believe that this ph<strong>en</strong>om<strong>en</strong>on involvescorrelation of electron states in several (three) partially populatedsubbands. Further studies are needed to understandthe nature of FQH effect in TQWs.We have studied symmetrically doped GaAs TQWs with a230 Å wide c<strong>en</strong>tral well and equal 100 Å wide lateral wells.The total electron sheet d<strong>en</strong>sity is n s = 9 × 10 11 cm −2 andthe mobility is 4 × 10 5 cm 2 /V s. The estimated d<strong>en</strong>sity inthe c<strong>en</strong>tral well is 30% smaller than in the side wells. Allmeasurem<strong>en</strong>ts have be<strong>en</strong> carried out in a resistive magnetat a temperature of T ≃ 100 mK up to 34 T.Figure 43 pres<strong>en</strong>ts our main observation: the FQH stateν =7/3 first disappears with increasing tilt angle, is th<strong>en</strong> replacedby an emerg<strong>en</strong>t ν = 12/5 state and exhibits a re<strong>en</strong>trancefor Θ = 55 ◦ with a very wide plateau. We explainthis behavior by the influ<strong>en</strong>ce of perp<strong>en</strong>dicular and parallelmagnetic fields. The perp<strong>en</strong>dicular field leads to a consecutivedepopulation of the subbands whereas the parallelcompon<strong>en</strong>t is responsible for a decrease of the subbandgaps due to suppression of tunnel coupling. If tunnel couplingis pres<strong>en</strong>t, we have always gaps betwe<strong>en</strong> subbands.Wh<strong>en</strong> tunnel coupling is cut off by the in-plane field, thedepopulation of the upper subband is accompanied by a decreaseof the separation betwe<strong>en</strong> the upper and the lowersubbands, as a result of modification of the TQW pot<strong>en</strong>tialprofile owing to electron redistribution, until subbands startto overlap. The overlap effect is ess<strong>en</strong>tial for total fillingfactors ν < 5/2. We estimate that the depletion of the uppersubband down to partial filling factor ν 3 = 1/3 correspondsto a strong overlap whereas the depletion to ν 3 = 2/5 correspondsto a weak overlap. This gives rise to a suppressionof ν = 7/3 and the emerg<strong>en</strong>ce of a more favourable plateauat ν = 12/5 but the re<strong>en</strong>trance of ν = 7/3 with increasing tiltangle cannot be attributed within this model, and is possiblyrelated to <strong>en</strong>hancem<strong>en</strong>t of electron-electron correlations bythe parallel magnetic field [Gusev et al., Phys. Rev. B 80,161302(R) (2009)].Figure 43: Longitudinal and Hall resistance for Θ = 0 ◦ (dashed),Θ = 46.3 ◦ (red/gray) and Θ = 55 ◦ (blue/dark grey) pres<strong>en</strong>t re<strong>en</strong>tranceof the FQH state ν=7/3 and the appearance of the emerg<strong>en</strong>tFQH state ν=12/5.Figure 44: Hall resistance R xy as a function of B ⊥ at 100 mKfor differ<strong>en</strong>t tilt angles. Plateau ν=7/3 fist dissappears and is replacedby ν= 12/5 with increasing tilt angle. For Θ = 49.5 ◦ , ν=7/3exhibits re<strong>en</strong>trant behavior. Several new FQH states occur.S. Wiedmann, J.C. PortalG.M. Gusev (Instituto de Física da Universidade de São Paulo, SP, Brazil), O.E. Raichev (Institute of SemiconductorPhysics, NAS of Ukraine, Kiev, Ukraine), A.K. Bakarov (Institute of Semiconductor Physics, Novosibirsk, Russia)34


2009 TWO-DIMENSIONAL ELECTRON GASMagneto-intersubband oscillations in multilayer electron systemsTwo-dim<strong>en</strong>sional (2D) electron systems with several occupiedsubbands exhibit magneto-intersubband (MIS) oscillationsdue to the modulation of intersubband scatteringprobability wh<strong>en</strong> Landau levels of differ<strong>en</strong>t subbands arealigned. In contrast to Shubnikov de Haas (SdH) oscillations,the MIS oscillations are only weakly damped with increasingtemperature. Rec<strong>en</strong>tly, MIS oscillations have be<strong>en</strong>observed and investigated in double quantum well systemswhich consist of two quantum wells coupled by tunneling[Mamani et al., Phys. Rev. B 77, 205327 (2008)]. The finalstep is now a theory g<strong>en</strong>eralized to the multi-subband casewith N layers which is pres<strong>en</strong>ted in this report, experim<strong>en</strong>tallyverified in triple quantum wells (TQWs).We have studied symmetrically doped GaAs TQWs witha total electron sheet d<strong>en</strong>sity n s = 9 × 10 11 cm −2 and mobilitiesof 5 × 10 5 cm 2 /V s. In a perp<strong>en</strong>dicular magneticfield, Landau levels (LLs) pass sequ<strong>en</strong>tially the Fermi <strong>en</strong>ergyand the LL staircase associated with each subband issketched in figure 45(a) as well as a FFT analysis allowingus to extract the corresponding <strong>en</strong>ergy gaps. We havefound ∆ 12 = 4.0 meV, ∆ 13 = 5.4 meV and ∆ 23 = 1.4 meVfor a TQW with d b = 14 Å . The theory is g<strong>en</strong>eralized tothe multi-subband case [Wiedmann et al., to be publishedin Phys. Rev. B (2009)]. Here we pres<strong>en</strong>t the MIS contributionto resistivity (second order quantum contribution).We use a simplified approximation that partial subband occupationsn j , transport scattering rates ν trj j ′ , and quantumlifetimes τ j are equal to each other (τ j = τ q ). Due to hightotal d<strong>en</strong>sity and strong tunnel coupling, this approximationis reasonable for our system. In the regime of classicallystrong magnetic fields, we obtain the magnetoresistance forN=3 in the formρ d (B)ρ d (0) = 1 + 2 [3 d2 1 + 2 ( )3 cos 2π∆12ω c+ 2 ( )3 cos 2π∆13+ 2 ( )]ω c 3 cos 2π∆23, (5)ω cto electron-electron scattering which becomes ess<strong>en</strong>tial forT >2.0 K. The result is in good agreem<strong>en</strong>t with experim<strong>en</strong>talobservations in single or bilayer systems, indicating thatthe s<strong>en</strong>sitivity to electron-electron scattering is the fundam<strong>en</strong>talproperty of magnetoresistance oscillations originatingfrom second-order Dingle factor.Figure 45: Landau level staircase for a three-subband system andpicture of a TQW with three occupied subbands (1,2,3). (b) FFTspectra for the TQW with a barrier thickness of d b = 14 Å .where d = exp(−π/ω c τ q ) is the Dingle factor. This theoreticalmodel is in a good agreem<strong>en</strong>t with our observations andconfirms also the value of the <strong>en</strong>ergy gaps ∆ j j ′. The magnetoresistancein equation (5) is calculated assuming that thescattering pot<strong>en</strong>tial is ess<strong>en</strong>tial only in the side wells sincegrowth technology implies that most of the scatterers residein the outer barriers.In figure 46 we pres<strong>en</strong>t temperature dep<strong>en</strong>d<strong>en</strong>ce of MISoscillations and the extracted averaged quantum lifetime.SdH oscillations are suppressed for T >4.2 K. The behaviorof τ q follows a T 2 -dep<strong>en</strong>d<strong>en</strong>ce and this is attributedFigure 46: (a) Temperature dep<strong>en</strong>d<strong>en</strong>ce of MIS oscillations and(b) extraction of averaged quantum lifetime as a function of temperaturefor samples with d b = 14 Å . For 4.2 K, SdH oscillationsare completely suppressed for B ≤0.6 T.S. Wiedmann, J.C. PortalN.C. Mamani, G.M. Gusev (Instituto de Física da Universidade de São Paulo, SP, Brazil), O.E. Raichev (Institute ofSemiconductor Physics, NAS of Ukraine, Kiev, Ukraine), A.K. Bakarov (Institute of Semiconductor Physics, Novosibirsk,Russia)35


TWO-DIMENSIONAL ELECTRON GAS 2009Interfer<strong>en</strong>ce of fractional microwave induced resistance oscillations withmagneto-intersubband oscillations in a bilayer systemMicrowave induced resistance oscillations (MIRO) whichevolve into “zero resistance states” (ZRS) in high mobilitysamples and for a suffici<strong>en</strong>tly high microwave power arecurr<strong>en</strong>tly both under experim<strong>en</strong>tal and theoretical investigation.They are governed by the ratio of the radiation frequ<strong>en</strong>cyω to the cyclotron frequ<strong>en</strong>cy ω c = eB/m ∗ , wherem ∗ is the effective mass of the electrons. With increasingmicrowave (MW) power, fractional MIROs (FMIROs)are observed which can be <strong>des</strong>cribed by ε = ω/ω c = n/mwith integer n and m and m ≥2. If a double quantum well(DQW) is exposed to microwave irradiation, photoresistancediffers from the single-subband case because of additionalintersubband scattering. MIS oscillations are increased/decreasedor show an inversion (peak flip) for lowfrequ<strong>en</strong>cies. The oscillating magnetoresistance is caused byan interfer<strong>en</strong>ce of the physical mechanisms responsible forthe MIS oscillations and conv<strong>en</strong>tional MIRO, strongly correlatedwith microwave frequ<strong>en</strong>cy. It has also be<strong>en</strong> foundthat the inelastic mechanism explains photoresistance measurem<strong>en</strong>tsin a two-subband system at low temperatures[Wiedmann et al., Phys. Rev. B 78, 121301(R) (2008)].In this contribution we report on experim<strong>en</strong>tal and theoreticalstudies of interfer<strong>en</strong>ce betwe<strong>en</strong> MIS oscillations andFMIROs. In a certain temperature range (8 K


2009 TWO-DIMENSIONAL ELECTRON GASMicrowave photoconductivity in multilayer systems: triple quantum wellsTwo-dim<strong>en</strong>sional (2D) systems exposed to microwave(MW) irradiation in the pres<strong>en</strong>ce of a weak perp<strong>en</strong>dicularmagnetic field have attracted much experim<strong>en</strong>tal andtheoretical interest over the past years. In systems withone occupied subband, the magnetoresistance exhibitsmicrowave-induced resistance oscillations (MIROs), whichare governed by the ratio of the radiaton frequ<strong>en</strong>cy ω tothe cyclotron frequ<strong>en</strong>cy ω c and evolve into “zero-resistancestates” for elevated MW int<strong>en</strong>sity and ultrahigh mobility.MIROs have also be<strong>en</strong> investigated in systems with two occupiedsubbands (double quantum wells, DQWs), wherethe magneto-intersubband (MIS) oscillations are observedin the abs<strong>en</strong>ce of microwave irradition. The MIS resonancesoccur wh<strong>en</strong> differ<strong>en</strong>t Landau levels of the two subbandsare sequ<strong>en</strong>tially aligned by the magnetic field. Themost interesting aspect of two-subband systems is the interfer<strong>en</strong>cebetwe<strong>en</strong> MIROs and MIS oscillations, which leadsto a peculiar magnetoresistance pattern [Wiedmann et al.,Phys. Rev. B 78, 121301(R) (2008)].We pres<strong>en</strong>t in this contribution the interfer<strong>en</strong>ce of MIS andMIROs which is theoretically studied in multilayer electronsystems and experim<strong>en</strong>tally confirmed in high-d<strong>en</strong>sitytriple quantum wells (TQWs). The dissipative resistivity inthe pres<strong>en</strong>ce of MW irradiation is giv<strong>en</strong> byA ω = P ω(2πω/ω c )sin(2πω/ω c )1 + P ω sin 2 . (8)(πω/ω c )In figure 49 we compare symmetrically doped GaAs TQWswith a total electron sheet d<strong>en</strong>sity of n s = 9 × 10 11 cm −2 , amobility of 5×10 5 cm 2 /V s with a c<strong>en</strong>tral well width of 230Å and side wells widths of 100 Å to the theoretical model inequation (7). The barrier thickness is d b = 14 Å. The MWelectric field is slightly varied around 3.2 V/cm.The MIS oscillation picture in TQWs is more complicatedbecause of the pres<strong>en</strong>ce of three subbands with <strong>en</strong>ergiesε j ( j = 1,2,3). The periodicity of the MIS oscillationsis determined by several subband separation <strong>en</strong>ergies∆ j j ′ = |ε j −ε j ′|. Therefore, if such a TQW is exposed to microwaveirradiation, MIS oscillations also change its oscillationpicture, correlated with the radiation frequ<strong>en</strong>cy. Thetheoretical model g<strong>en</strong>eralized to the multi-subband case isin agreem<strong>en</strong>t with experim<strong>en</strong>tal results for N=3.ρ MWd = ρ d + ρ in + ρ di , (6)where ρ d is the dark resistivity. ρ in and ρ di are themicrowave-induced contributions due to inelastic [Dmitrievet al., Phys. Rev. B 71, 115316 (2005)] and displacem<strong>en</strong>tmechanism with the dominance of the inelastic contributionat low temperature because of τ in ∝ T −2 . In a simplifiedapproach and for the case of three layers (N=3), we assumethat the partial d<strong>en</strong>sities n j , transport scattering rates ν trj j ′ ,and Dingle factors d j = e −π/ω cτ j , where τ j is the quantumlifetime for subband j, are equal to each other (d j = d).Th<strong>en</strong>, neglecting the SdH oscillations, one can write themagnetoresistance in the form:ρ d (B)ρ d (0) = 1 + 2 [3 (1 − A ω)d 2 1 + 2 ( )3 cos 2π∆12ω c+ 2 ( )3 cos 2π∆13+ 2 ( )]ω c 3 cos 2π∆23, (7)ω cwhich <strong>des</strong>cribes both the contribution of MIS oscillationsgoverned by the intersubband <strong>en</strong>ergy gaps ∆ j j ′ and modificationof the quantum part of the resistivity by the MWirradiation, giv<strong>en</strong> by a dim<strong>en</strong>sionless factorFigure 49: Measured (upper panel) and calculated (lower panel)photoresistance of a TQW with a barrier thickness of 14 Å exposedto MW irradiation at a lattice temperature of 1.4 K. Thecuvres for 70, 110 and 170 GHz are shifted up for clarity.S. Wiedmann, J.C. PortalN.C. Mamani, G.M. Gusev (Instituto de Física da Universidade de São Paulo, SP, Brazil), O.E. Raichev (Institute ofSemiconductor Physics, NAS of Ukraine, Kiev, Ukraine), A.K. Bakarov (Institute of Semiconductor Physics, Novosibirsk,Russia)37


TWO-DIMENSIONAL ELECTRON GAS 2009Hole cyclotron resonance in a two-dim<strong>en</strong>sional semimetalRec<strong>en</strong>tly a two-dim<strong>en</strong>sional (2D) semimetal was discoveredin undoped HgTe quantum wells (QWs) with (013)surface ori<strong>en</strong>tation. This semimetal exists due to the featureof size quantization in (013) surface ori<strong>en</strong>ted HgTequantum wells with inverted band structure with a thicknessof thickness 18-21 nm. It was established that the <strong>en</strong>ergyspectrum of this system is determined by the overlap(about 10 meV) of the electron <strong>en</strong>ergy dispersion curve witha minimum in the c<strong>en</strong>ter of the Brillouin zone and the val<strong>en</strong>ceband with two maxima along [0-31] direction [Kvon,et al., JETP Lett. 62, 502 (2008)]. It was also shown thatin such QWs a simultaneous exist<strong>en</strong>ce of 2D electrons andholes with d<strong>en</strong>sities of about 10 11 cm −2 and high mobilityof both 2D electrons µ n = (3 − 6) × 10 5 cm 2 /V·s and 2Dholes µ p = (3 − 10) × 10 4 cm 2 /V·s can be realized. So inthis report we pres<strong>en</strong>t the results of the first experim<strong>en</strong>talstudy of hole cyclotron resonance (CR) in a 2D semimetal.Figure 50: Cyclotron resonance of holes: a, photoconductivityG ph vs magnetic field B for three differ<strong>en</strong>t frequ<strong>en</strong>cies of microwaveradiation and b, photoconductivity peak position BCR h vsfrequ<strong>en</strong>cy of microwaves.In the pres<strong>en</strong>t work CR was studied in photoconductivitymeasurem<strong>en</strong>ts. The samples were in Hall bar geometryfabricated on the basis of undoped (013)-grown 20 nmthick Cd x Hg 1−x Te/HgTe/Cd x Hg 1−x Te QWs with x = 0.75.Electron and hole d<strong>en</strong>sities (N s , P s ) and their mobility (µ n ,µ p ) were found from Hall data to have the following valuesin the samples studied: N s = (4 − 5) × 10 10 cm −2 andµ n = (5 − 6) × 10 5 cm 2 /V·s; P s = (1 − 1.3) × 10 11 cm −2and the mobility µ p = (3.5 − 6.6) × 10 4 cm 2 /V·s. TheseHall bars were exposed to microwave irradiation in the frequ<strong>en</strong>cyrange from 80 to 170 GHz. Photoconductivity G phwas measured using modulation technique and in magneticfields up to 6 T and at temperatures from 1.4 K to 4.2 K.Cyclotron resonance in the system studied arises becauseof the heating of 2D electrons or holes caused by a resonantincrease of the absorption of microwave radiation at photon<strong>en</strong>ergies equal to the distance betwe<strong>en</strong> Landau levels.So the dep<strong>en</strong>d<strong>en</strong>cies of the photoconductivity on magneticfield G ph (B) should be a curve with a sequ<strong>en</strong>ce of maximaand minima where the position dep<strong>en</strong>ds on photon <strong>en</strong>ergyand type of carries. In the studied range of microwave frequ<strong>en</strong>ciesand magnetic fields, we resolved cyclotron resonancesfor holes only. CR of electrons was not observedbecause of a considerably smaller effective mass and CRwas situated too close to zero magnetic field. For observationof electrons CR one should use higher microwavefrequ<strong>en</strong>cies.The results of photoconductivity G ph measurem<strong>en</strong>ts areshown in figure 50(a). One can see that measured signalG ph (B) is the wide resonance with a certain maximum atB = 0.83 T for a frequ<strong>en</strong>cy of f = 120 GHz. The dep<strong>en</strong>d<strong>en</strong>ceof the position this maximum on the frequ<strong>en</strong>cy ispres<strong>en</strong>ted in figure 50(b). The hole effective mass foundfrom the positions of the CR peaks is m p = (0.19±0.01)m 0 .This is the first measurem<strong>en</strong>ts of hole effective mass in 2Dsemimetal in HgTe QWs. It is interesting to compare measuredhole mass with electron mass m e = 0.025 × m 0 inthe HgTe metallic state [Kvon, et al., Physica E 40, 1885(2008)]. As expected, hole effective mass is ≈ 7 − 8 timesbigger than electron effective mass.S. Wiedmann, J.C. PortalD. A. Kozlov, Z. D. Kvon, N. N. Mikhailov, S. A. Dvoretsky (Institute of Semiconductor Physics, RAS, Novosibirsk,Russia)38


2009 TWO-DIMENSIONAL ELECTRON GASElectron-Phonon Interactions in a single modulation doped Ga 0.24 In 0.76 As/InPQuantum WellAbsolute magneto-transmission experim<strong>en</strong>ts, as a function decreases an additional interaction sets in (figure 51) andof the magnetic field B up to 13 T, have be<strong>en</strong> performed clearly follows the expected interaction by polaronic effectson a series of single modulation doped Ga 0.24 In 0.76 As/InP with the LO mo<strong>des</strong>. The relative str<strong>en</strong>gth of this interaction,Quantum Well (QW) with a width dw = 10 nm. The carrierconc<strong>en</strong>tration N s is monitored by experim<strong>en</strong>tal condi-mimicked by Im(−1/ε phonon ), is displayed in figure 52.tions from (2 − 4.2) × 10 11 cm −2 with mobilities rangingfrom 10 5 cm 2 /Vs to 2×10 5 cm 2 /Vs respectively. In terms ofphonons the mixed compound Ga x In 1−x As is a two mo<strong>des</strong>ystem with two transverse optical (TO) phonons varyinglinearly with the x cont<strong>en</strong>t betwe<strong>en</strong> those of InAs and GaAswhereas the two longitudinal optical (LO) phonons are coupledby the macroscopic electric field. As such the “longitudinaloscillator str<strong>en</strong>gth” related to the Fröhlich interactionis partly transferred from the lower <strong>en</strong>ergy LO mode to thehigher one (Nash et al. Semicond. Sci. Technol. 2,329(1987)).The transmission spectra are simulated for differ<strong>en</strong>t valuesof B with a multi-dielectric model (Bychkov et al. Phys.Rev. B 70,85306 (2004)). In the simulation process theFigure 51: Variation of δdielectric function of the doped QW is expressed as:0 with the <strong>en</strong>ergy (ω c ) for differ<strong>en</strong>tcarrier conc<strong>en</strong>trations N s in units of 10 11 cm −2 .ω 2 p/dwε xx (ω,B) = ε phonon −ω[ω − (ω 0 − Re(Σ)) + ı(η + Im(Σ))]where ω 2 p, the square of the plasma frequ<strong>en</strong>cy is a functionof N s . ω c = ω 0 −Re(Σ) is the observed cyclotron resonance(CR) frequ<strong>en</strong>cy and δ 0 = η + Im(Σ) the effective dampingparameter. Besi<strong>des</strong> the known dielectric parameters <strong>en</strong>teringinto the expression of phonons for all layers, the only fittingparameters for each value of B are ω c and δ 0 . In the abs<strong>en</strong>ceof any specific interaction, which will give rise to theself <strong>en</strong>ergy Σ(ω), the spectra are well simulated with ω 0 (B)which takes into account non-parabolicity and with thedamping parameter η reflecting the non-resonant interactionwith background impurities. Im(Σ(ω)) and Re(Σ(ω)) Figure 52: Fit of δ 0 − η (blue line) for data with N s = 4.2 × 10 11should be related by the Kramers-Krönig (KK) transformation.We focus this report on the results obtained forcm −2 (red stars). The Imaginary part of the ε phonon and−1/ε phonon are displayed as gre<strong>en</strong> and mag<strong>en</strong>ta lines respectively.the fitted values of δ 0 as a function of the <strong>en</strong>ergy ω c .These results are displayed in Figure 51 for a giv<strong>en</strong> sampleWhereas the simulation with the TO interaction is ratherand differ<strong>en</strong>t carrier conc<strong>en</strong>trations. Whereas δ 0 remainssmall for CR <strong>en</strong>ergies lower than the phonon <strong>en</strong>ergies oftrivial, that with the polaronic effects requires to fit the evolutionof δ 0 at <strong>en</strong>ergies much higher than the LO <strong>en</strong>ergiesGa 0.24 In 0.76 As, it increases noticeably wh<strong>en</strong> <strong>en</strong>tering the<strong>en</strong>ergy range of these phonons.(C. Faugeras et al. Phys. Rev. B 80, 073403 (2009))whichcorrespond to data obtained at higher fields.For the higher N s values, the data can be fitted withIm(ε phonon ) as shown in figure 52 if we increase the broad<strong>en</strong>ingof phonons due to strain effects. This clearly demon-appears to be unique to id<strong>en</strong>tify and ev<strong>en</strong> quantify the dif-Nevertheless, without any further information, this systemstrates that the interaction occurs at the TO mo<strong>des</strong> with fer<strong>en</strong>t types of electron-phonon interactions occurring in athe mechanism of the deformation pot<strong>en</strong>tial. Wh<strong>en</strong> N s quasi-two dim<strong>en</strong>sional electron gas.M. Orlita, C. Faugeras, G. MartinezS. Stud<strong>en</strong>ikin, P. Poole, G. Aers, Institute of Microstructural Sci<strong>en</strong>ces, NRC, Ottawa, Canada39


TWO-DIMENSIONAL ELECTRON GAS 2009Temperature effect on Coulomb pseudogap in electron tunneling betwe<strong>en</strong>Landau-quantized two-dim<strong>en</strong>sional gasesThe pseudogap is common effect for the tunnel structureswith two-dim<strong>en</strong>sional layers. It is revealed as in high-T Csuperconductors so in semiconductor heterostructures. Experim<strong>en</strong>tallya pseudogap is observed as a suppression ofthe tunnel curr<strong>en</strong>t at the low bias voltage [Eis<strong>en</strong>stein etal., Phys. Rev. Lett. 69, 3804 (1992)] or an additionalhigh voltage shift of the resonant curr<strong>en</strong>t peak in the I-Vcurve [Popov et al., JETP, 102, 677 (2006)]. In this cas<strong>en</strong>o signature of the gap is revealed in the lateral electrontransport in the two-dim<strong>en</strong>sional electron gas (2DEG). Theorigin of the pseudogap is still under investigation. For examplethere is an inhomog<strong>en</strong><strong>en</strong>eous model [Fogler et al.,Phys. Rev. B, 54, 1853 (1996)], in which a 2DEG is segregatedon two phases with differ<strong>en</strong>t integer filling factorsdue to the scre<strong>en</strong>ed Coulomb interactions of the electrons.The electron spectrum is very differ<strong>en</strong>t in the each phasedue to the differ<strong>en</strong>t value of exchange <strong>en</strong>hancem<strong>en</strong>t of spinsplittingof the Landau levels (LL). H<strong>en</strong>ce in the averagetunnel spectrum one should to observe two maxima correspondedto the spin-split LL. This model can explain theresonance splitting but not the high-voltage shift of the resonanceobserved in the tunnel junction betwe<strong>en</strong> 2DEGs withdiffer<strong>en</strong>t electron conc<strong>en</strong>trations. In other models the electrontunneling is considered as an instant ev<strong>en</strong>t comparedwith the <strong>en</strong>ergy relaxation of the whole 2DEG. This meansthe tunneling electron should have some extra <strong>en</strong>ergy or <strong>en</strong>ergyof the pseudogap to organize its relaxation. Severaltypes of the collective relaxations had be<strong>en</strong> considered suchas composite fermion scattering and magnetoroton excitations.The schematic conduction-band-bottom diagram of the tunneldiode is shown in the insert (a) in figure 53 with thequantum subband levels in the 2DEGs. The parametersof the 2DEGs are the following: the conc<strong>en</strong>tration of the2DEG with the level E 01 is n 1 = 4×10 11 cm −2 ; the conc<strong>en</strong>trationof the 2DEG with level E 02 is n 2 = 6 × 10 11 cm −2 .The tunnel characteristics were measured at liquid 3 He temperaturesranged from 0.5 K up to 1.5 K. Curr<strong>en</strong>t peakor the second derivative minimum corresponds to the firstcoher<strong>en</strong>t resonance at the bias voltage V r = 6.5 mV, i.e.,E 01 (V r ) = E 02 (V r ). The second derivative maximum atV s = −14 mV associates with the second resonance, i.e.,E 01 (V s ) = E 12 (V s ). In the magnetic field directed perp<strong>en</strong>dicularthe 2DEG planes the resonant features had be<strong>en</strong>shifted in voltage position (see square symbols showing positionsV r in figure 53). This voltage shift consists of twopart: first is the single-particle one that can be <strong>des</strong>cribed inthe single-particle model (see sections of lines in figure 53)and the second part is the pseudogap shift ∆V . The pseudogapshift have be<strong>en</strong> studied at temperature from 0.5 K up to10 K and unexpectable strong temperature dep<strong>en</strong>d<strong>en</strong>ce hasbe<strong>en</strong> revealed at the high magnetic field B > 12 T at lowtemperatures T < 2 K. This can be se<strong>en</strong> from insert (b) infigure 53 where the pseudogap shifts are shown by squaresymbols for T = 1.6 K and by circles for T = 0.5 K. It isinteresting to note that the temperature dep<strong>en</strong>d<strong>en</strong>ce takesplace at the fields wh<strong>en</strong> the cyclotron <strong>en</strong>ergy exceeds theintersubband one. This observation is accompanied by thedecreasing of the pseudogap growth (see insert (b) in figure53) and decreasing of the pseudogap shifts of the elasticreplicas. All this facts point on that the psedogap is forminginflu<strong>en</strong>ced by intersubband plasmons. To date there isno theory considering such kind of effects.Figure 53: Topography map of the second curr<strong>en</strong>t derivative asa function of a bias voltage and magnetic field. The experim<strong>en</strong>talvalues of the resonant voltage V r are shown as squares. Thevalues calculated in the single-particle model are shown as sectionsof lines. In the insert (a) the diagram of the conduction-bandbottom are shown with levels in the quantum wells. The diagramis shown for zero bias and zero <strong>en</strong>ergy corresponds to the Fermilevel. In the insert (b) the pseudogap shift ∆V is plotted versusmagnetic field as squares for T = 1.5 K and circles for T = 0.5 K.S. Wiedmann, J.-C. PortalV.G. Popov (Institute of Microelectronics Technology of RAS, Chernogolovka, Moscow district, Russia)40


2009Semiconductors and Nanostructures41


2009 SEMICONDUCTORS AND NANOSTRUCTURESOn the trigonal field acting at the Cr 3+ ( 2 E states) in RubyAs the magnetic field breaks the time-reversal symmetry,magneto-optical spectroscopy allows to unravel details intransition-metal ions electronic structure by producing effici<strong>en</strong>tlifts of deg<strong>en</strong>eracy. In particular, interaction betwe<strong>en</strong>electronic spin and orbital magnetic mom<strong>en</strong>ts with an appliedmagnetic field B yield a splitting of electronic states,namely the well-known Zeeman effect.Repres<strong>en</strong>tative results are shown in figure 54. In particular,the observed splitting in very high field above 50 T unveilsthe exist<strong>en</strong>ce of two parameters ∆ 1 and ∆ 2 ; the deviation ofthe excited state Landé factor from the value of the groundstate factor g 0 (see figure 55). Under high pressure, thesecoeffici<strong>en</strong>ts exhibit a significant linear increase that unveilsan unexpected increase of the trigonal field under pressure.The relative <strong>en</strong>hancem<strong>en</strong>t of the trigonal field matrix elem<strong>en</strong>t< k| =< t 2g |V tr |t 2g > is 6.2 × 10 −3 /GPa.In fact there are two contributions to the pressure dep<strong>en</strong>d<strong>en</strong>ceof the trigonal crystal-field <strong>en</strong>ergy. The first one isexplicit and positive and scales with the trigonal coordinateQ t , whereas the second term dep<strong>en</strong>ds implicitly on the evolutionof the system s<strong>en</strong>sitivity to the trigonal distortion i.e.on the changes of the coupling parameter with pressure at aconstant Q t value. Crystallographic data under pressure onpure Al 2 O 3 allows to assume that the crystal is homotheticallycontracted and therefore the distortion is reduced as itscales with the a lattice parameter.Figure 54: Typical magneto-photoluminesc<strong>en</strong>ce spectrum at highpressure (5 GPa) and high field (56 T). Eight major peaks (A-H)are recorded. Logarithmic int<strong>en</strong>sity scale <strong>en</strong>hances the visibilityof the four weaker peaks (a-h). (b) Zeeman <strong>en</strong>ergy splitting fanchart highlighting the two pairs of peaks (BC) and (FG) giving directaccess to ∆ 1 and ∆ 2 the intrinsic splitting factor of the excitedstates related to the trigonal field compon<strong>en</strong>t.We have reported high-field magneto-optical measurem<strong>en</strong>tsunder high pressure on ruby single crystals up to 10 GPaand 56 T [Millot et al., Phys. Rev. B 78, 155125 (2008)].Figure 55: Zeeman splitting of ground state and first excitedstates of ruby. Observed emission lines are <strong>des</strong>cribed by allowed(solid arrows) and forbidd<strong>en</strong> (dashed arrows) dipolar absorptiontransitionTh<strong>en</strong> the observed variation is consist<strong>en</strong>t with the pres<strong>en</strong>tmodel and reflects the increase of the trigonal coupling parameterwith pressure, its dep<strong>en</strong>d<strong>en</strong>ce being proportional toR −n with n = 5. This value agrees with the expon<strong>en</strong>t derivedfrom crystal-field theory but in the pres<strong>en</strong>t case is obtainedempirically from magneto-optical spectroscopy, andconstitutes the first experim<strong>en</strong>tal evid<strong>en</strong>ce of a R −5 law.M. Millot, S. George and J.M. BrotoJ. Gonzalez and F. Gonzalez (DCITIMAC, Santander, Spain)43


SEMICONDUCTORS AND NANOSTRUCTURES 2009Mobility spectrum analysis in InN:MgThe mechanism of electrical conductivity and the possibleoccurr<strong>en</strong>ce of superconductivity in InN remains the subjectof considerable controversy. All rec<strong>en</strong>t Hall measurem<strong>en</strong>tsof InN samples doped with Mg or Be acceptors give a signfor the Hall voltage appropriate for electrons. This anomalousresult is presumably due to the pres<strong>en</strong>ce of an n-typesurface inversion layer. One of the method used to detectthe expected pres<strong>en</strong>ce of multi-carrier conduction in theInN system is the measurem<strong>en</strong>t of the resistivity t<strong>en</strong>sor as afunction of magnetic field to perform a quantitative mobilityspectrum analysis. In the case of InN:Mg such an analysisshould in particular give the signs of the contributionsoriginating from electrons and holes if both are pres<strong>en</strong>t.However, in the case of InN:Mg this is a chall<strong>en</strong>ging measurem<strong>en</strong>tsince the mobility of holes is probably very lowand comparable with that of the surface electrons. In addition,the samples are inhomog<strong>en</strong>ous and unfortunately, theycan be measured only in the van der Pauw configurationbecause etching of InN samples to produce Hall bars stillposes a problem. All this makes it difficult to obtain preciseabsolute values of the ρ xx and ρ xy resistivity compon<strong>en</strong>ts,which is indisp<strong>en</strong>sable for a reliable mobility spectrumanalysis. Moreover, ev<strong>en</strong> for strictly n-type samplesthere oft<strong>en</strong> appears in the mobility spectrum the so called“ghost holes” which can lead to errors in the interpretationof the results. Thus, an appearance of a hole peak in themobility spectrum is not necessarily a reliable signature ofthe real pres<strong>en</strong>ce of holes in a sample.peak is higher than electron peak revealed a positive signfor the thermopower). It also agrees very well with the conclusionthat only for moderate Mg cont<strong>en</strong>t can free holesreally be detected in InN:Mg, while for higher doping theformation of donor-like defects (in agreem<strong>en</strong>t with amphotericdefects model) makes the sample progressively moreand more n-type.Figure 56: Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of a resistivity t<strong>en</strong>sor compon<strong>en</strong>tsρ xx and ρ xy of the E1053 sampleWe have performed a systematic investigation of 11InN:Mg samples with Mg-doping from 6 × 10 18 cm −3 to7.3 × 10 20 cm −3 together with 3 undoped (n-type) InN refer<strong>en</strong>cesamples. Our previous preliminary measurem<strong>en</strong>tswith two van der Pauw configurations and magnetic fieldup to 19 T showed hole peaks in mobility spectrum analysisbut it was problematic to find a reasonable correlationbetwe<strong>en</strong> the mobility spectra and the nominal Mg-doping.Our rec<strong>en</strong>t measurem<strong>en</strong>ts show that only all possible permutationsof configurations of curr<strong>en</strong>t and voltage probesand both polarities of the magnetic field up to 28 T givesreliable results. Figure.56 pres<strong>en</strong>ts typical ρ xx and ρ xytraces as a function of the magnetic field. In figure 57 wepres<strong>en</strong>t the results of mobility spectrum analysis for a seriesof samples with increasing Mg cont<strong>en</strong>t (from 6 × 10 18to 4.2×10 20 cm −3 ) for the samples E1003 to E1041 respectively).The obtained series of spectra correlates well withthe measurem<strong>en</strong>ts of thermoelectric power performed onthe same set of samples (only sample E1053 for which holeFigure 57: Mobility spectrum analysis of a series of InN:Mg sampleswith increasing Mg cont<strong>en</strong>t (from E1053 to E1041, respectively).D.K. MaudeL. Dmowski (Institute of High Pressure Physics, Warsaw), L.Konczewicz (GES-UM2, Montpellier), M.Baj (Institute ofExperim<strong>en</strong>tal Physics, University of Warsaw)44


2009 SEMICONDUCTORS AND NANOSTRUCTURESCyclotron effective mass measurem<strong>en</strong>ts in Indium NitrideAmong the group III-nitride materials, the electronic structureof InN is matter of continuing debate <strong>des</strong>pite significantprogress during the last decade in understandingthe band structure, as the revision of its band gap <strong>en</strong>ergyfrom 1.8 − 2.1 eV to 0.7 eV. So far, band parameters aremostly derived from indirect methods of limited accuracysuch as infrared reflectivity measurem<strong>en</strong>ts. For instance,the values of the effective mass remain scattered in a widerange from 0.044 m 0 to 0.093 m 0 . Moreover, a stronglyanisotropic electronic structure of the bulk crystal has be<strong>en</strong>claimed to explain Shubnikov-de-Haas (SdH) oscillationsand magneto-optical properties. To date, the synthesis ofhighly pure InN single crystals remains a chall<strong>en</strong>ge and, inaddition, most measurem<strong>en</strong>ts are affected by the pres<strong>en</strong>ceof an intrinsic low mobility surface and/or interface electronaccumulation layer that op<strong>en</strong>s parallel conduction channels.an isotropic electron-LO phonon coupling constant in InN,α = 0.22, the polaron mass ism ∗ P = m∗ P= (1 + α/12)/(1 − α/12). (10)m∗ One finds a 4% correction that finally gives the bare massat the bottom of the conduction band equal to m ∗ 0 = 0.055±0.002 m 0 . The band parameter E p in the dispersion relation(1) thus becomes E p = 12 eV , with E g = 0.69 eV.We have rec<strong>en</strong>tly performed the first measurem<strong>en</strong>t of thebulk electron cyclotron effective mass by Landau levelsspectroscopy: the most direct approach to measure effectivemasses. To derive the mass, we have used the temperaturedep<strong>en</strong>d<strong>en</strong>ce of the SdH oscillation amplitu<strong>des</strong> measuredunder magnetic field up to 60 T in the temperaturerange 2 − 70 K. A set of InN samples 1 µm thick havingHall conc<strong>en</strong>trations 2 − 3 − 6 × 10 18 cm −3 has be<strong>en</strong> investigated.We found an isotropic electron cyclotron effectivemass equal to 0.062 ± 0.002 m 0 but the highest doped sampleexhibits a puzzling anisotropy.In the pres<strong>en</strong>t study, we find a single SdH series (see figure58) for magnetic field parallel to the c-axis in contrastwith [Inushima et al, Phys. Rev. B 72, 085210(2005)] where an additional SdH series at higher frequ<strong>en</strong>cyis reported for a sample with a similar Hall conc<strong>en</strong>trationn H = 2.2 × 10 18 cm −3 . Our single series behaves like themain series of this previous study and keeps the same periodwh<strong>en</strong> the magnetic field is tilted towards a direction perp<strong>en</strong>dicularto the c-axis. Consequ<strong>en</strong>tly, this series accounts foran isotropic bulk Fermi surface as stated in this work. Onthe other hand since 2D-surface accumulation series are notevid<strong>en</strong>ced, one may suggest that the surface electrons havea low mobility that broad<strong>en</strong>s the 2D-Landau levels and/orinhomog<strong>en</strong>eous electron conc<strong>en</strong>tration causing Fermi levelfluctuations that washes out the oscillations.Taking into account non-parabolicity corrections the bottomband effective mass is[m ∗ 0 = m ∗ 1 − E ]F( m∗− 1) 2 , (9)E g m 0and takes the value m ∗ 0 = 0.057 m 0. Another correction tobe tak<strong>en</strong> into account is the polaron contribution. AssumingFigure 58: (a) Resistance versus magnetic field for the three samplesS1, S2 (left scale) and S3 (right scale) measured at 2 K. (b)SdH oscillations versus reciprocal magnetic field obtained fromthe magnetoresistance curves; a parabolic back-ground contributionhas be<strong>en</strong> subtracted and all curves have be<strong>en</strong> shifted verticallyfor clarity. (c) Temperature dep<strong>en</strong>d<strong>en</strong>ce of the oscillation amplitudefor SdH peaks with N = 3 and N = 4 Landau level index(sample S1)To summarize, electron cyclotron effective mass of InN onc-sapphire substrate is obtained from the temperature dep<strong>en</strong>d<strong>en</strong>ceof Shubnikov-de Haas oscillations. An isotropiccyclotron effective mass equal to 0.062 ± 0.002 m 0 is measuredfor samples having bulk electron conc<strong>en</strong>tration in therange 1 − 4 × 10 18 cm −3 . After non-parabolicity and polaroncorrections, the effective mass at the bottom of theband is found to be m ∗ 0 = 0.055 m 0 ± 0.002.J.M. Poumirol, M. Millot, M. Goiran and J. LeotinW. Walukiewicz (Lawr<strong>en</strong>ce Berkeley <strong>National</strong> Laboratory, Berkeley, USA) and I. Gherasoiu (RoseStreet Labs Energy,Pho<strong>en</strong>ix, USA)45


SEMICONDUCTORS AND NANOSTRUCTURES 2009Oscillatory magneto-absorption under pressure in Indium Sel<strong>en</strong>ideIndium sel<strong>en</strong>ide is a layered semiconductor widely investigatedin the last deca<strong>des</strong> for its pot<strong>en</strong>tial optoelectronic applicationscharacterized by an anisotropic anomalous bandstructuredue to the balance betwe<strong>en</strong> coval<strong>en</strong>t and van derWaals bonds. Various experim<strong>en</strong>ts have revealed a puzzlingbehavior for the electron effective mass.Modern ab-initio band structure calculations by NAO-DFTcombined with optical measurem<strong>en</strong>ts under high pressurehave explained this anomaly and have also unveiled newinteresting features such as the onset of a ring-shaped val<strong>en</strong>ceband maximum above 2 GPa. In fact, a specific k.pmodel has rec<strong>en</strong>tly be<strong>en</strong> proposed for this class of layeredsemiconductors [Segura et al., Phys. Stat. Solidi B 235(2),267276 (2003)].Oscillatory magneto-absorption spectroscopy measurem<strong>en</strong>tsunder high pressure yield a very deep insight intothe unusual electronic properties of this compound. We obtainedfor the first time clear signature of the Landau quantizationin a wide <strong>en</strong>ergy range above the fundam<strong>en</strong>tal gap,giving access to the conduction band non-parabolicity (figures59 and 60). In addition, the high field regime for theexcitonic feature has be<strong>en</strong> studied.The pressure dep<strong>en</strong>d<strong>en</strong>ce of the magneto-fingerprints unveilan increase of the reduced effective mass similar withthe evolution of the second gap transition, which confirmsthe main hypothesis of the specific k.p model. Moreover,the re<strong>en</strong>trant behavior of the pressure-qu<strong>en</strong>ched excitonpeak under high magnetic field (figure 61) unveils anunusual ring-shaped val<strong>en</strong>ce band maximum with a smallhole effective mass as suggested by previous transport experim<strong>en</strong>tsunder pressure and ab-initio calculations.Figure 59: Oscillatory magneto-absorption spectroscopy colorplot of InSe measured at 4 K up to 53 T. The excitonic groundstate feature is clearly distinguishable around 1.34 eV as well asinterband Landau level transition which <strong>en</strong>ergy increases linearlywith the applied magnetic field.Using a toy model taking into account a linear Landau gapop<strong>en</strong>ing and the reported pressure dep<strong>en</strong>d<strong>en</strong>ce of the val<strong>en</strong>ceband maxima and conduction band minima form previousoptical measurem<strong>en</strong>ts under pressure we can estimatethe hole mass on the secondary maximum to be ∼ 0.03 m 0 .Figure 60: Interband Landau fan chart recorded in the diamondanvil cell.Figure 61: Re<strong>en</strong>trant behavior of the pressure-qu<strong>en</strong>ched excitonpeak under high magnetic field. This unveils an unusualring-shaped val<strong>en</strong>ce band maximum with a small hole effectivemass.M. Millot, S. George and J.M. BrotoA. Segura (ICMUV, Val<strong>en</strong>cia, Spain)46


2009 SEMICONDUCTORS AND NANOSTRUCTURESMagnetoresistance in β-FeSi 2 on n-type Si substratesHall bars consisting of 30nm of FeSi were deposited by DCmagnetron sputtering at 30 W in a high vacuum onto nativeoxide Si (001) on to n-type phosphorous doped Si substrateswith 1-10 Ω resistivity. Post deposition the films were annealedfor 10 hours at 850 ◦ C . At these temperatures withthe breakdown of the native oxide, the film harvested theunderlying Si. X-ray diffractometry confirmed β-FeSi 2 asthe final stable phase upon the substrate. Once this wasconfirmed, Cu top electro<strong>des</strong> were deposited, also definedusing shadow masking during sputtering. The resistance ofthe bilayer structure was measured using standard 4 wirelock-in techniques in magnetic fields, H, up to 22 T. Themagnetoresistance, MR=∆R/R, was th<strong>en</strong> calculated fromthe following equation:A similarly large positive MR has be<strong>en</strong> observed in borondoped Si [Schoonus et al., Phys. Rev. Lett., 100, 127202(2008)]. This effect has be<strong>en</strong> attributed to autocatalytic impactionisation in the Si. They observe isotropic MR unlikethe MR in our system. All data displayed is in the transversefield (magnetic field perp<strong>en</strong>dicular to the curr<strong>en</strong>t direction),wh<strong>en</strong> the curr<strong>en</strong>t and magnetic field direction concura smaller effect is measured.∆RRR(H) − R(0)= , (11)R(0)Figure 63: MR at the crossover betwe<strong>en</strong> conduction through thefilm and substrate. Above 20 K an external magnetic field increasesthe substrate resistance until it becomes comparable to thefilm at which point the relatively smaller MR in the film is observed.At 14.4 K it is assumed that all conduction is through theβ-FeSi 2 and 11 % MR is measured.Figure 62: MR of the bilayer, the peak MR, arising from the Sioccurs at ∼45K. Below this temperature the β-FeSi 2 layer resistanceis lower than the Si and with the change in curr<strong>en</strong>t path theMR t<strong>en</strong>ds to plateau.At high temperatures the resistance of the film far exceededthat of the substrate, therefore the majority of the curr<strong>en</strong>tshunted through the substrate. At these temperatures themagnetoresistance of the doped Si substrate is appar<strong>en</strong>t.This large positive MR has rec<strong>en</strong>tly observed in phosphorousdoped silicon [Delmo et al., Nature, 457, 1112 (2009)],explained in terms of breaking of the space charge effect.The extraordinarily large MR saturates as the substrate resistancecompares to that of the film. Figure 62 illustratesthe MR in the doped Si. This MR increases with decreasingtemperatures until the majority of the conduction is throughthe β-FeSi 2 film. At low temperatures (∼25 K) the Si substrateresistance exceeds the film and it can be assumed thatconduction is predominantly directed through the β-FeSi 2layer. This is demonstrated in figure 63, suggesting thecrossover betwe<strong>en</strong> the two regimes. The large MR of theSi underlayer is increased by the external magnetic field.As this resistance exceeds begins to exceed that of the filmonly the MR inher<strong>en</strong>t to the β-FeSi 2 layer is observed. Theexternal magnetic field creates a non linear Hall effect thatwas measured simultaneously to the MR. The non-linearityis most pronounced below 30K where the high magneticfields, and large MR of the doped Si causes the conductionpath to change.D. K. MaudeN. A. Porter, C. H. Marrows, (School of Physics and Astronomy, University of Leeds, Leeds, UK, LS2 9JT),47


SEMICONDUCTORS AND NANOSTRUCTURES 2009Two-dim<strong>en</strong>sional weak localization in polycrystalline granular SnO 2 filmsThe ph<strong>en</strong>om<strong>en</strong>on of quantum interfer<strong>en</strong>ce in disorderedconductors is well known and its effects on the electricalconductance are widely used to determine the inelasticscattering time of charge carriers, and thus, the mechanismsof inelastic scattering. Because of the promin<strong>en</strong>teffects of weak localization in 2D systems they became anobject of int<strong>en</strong>sive studies. However, the reduced dim<strong>en</strong>sionalityand the pres<strong>en</strong>ce of disorder lead not only to <strong>en</strong>hancem<strong>en</strong>tof interfer<strong>en</strong>ce effects, but also to the necessityto take into account the electron-electron interaction. It appearedthat such characteristics as d<strong>en</strong>sity of states, temperatureand magnetic field dep<strong>en</strong>d<strong>en</strong>cies of electrical conductancecould be <strong>des</strong>cribed only if one takes into accountthe effects of electron-electron interaction in a disorderedlow-dim<strong>en</strong>sional system [Altshuler and Aronov, Modernproblems in cond<strong>en</strong>sed matter sci<strong>en</strong>ces Vol 10, Efros andPollak. ed., North Holland 1985]. Moreover, the dephasingmechanisms in weak localization are strongly relatedto interaction effects; inelastic electron-phonon scattering,quasi-elastic electron-electron scattering with small <strong>en</strong>ergytransfer. The interplay of interfer<strong>en</strong>ce and interaction effectsremains a puzzling problem that is still far from beingsolved.(2006)] where the weak localization model is ext<strong>en</strong>ded beyondthe diffusion limit. In the frame of this model, onlysmall closed loops are believed to give contribution to theeffect of weak localization at such high magnetic fields, theminimum number of collisions in each loop being 3. Onecan suppose that relative to electron-electron interaction effects,these triangles should be easier to study rather thanany complicated electronic path with a large number of collision.As in many materials the dephasing in the weak localizationeffect was found to be due to electron-electroninteractions, the study of these materials in high magneticfields should provide important information about these interactions(single electron’s wave function interfer<strong>en</strong>ce is<strong>des</strong>troyed, so the interaction effects should give the maincontribution to magnetoconductance).In our SnO 2 polycrystalline films the low transverse magneticfield dep<strong>en</strong>d<strong>en</strong>ce of the conductance is positive andcan be <strong>des</strong>cribed in the frame of a 2D weak localizationmodel, the phase breaking mechanism being electronelectronscattering with small <strong>en</strong>ergy transfer.In figure 64, the dep<strong>en</strong>d<strong>en</strong>ce of the magnetoconductance onthe normalized magnetic field B/B ϕ , measured on the samesample, are pres<strong>en</strong>ted over the full range of applied magneticfield up to 50 T. Here, B ϕ is the value of magnetic fieldat which the flux of magnetic field through an area <strong>en</strong>closedby the electron’s paths becomes equal to the flux quantumh/2e. From both the inset, where the curves are pres<strong>en</strong>tedin linear coordinates, and from the main part of figure 64,one can see that at high fields the curves exhibit differ<strong>en</strong>tbehaviour and no longer overlap any more. We thus suggestthe necessity to take into account the anisotropy ofthe scattering pot<strong>en</strong>tial in order to <strong>des</strong>cribe the observedresults. Differ<strong>en</strong>t particularities of single scattering ev<strong>en</strong>tsmay have influ<strong>en</strong>ce at differ<strong>en</strong>t temperatures in this highfield region.The experim<strong>en</strong>tal curves in figure 64 resemble those derivedby Zduniak et al. [Phys. Rev. B 56, 1996 (1997)]and by German<strong>en</strong>ko et al. [Phys. Rev. B 73, 233301Figure 64: The magnetic field dep<strong>en</strong>d<strong>en</strong>cies of magnetoconductanceas a function of normalized magnetic field. Inset shows fielddep<strong>en</strong>d<strong>en</strong>cies of magnetoresistance in linear coordinates measuredon the same sample.The analysis of high-field magnetoresistance data, obtainedon our samples of SnO 2 polycrystalline thin films, will provideanother one possibility to justify the mechanism ofelectron-electron interaction in disordered systems. The advantageof our samples is in highly controllable degree ofdisorder, which provi<strong>des</strong> possibility to tune the range of occurr<strong>en</strong>ceof quantum interfer<strong>en</strong>ce under applied magneticfields.T. A. Dauzh<strong>en</strong>ka, J. GalibertV. K. Ks<strong>en</strong>evich (Belarus State University, Dept Phys. SC & Nanoelectronics, BY-Minsk), I.A. Bashmakov (BelarusState Univ. Research Institute of Physicochemical Problems, BY-Minsk)48


2009 SEMICONDUCTORS AND NANOSTRUCTURESMagnetoresistance mobility extraction in FinFET triple gate devicesWe have applied the geometric magnetoresistance (MR)technique to FinFET devices. The geometric µ MR mobilityis give by ρ(B) = ρ 0 (1 + µ 2 MR B2 ) where ρ 0 is the zeromagnetic field (B = 0) resistivity. The devices studied inthis work are triple-gate FinFET from IMEC in Belgium.The devices characteristics used are: oxide thickness of2 nm (EOT), fin height of 60 nm, channel width (W f in )of 10µm, the channel l<strong>en</strong>gth (L) varies from 90 − 910 nm.The electrical characteristics were acquired using a semiconductorparameter analyzer (HP 4156A) measuring thedrain curr<strong>en</strong>t-voltage I D (V G ) curves at differ<strong>en</strong>t magneticfields, low temperatures and for low drain bias (linear region:V DS = 50 mV) in order to compute the µ MR . Thismethod works for transistor l<strong>en</strong>gth much smaller than thewidth (typically W/L > 5).Another problem with the use of short devices at low temperaturesis the series resistance effect. Figure66(b) showsthat there is a reduction of the mobility with decreasingchannel l<strong>en</strong>gth, while for long channels, the phonon scatteringis dominant. However, it is noted that the mobility increasesis att<strong>en</strong>uated for shorter devices, owing to the largeseries resistance, which masks the mobility <strong>en</strong>hancem<strong>en</strong>t atlow temperature.In order to obtain the µ MR , we plot the µ MR resistance ratioR(B)/R 0 for various values of V G as a function of B 2as shown in figure 65 for typical transistor with a channell<strong>en</strong>gth of 410 nm, fin width of 10µ m at T = 100 K. Theother devices measured pres<strong>en</strong>t the same behaviour.From the slope of this curve, for each applied gate voltageV G , the mobility µ MR can be calculated. The mobility µ MR isplotted as a function of V G in figure 66(a). In order to makea comparison, we also plott the variations of effective mobilityµ e f f and field-effect mobility µ FE . These curves havebe<strong>en</strong> calculated by taking µ FE = gm/((W/L)C ox V D ) andµ e f f = √ µ 0 − µ FE at B = 0. The low electric-field mobilityµ 0 were extracted using Y (V G ) = I D / √ gm(V G ), whichallows us to eliminate the first-order mobility att<strong>en</strong>uationfactor and source-drain series resistance effects [Ghibaudo,Electron Lett. 24, 543 (1988)]. While here we pres<strong>en</strong>t resultsfor one transistor at one temperature, for all the transistorsmeasured, at three differ<strong>en</strong>t temperatures (77K, 100Kand 200K), same behaviour was observed.Figure 65: µ MR ratio R(B)/R 0 in function of square of magneticfield for differ<strong>en</strong>t values of gate bias. The symbol line repres<strong>en</strong>tsthe “intrinsic” mobility ratio µ 0 (0)/µ 0 (B) extracted from the Y–function. For L = 410 nm and T = 100 K.In figure 65 we plot the low-field mobility ratioµ 0 (0)/µ 0 (B) as a function of B 2 that was extracted by thestandard relation µ 0 (B) = µ 0 /(1+µ 2 0,MR B2 ). From the slopeof these lines it is possible to extract the low-field MR mobilityµ 0,MR (figure 66 (b) that is indep<strong>en</strong>d<strong>en</strong>t of both thegate bias and the magnetic field.Figure 66(b) shows the µ 0,MR and µ 0 for transistors as afunction of the channel l<strong>en</strong>gth, for differ<strong>en</strong>t temperatures.µ 0,MR is higher than µ 0 for all temperatures. As the temperaturedecreases there is an increase in the mobility dueto the reduced phonon scattering [Ohata, ESSDERC 2004,109 (2004)].Figure 66: a)Variations of µ MR mobility, effective mobility andfield effect mobility (corresponding to a zero magnetic field) versusgate voltage. For L = 410 nm and T = 100 K. b) Low-field mobilityµ 0 and low-field, MR mobility µ 0,MR versus channel l<strong>en</strong>gthat differ<strong>en</strong>t temperaturesD.K. MaudeC. D. G. dos Santos , J. A. Martino (EPUSP- Escola Politécnica da Universidade de São Paulo, São Paulo, Brazil), S.Cristoloveanu (IMEP, Gr<strong>en</strong>oble, France)49


SEMICONDUCTORS AND NANOSTRUCTURES 2009Spin polarization of carriers in a GaAs/GaAlAs resonant tunneling diodeSpin polarized carrier systems are of interest particularlywith a view to polarized spin injection for giant magnetotoresistance(GMR) devices and spintronics applications.However, for various physical reasons, spin polarized injectionis in g<strong>en</strong>eral difficult to achieve in real devices. Herewe show that it is possible to monitor the spin polarizationof carriers throughout a resonant tunneling dio<strong>des</strong> using polarizationresolved micro-photoluminesc<strong>en</strong>ce.We have investigated the spin polarization of carriersin asymmetrical n-i-n GaAs/GaAlAs resonant tunnelingdio<strong>des</strong> (RTD) by analyzing the polarized resolved photoluminesc<strong>en</strong>cefrom both GaAs quantum well (QW) and contactlayers under applied voltage and magnetic field. Forthe measurem<strong>en</strong>ts a micro-photoluminesc<strong>en</strong>ce setup with alow temperature x − y − z displacem<strong>en</strong>t stage was used tosimultaneously perform transport and photoluminesc<strong>en</strong>ceon single RTD etched mesa structure. Figure 67 shows aschematic band diagram of our device under forward biasvoltage, light excitation, and magnetic field parallel to thetunnel curr<strong>en</strong>t. Under applied bias, the photo-g<strong>en</strong>eratedholes from the top contact can tunnel through the structureand recombine with electrons into the QW and contact layers.Figure 68 pres<strong>en</strong>ts typical polarized resolved photoluminesc<strong>en</strong>cespectra at 0.195 V bias voltage. The higher <strong>en</strong>ergyemission peak (∼ 1.605 eV) is attributed to the fundam<strong>en</strong>talquantum well (QW) transition whereas the emissionaround 1.52 eV is due to various optical transitions in thecontact layers including the indirect recombination betwe<strong>en</strong>free holes and electrons in the two dim<strong>en</strong>sional electron gas(h-2DEG) formed at the accumulation layer (∼ 1.512 eV).charge d<strong>en</strong>sity, filling factors and spin polarization of thetwo-dim<strong>en</strong>sional gas formed in the accumulation layer.Figure 67: Schematic band diagram of our device under forwardbias, light excitation and magnetic field parallel to the tunnel curr<strong>en</strong>t.Figure 68: A repres<strong>en</strong>tative photoluminesc<strong>en</strong>ce spectra from theQW and contact layers measured at B = 19 T and T = 4.2 K.In a magnetic field the photoluminesc<strong>en</strong>ce from the QWand contact layers shifts to higher <strong>en</strong>ergies and shows oscillationsin int<strong>en</strong>sity (not shown). Figure 69 shows themagnetic field dep<strong>en</strong>d<strong>en</strong>ce of circular polarization degreefrom the QW, contact layers (total PL spectra) and fromthe h-2DEG emission. The polarization of the carriers,P = (I σ+ −I σ− )/(I σ+ +I σ− ), can be obtained from the integratedint<strong>en</strong>sity of the polarization resolved photoluminesc<strong>en</strong>ce.We have observed that the QW emission pres<strong>en</strong>tsnegative polarization degree up to 55% which oscillateswith magnetic field. A similar behavior is observed for theemission from the GaAs contact layers.To further understand this data we are curr<strong>en</strong>tly in the processof modeling the spin polarization of carriers in thestructure taking into account the carrier tunneling, carrierFigure 69: Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of spin polarization of theQW, GaAs contact layers and from the h-2DEG emissions.J. Kunc, M. Orlita, D. K. MaudeY. Galvão Gobato, L.F. dos Santos (Federal University of São Carlos, Brazil), M. H<strong>en</strong>ini (School of Physics and Astronomy,University of Nottingham, UK)50


2009 SEMICONDUCTORS AND NANOSTRUCTURESSpectroscopy and optical manipulation of a single Mn spin in a CdTe-basedquantum dot in high magnetic fieldQuantum dots containing single magnetic ions have rec<strong>en</strong>tlyattracted significant interest as systems close to theultimate limit of information storage miniaturization. Aneffici<strong>en</strong>t optical read-out of the Mn spin state has be<strong>en</strong>demonstrated [Besombes et al., Phys. Rev. Lett. 93,207403 (2004)] as well as the writing and storing of theinformation using the Mn spin state. It has be<strong>en</strong> shown thatit is possible to optically manipulate the single Mn spin byinjecting the spin-polarized excitons into the quantum dot,either by direct quasi-resonant excitation of the dot with circularlypolarized light [Le Gall et al., Phys. Rev. Lett. 102,127402 (2009)] or by using a spin-conserving transfer ofthe excitons betwe<strong>en</strong> two coupled quantum dots [Goryca etal., Phys. Rev. Lett. 103, 087401 (2009)].We have applied the micro-photoluminesc<strong>en</strong>ce measurem<strong>en</strong>tsto directly probe states of a single Mn atom embeddedin a CdTe quantum dot in high magnetic fields.The sample was placed in a micro-photoluminesc<strong>en</strong>ce setupconsisting of precise piezo-electric three-dim<strong>en</strong>sional stageand a microscope objective. The micro-photoluminesc<strong>en</strong>cesystem was kept at the temperature of 4.2 K in a cryostatplaced in a resistive magnet producing magnetic field up to28 T. The field was applied parallel to the the growth axisof the sample (Faraday configuration).Figure 70: Color-scale plot of the photoluminesc<strong>en</strong>ce int<strong>en</strong>sityof a single Mn-doped QD as a function of emission <strong>en</strong>ergy andmagnetic field. The branches of emission lines can be assigned tobright (X) and dark (DX) exciton transitions.The photoluminesc<strong>en</strong>ce of the QD’s was excited by circularlypolarized tunable dye laser in the range 570−610 nm.The excitation beam and the collected PL signal werepassed though a mono-mode fiber connected directly to themicroscope objective. Optical spectra have be<strong>en</strong> recordedfor both circular polarization of light.An example of the PL measurem<strong>en</strong>t of a neutral excitonspectrum of a single Mn-doped QD as a function of themagnetic field is shown in figure 70. It reveals not only detailsof the optical transitions of the so called bright excitons(excitons with J = 1), but also transitions of dark excitons(J = 2) are clearly visible (5 lines in the low <strong>en</strong>ergy partof the spectra). This is due to the mixing of electron spinstates by electron-Manganese exchange interaction and opticalori<strong>en</strong>tation of the spin of the Mn ion.Calculated excitonic transitions in a dot containing a singleMn ion is shown in figure 71. It is clearly visible that inthe case of dark excitons we should indeed observe only 5lines, in contrast to bright excitons (two upper branches oflines in figure 71), where 6 strong lines should be visiblein each circular polarization for detection. The number ofthese lines reflects the 6 possible spin projections of the Mnion (S = 5/2) onto the quantization axis.Figure 71: Calculated optical transitions of a single Mn-dopedQD. Line width reflects the oscillator str<strong>en</strong>gth, colors indicate circularpolarization of the emitted light (red - σ + , blue - σ − )M. Goryca, P. Plochocka, P. Kossacki, M. PotemskiP. Wojnar (Institute of Physics, Polish Academy of Sci<strong>en</strong>ces, Warsaw), J. A. Gaj (Institute of Experim<strong>en</strong>tal Physics,University of Warsaw)51


SEMICONDUCTORS AND NANOSTRUCTURES 2009InP/GaP self-assembled quantum dots under extreme conditionsSemiconductor quantum dots are promising for the fabricationof novel optoelectronic devices and a number of investigationshave be<strong>en</strong> carried out to understand the electronicand optical properties of quantum dot systems. One powerfulmethod toward understanding the electronic states andshell structure is to investigate photoluminesc<strong>en</strong>ce (PL) inmagnetic fields.5 nm is inferred, which is smaller than the radius of thequantum dots of about 10 nm. Thus, the measurem<strong>en</strong>t provi<strong>des</strong>further evid<strong>en</strong>ce that the electrons belong to the InPvalleys and suggests a type-I band alignm<strong>en</strong>t for InP/GaPquantum dots [Dewitz et al., Appl. Phys. Lett. 95, 151105(2009)].The quantum dot material systems that have be<strong>en</strong> the mostext<strong>en</strong>sively investigated using magnetoluminesc<strong>en</strong>ce areInGaAs/GaAs and InP/InGaP quantum dots. The InP/GaPquantum dot material system has received significantly lessatt<strong>en</strong>tion. It is very interesting, however, for both a fundam<strong>en</strong>talunderstanding of quantum dots based on directindirectband gap semiconductors, as well as its pot<strong>en</strong>tialapplications for visible light emitters.Figure 73: Pressure dep<strong>en</strong>d<strong>en</strong>ce of the magneto-photoluminesc<strong>en</strong>cededuced values of the confinem<strong>en</strong>t l<strong>en</strong>gth l 0 (squares) andthe exciton effective Bohr radius a ∗ (triangles) within the quantumdots. This reveals an increase of the quantum confinem<strong>en</strong>t in theplane of the dots.Figure 72: Pressure dep<strong>en</strong>d<strong>en</strong>ce of the <strong>en</strong>ergy of the two photoluminesc<strong>en</strong>celines up to 1.2 GPa. These two lines correspond tothe direct radiative recombination betwe<strong>en</strong> the ground and the firstexcited states of the dots. An unusually low pressure coeffici<strong>en</strong>tis measured (indicated by the slopes of the solid lines, which arelinear fits to the data).We have first investigated the radiative recombination inInP/GaP self-assembled quantum dots measured in highmagnetic fields. Using magneto-photoluminesc<strong>en</strong>ce spectroscopythe reduced effective mass is determined to havea value of 0.094 m 0 expected for electron states associatedwith the InP valley. Using the determined effective massand the diamagnetic shift in the photoluminesc<strong>en</strong>ce peakat low magnetic fields, an average exciton radius of aboutIn addition, we have also performed cryog<strong>en</strong>ichigh-pressure photoluminesc<strong>en</strong>ce and magnetophotoluminesc<strong>en</strong>ceexperim<strong>en</strong>ts in the 1 GPa range, inseveral cycles. As previously reported [Goñi et al., Phys.Rev. B 67, 075306 (2003)], the luminesc<strong>en</strong>ce is qu<strong>en</strong>chedat 1.2 GPa, and the int<strong>en</strong>sity decreases continuously. However,our experim<strong>en</strong>ts do not show any signature of theΓ → X crossover reported to occur betwe<strong>en</strong> ambi<strong>en</strong>t pressureand 0.3 GPa. We observe in fact a linear and continuousincrease of both the ground state and the first excitedexcitonic state photoluminesc<strong>en</strong>ce features up to 1.2 GPawhere the emission is suppressed. A very low pressure coeffici<strong>en</strong>tis measured which may originate from a decreaseof the quantum confinem<strong>en</strong>t along z driv<strong>en</strong> by a strong increaseof the effective mass. On the other hand, in the planeof the dots, an increase of the quantum confinem<strong>en</strong>t is evid<strong>en</strong>ced[Millot et al., accepted in High Pressure Research].M. Millot, S. George, J. Leotin and J.M. BrotoC.v. Dewitz, F. Hatami and W.T. Masselink (Humboldt-Universitt, Berlin, Germany) and J. Gonzalez (DCITIMAC,Santander, Spain)52


2009Metals, Superconductors and StronglyCorrelated Systems53


2009 METALS, SUPERCONDUCTORS...Thermo-electric study of Fermi surface reconstruction in YBa 2 Cu 3 O yThe Seebeck and Nernst coeffici<strong>en</strong>ts S and ν of the high-T c superconductor YBa 2 Cu 3 O y (YBCO) were measured ina single crystal with a hole conc<strong>en</strong>tration p = 0.12 in magneticfields up to H = 28 T. For temperatures down to 9 K, νbecomes indep<strong>en</strong>d<strong>en</strong>t of field by H ≃ 30 T, showing that byth<strong>en</strong> the Nernst signal due to superconducting fluctuationshas become negligible. In this field-induced normal state,S/T and ν/T are both large and negative in the T → 0 limit.The magnitude of S/T is consist<strong>en</strong>t with the small Fermisurface pocket previously detected via quantum oscillationsin YBCO at a similar doping and its negative sign confirmsthat the pocket is electron-like. For more information see[J. Chang et al., arXiv:0907.5039].Our Nernst measurem<strong>en</strong>ts in YBCO reveal that the quasiparticlecontribution in cuprates can be as large as the vortexcontribution, on which most of the att<strong>en</strong>tion has be<strong>en</strong> focuseduntil now, see for example [Yayu Wang et al., Phys.Rev. B 73, 024510 (2006)]. We expect this quasiparticlecontribution, which can be of either sign, to dominate theNernst signal well above T c , as found in the hole-dopedcuprate Eu-LSCO [O. Cyr-Choiniere et al., Nature 458, 743(2009)] and the electron-doped cuprate Pr 2−x Ce x CuO 4 [P.Li and R.L. Gre<strong>en</strong>e, Phys. Rev. B 76, 174512 (2007)],where quasiparticle and vortex signals have also be<strong>en</strong> dis<strong>en</strong>tangled.The sample was an uncut, unpolished, detwinned crystal ofYBCO grown, at UBC in Vancouver (Canada), in a nonreactiveBaZrO 3 crucible from high-purity starting materials.The dopant oxyg<strong>en</strong> atoms (y = 6.67) were made to orderinto an ortho-VIII superstructure, yielding a superconductingtransition temperature T c = 66.0 K. Transport propertieswere measured via gold evaporated contacts (resistance< 1 Ω), in a six-contact geometry. The thermal gradi<strong>en</strong>t∆T was applied along the a-axis and the field H along thec-axis. For a detailed <strong>des</strong>cribtion of the experim<strong>en</strong>tal setupsee [O. Cyr-Choiniere et al., Nature 458, 743 (2009)].The Nernst and Seebeck coeffici<strong>en</strong>ts are plotted as a functionof magnetic field in Fig. 1. At T >80 K, the Seebeckcoeffici<strong>en</strong>t S is ess<strong>en</strong>tially field indep<strong>en</strong>d<strong>en</strong>t. At T


METALS, SUPERCONDUCTORS... 2009Anomalous criticality in the electrical resistivity of a high-T c cuprateAn important theme in strongly correlated electron systemsis quantum criticality and the associated quantum phasetransitions that occur at zero temperature upon tuning anon-thermal control parameter g (e.g. pressure, magneticfield H or composition) through a critical value g c . Onefeature of such a system is the influ<strong>en</strong>ce that critical fluctuationshave on the physical properties over a wide region inthe (T , g) phase diagram above the quantum critical point(QCP), inside which the system shows marked deviationsfrom conv<strong>en</strong>tional Landau Fermi-liquid behaviour. A numberof candidate non-Fermi-liquid systems have emerged,particularly in the heavy-fermion family, though there areothers, e.g. certain transition metal-oxi<strong>des</strong>, that displaysimilar characteristics.The physics of copper-oxide high temperature superconductorsmay also be governed by proximity to a QCP.The g<strong>en</strong>eric temperature-doping (T , p) phase diagram resemblesthat se<strong>en</strong> in the heavy-fermions, with an appar<strong>en</strong>tfunnel-shaped region that either pierces or skirts the superconductingdome. Above this region, cuprates display anin-plane resistivity ρ ab that varies linearly with temperatureover a wide temperature yet narrow doping range. ThisT -linear resistivity has be<strong>en</strong> widely interpreted, in tandemwith other anomalous transport properties, as a manifestationof scale-invariant physics borne out of proximity to theQCP. This viewpoint has remained untested, largely due tothe high upper critical field H c2 values in hole-doped high-T c cuprates that restrict access to the important limiting lowtemperatureregion below T c (p).In our experim<strong>en</strong>t, we employed a combination of persist<strong>en</strong>tand pulsed high magnetic fields to expose the normalstate of La 2−x Sr x CuO 4 (LSCO) over a wide dopingand temperature range and studied the evolution of ρ ab (T )with carrier d<strong>en</strong>sity, from the slightly underdoped (p =0.15) to the heavily overdoped (p = 0.33) region of thephase diagram. Our measurem<strong>en</strong>ts revealed the preservationof the T -linear resistivity in all superconducting samplesto temperatures as low as 1.5 K [Cooper et al., Sci<strong>en</strong>ce323, 603 (2009)]. Indeed, for all dopings, the ρ ab (T )curves for T < 200 K could be fitted either to the expressionρ ab (T ) = α 0 + α 1 T + α 2 T 2 or to a parallel-resistorformalism1/ρ ab (T ) = 1/[α 0 + α 1 T + α 2 T 2 ] + 1/ρ max withρ max (= 900 ± 100µΩcm). The inclusion of ρ max helps toaccount smoothly for the escalation of ρ ab (T ) to highertemperatures and makes the values of α 1 and α 2 ins<strong>en</strong>sitiveto the temperature range of fitting.Figure 75: Doping evolution of the temperature-dep<strong>en</strong>d<strong>en</strong>t coeffici<strong>en</strong>tsof ρ ab (T ). (A) Doping dep<strong>en</strong>d<strong>en</strong>ce of α 1 , the coeffici<strong>en</strong>tof the T -linear resistivity compon<strong>en</strong>t. (B) Doping dep<strong>en</strong>d<strong>en</strong>ceof α 2 , the coeffici<strong>en</strong>t of the T 2 resistivity compon<strong>en</strong>t. Inboth panels, solid squares are coeffici<strong>en</strong>ts obtained from least--square fits of the ρ ab (T ) curves for T < 200 K to the expressionρ ab (T ) = α 0 + α 1 T + α 2 T 2 , whilst the filled circles are obtainedfrom fits over the same temperature range to a parallel-resistor-formalism1/ρ ab (T ) = 1/[α 0 +α 1 T +α 2 T 2 ]+1/ρ max withρ max = 900± 100 µΩcm. The op<strong>en</strong> symbols are obtained fromcorresponding fits made to the ρ ab (T ) data of [Ando et al., Phys.Rev. Lett. 93, 267004 (2004)] betwe<strong>en</strong> 70 K and 200 K. Thedashed lines are gui<strong>des</strong> to the eye.As shown in the top panel of figure 75, for both sets ofdata and analysis, α 1 is se<strong>en</strong> to grow rapidly with decreasingp, attaining a maximum value of around 1 µΩcm/K atp c = 0.185 ± 0.005. The preservation of T -linear resistivityin LSCO over such a wide doping range is wholly unexpectedand contrasts markedly with what is observed inother candidate quantum critical systems. Our analysis alsoreveals (figure 75) that the magnitude of the T -linear termscales monotonically with T c on the strongly overdopedside but saturates, or is maximal, at a critical doping levelp crit ∼ 0.19 at which superconductivity itself is most robust.The observation of a singular doping conc<strong>en</strong>tration inLSCO close to p = 0.19 at which a bulk transport propertyundergoes a fundam<strong>en</strong>tal change at low T l<strong>en</strong>ds support toearlier thermodynamic studies that showed the pseudogaptemperature T ∗ or <strong>en</strong>ergy scale ∆ g vanishes inside the superconductingdome, rather than at its apex. The magnitudeof α 1 at p = p crit , coupled with other features of the data,suggests that the op<strong>en</strong>ing of the pseudogap coinci<strong>des</strong> withthe loss of quasiparticle coher<strong>en</strong>ce for states near the zoneboundaries.B. Vignolle, C. ProustR. A. Cooper, Y. Wang, N. E. Hussey (University of Bristol, Bristol, UK)56


2009 METALS, SUPERCONDUCTORS...Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of the superconducting <strong>en</strong>ergy gap inBi 2 Sr 2 CaCu 2 O 8+δIn a conv<strong>en</strong>tional BCS materials superconductivity is suppressedby a magnetic field since the superconducting <strong>en</strong>ergygap 2∆ decreases continuously with increasing fieldand vanishes at a critical field H c2 . The reported behaviorof 2∆ in high-T c cuprates studied by a tunnelingmethod ranges from almost magnetic field indep<strong>en</strong>d<strong>en</strong>tin hole-doped cuprates to a strong H-dep<strong>en</strong>d<strong>en</strong>ce inelectron-doped cuprates. Interlayer tunneling spectroscopyof Bi 2 Sr 2 CaCu 2 O 8+d (Bi2212) shows that a peak in thetunneling conductance dI/dV associated with 2∆ broad<strong>en</strong>sand shifts towards higher voltages with increasing magneticfield. Such a behavior of 2∆ has never be<strong>en</strong> observed inBCS superconductors. The superconducting gap in optimallydoped and overdoped Bi2212 is close in size to thepseudogap questioning if the gap of the superconductingstate is detected at all in the tunneling measurem<strong>en</strong>t. Rec<strong>en</strong>tangle-resolved photoemission spectroscopy (ARPES)studies of Bi2212 showed that the spectral gap in the nodaland antinodal regions of mom<strong>en</strong>tum space has a distinctlydiffer<strong>en</strong>t temperature dep<strong>en</strong>d<strong>en</strong>ce [Lee et al. Nature 450, 81(2007)]. This suggests that the magnetic field dep<strong>en</strong>d<strong>en</strong>ceof the <strong>en</strong>ergy gap at differ<strong>en</strong>t points of the Fermi surfaceshould also very differ<strong>en</strong>t. Most experim<strong>en</strong>ts are carriedout in the c-axis tunneling configuration where the tunnelingsamples an angular average over the ab-plane d<strong>en</strong>sity ofstates. In the case of ab-plane tunneling, the tunneling occursalong the CuO 2 planes and the shape of spectra can bequite differ<strong>en</strong>t dep<strong>en</strong>ding on the tunneling direction. Wehave performed ab-plane tunneling experim<strong>en</strong>ts on threeslightly underdoped Bi2212 single crystals (T c =84 K and∆T c = 1.5 K) using break junctions in magnetic fields upH = 20 T. Mechanically retuning the break junction repeatedlyin liquid helium, we were able to fabricate a large numberof tunnel junctions at differ<strong>en</strong>t places along the initialbreak of the crystal where tunneling occurs in the ab-plane.Figure 76(a) displays the tunneling conductances dI/dV asa function of the bias voltage V . All curves have a shapetypical for SIS tunnel junctions with sharp peaks in the conductanceat the voltage ±V = 2∆/e. 2∆ is 45 meV at 4.2 Kwhich, is reasonable wh<strong>en</strong> compared with our previous results.In contrast to previous measurem<strong>en</strong>ts on Bi2212,where the position of the gap peak remained almost unchangedin an applied magnetic field, the superconductingconductance peaks in figure 76(a) decrease in magnitudeand shifts to lower voltages with increasing magnetic field.The only possible interpretation of such a behavior of thetunnel spectra is the suppression of 2∆ by magnetic field.To our knowledge, this is the first unambiguous observationof the suppression of the superconducting gap by magneticfield in tunneling investigations of the Bi2212 system.In figure 76(b), we pres<strong>en</strong>t the magnetic field dep<strong>en</strong>d<strong>en</strong>ceof 2∆ using a semilog scale for the sample No. 1 extractedfrom the gap spacing in the dI/dV curves in figure76 (a).Data for break junctions No. 2 and No. 3 formed on twoother Bi2212 single crystals are also included to demonstratethe reproducibility of the field dep<strong>en</strong>d<strong>en</strong>ce of 2∆.This figure suggests that 2∆ shows a logarithmic decreasewith magnetic field (dashed lines), although we cannot excludeand expon<strong>en</strong>tial dep<strong>en</strong>d<strong>en</strong>ce which also reproducesthe data reasonably well (not shown).Figure 76: (a) Tunneling conductances dI/dV as a function ofthe bias voltage V for a tunnel break junction measured at variousmagnetic fields applied parallel to the c axis of the crystal (sampleNo. 1). All dI/dV curves except the lowest one are offset verticallyfor clarity. (b) The magnetic field dep<strong>en</strong>d<strong>en</strong>ce of 2∆ plottedusing a semilog scale for the three break junctions formed on eachof the three Bi2212 single crystals.B. A. Piot, D. K. MaudeS. I. Ved<strong>en</strong>eev (P.N. Lebedev Physical Institute, Russian Academy of Sci<strong>en</strong>ce, Moscow, Russia)57


METALS, SUPERCONDUCTORS... 2009Magnetoresistance anisotropy and AMRO in the electron dopedsuperconducting cuprate Nd 2−x Ce x CuO 4Rec<strong>en</strong>t discoveries of magnetic quantum oscillations inhole- and electron-doped cuprate superconductors clearlydemonstrate the importance of high-field magnetotransportexperim<strong>en</strong>ts for exploring the Fermi surface inthese materials. Besi<strong>des</strong> quantum oscillations, semiclassicalangle-dep<strong>en</strong>d<strong>en</strong>t magnetoresistance oscillations(AMRO) are known to be a very effici<strong>en</strong>t method forFermi surface studies of layered systems, such as organicconductors [Kartsovnik, Chem . Rev. 104, 5737(2004)]. AMRO have also be<strong>en</strong> observed in hole-overdopedTl 2 Ba 2 CuO 6+δ [Hussey et al., Nature 425, 814 (2003)].Aiming to find AMRO in the electron-doped superconductorNd 2−x Ce x CuO 4 (NCCO), we have performed detailedstudies of the angular dep<strong>en</strong>d<strong>en</strong>ce of its interlayer magnetoresistance.The experim<strong>en</strong>ts were performed on crystalswith doping levels in the range 0.13 ≤ x ≤ 0.17, in a 28 Tresistive magnet. The samples were mounted on a homemadetwo-axes rotating stage allowing an in situ rotation ata fixed B, at temperatures down to 1.4 K. The interlayer resistanceR c was measured as a function of angle θ betwe<strong>en</strong>the field direction and [001] axis of the crystal, at differ<strong>en</strong>tfixed angles ϕ, see inset in Fig. 77(a).0.17. H<strong>en</strong>ce, the relevant Fermi surfaces should be id<strong>en</strong>ticalfor all these compositions. On the other hand, ShubnikovdeHaas data [Helm et al., Phys. Rev. Lett. 103,157002(2009)] suggest a reconstruction of the Fermi surface to occurbetwe<strong>en</strong> x = 0.16 and 0.17. The appar<strong>en</strong>t discrepancy isresolved by taking into account a possible magnetic breakdownbetwe<strong>en</strong> the hole- and electron-like parts of the reconstructedFermi surface. In this case, one should consider apossibility that the Fermi surface is reconstructed over the<strong>en</strong>tire superconducting doping range. Further experim<strong>en</strong>tson AMRO and magnetoquantum oscillations at fields above30 T are ess<strong>en</strong>tial to clarify the details of the Fermi surfaceevolution in overdoped NCCO and its implications for superconductivity.As shown in figure 77(a), underdoped NCCO crystals displayan anomalous dome-like shape of R c (θ), which is mostlikely associated with spin dep<strong>en</strong>d<strong>en</strong>t scattering in a magneticallyordered system. Notably, this behavior is observedev<strong>en</strong> for superconducting compositions, up to the optimaldoping level. The pres<strong>en</strong>ce of ordered spins readjusted atchanging the magnetic field ori<strong>en</strong>tation is manifested in ahysteresis betwe<strong>en</strong> up and down θ-sweeps.At increasing Ce conc<strong>en</strong>tration to the optimal and, further,to the overdoped regime, the anomalous contribution tomagnetoresistance weak<strong>en</strong>s, giving way to the conv<strong>en</strong>tionalmechanism associated with the orbital effect of magneticfield on charge carriers. This gives rise to the positive slopeof the angular dep<strong>en</strong>d<strong>en</strong>ce, dρ c /d|θ| > 0 in an ext<strong>en</strong>dedangular range, 30 ◦ < |θ| 80 ◦ , as shown in Fig. 77(b) fora sample with x = 0.165. The most interesting feature inthis range is a shallow hump superposed on the monotonicslope around ±52 ◦ . The same feature has be<strong>en</strong> found onsamples with x = 0.16 and 0.17 (the latter being the highestaccessible doping level for NCCO). The position of thehump stays constant at changing temperature or magneticfield str<strong>en</strong>gth. Such a behavior is characteristic of AMRO.At this stage, a rigorous quantitative analysis of the AMROfeatures is difficult due to their small amplitude. Nevertheless,already from the existing data one can draw an importantqualitative conclusion. The positions of the AMROturn out to be the same, at all ϕs, for x = 0.16,0.165, andFigure 77: Angle-dep<strong>en</strong>d<strong>en</strong>t interlayer magnetoresistance ofNd 2−x Ce x CuO 4 at B = 28 T, T = 1.4 K. (a) Underdoped sample,x = 0.13, exhibits an anomalous dome-like shape with a hysteresisbetwe<strong>en</strong> up and down θ-sweeps. At |θ| > 70 ◦ the resistancesharply drops due to the onset of superconductivity. Inset showsthe geometry of the experim<strong>en</strong>t. (b) For the overdoped sample,x = 0.165, a conv<strong>en</strong>tional magnetoresistance dominates at least at30 ◦ < |θ| < 70 ◦ . Arrows point to AMRO features whose positionsdep<strong>en</strong>d on azimuthal angle ϕ.I. SheikinM. V. Kartsovnik and T. Helm (Walther-Meissner-Institut, Garching, Germany)58


2009 METALS, SUPERCONDUCTORS...Transport measurem<strong>en</strong>ts of H c2 and its anisotropy in FeSe 1−x Te x single crystalsExploring the temperature dep<strong>en</strong>d<strong>en</strong>ce of H c2 and itsanisotropy in the new Fe superconductors is an importantexperim<strong>en</strong>tal tool to help revealing the mechanism of superconductivity.For example in LaFeAsO 0.89 F 0.11 , the upturnin curvature for H c2 was observed, which suggeststwo-band superconductivity [Hunte et al, Nature 453, 903(2008)]. The high transition temperatures imply high valuesof H c2 , meaning that it is not easy to obtain the full curvedown to low temperature, and many low temperature valuesof H c2 are in fact extrapolations. However, in order to comparethe real behavior to theoretical models, measurem<strong>en</strong>tsdown to low temperature, and thus at very high field, ar<strong>en</strong>ecessary.A serious limitation at pres<strong>en</strong>t is that the homog<strong>en</strong>eity ofmany samples that are studied is highly questionable, andthe highest T c values are obtained on doped, probably inhomog<strong>en</strong>eous,systems. From this aspect the rec<strong>en</strong>t discoveryof superconductivity in FeSe and FeTe 1−x Se x suggestsa promising new direction as these compounds are close tobeing stoichiometric and have a relatively simple structure.We have rec<strong>en</strong>tly grown single crystals of FeSe [Braithwaiteet al, J. Phys.: Cond<strong>en</strong>s. Matter 21, 232202 (2009)],which so far are not homog<strong>en</strong>eous, and FeTe 1−x Se x whichshow homog<strong>en</strong>eous bulk superconductivity, with T c around14 K, characterized by specific heat measurem<strong>en</strong>ts (figure78), and seem suitable for more detailed studies.In the LNCMI-Gr<strong>en</strong>oble, we have measured the anisotropyof H c2 on our FeTe 1−x Se x single crystals up to 28 T. Thisgives a very precise determination of a large part of thecurve. These measurem<strong>en</strong>ts have be<strong>en</strong> completed by measurem<strong>en</strong>tsin pulsed field in LNCMI-Toulouse where thelow temperature part of the curve was obtained, showingthat H c2 reaches almost 50 T at low temperature (figure 79).Analysis of the data is now in progress but a preliminarystudy suggests that although H c2 significantly exceeds thePauli limit, some Pauli limiting is occurring, and this isquite anisotropic. Refinem<strong>en</strong>ts of the analysis and preparationof a publication are in progress.Figure 78: Specific heat of the single crystal of FeSe 1−x Te xgrown in CEA/Gr<strong>en</strong>oble used in these measurem<strong>en</strong>ts. Inset showsthe electronic part of C/T after subtraction of the phonon contribution.Figure 79: Upper critical field of a FeSe 1−x Te x single crystalgrown in CEA/Gr<strong>en</strong>oble, combining DC field measurem<strong>en</strong>ts upto 9 T made in CEA/Gr<strong>en</strong>oble, DC field measurem<strong>en</strong>ts up to 28T made in LNCMI/Gr<strong>en</strong>oble, and pulsed field measurem<strong>en</strong>ts upto 55 T made in LNCMI/Toulouse. Lines show fits made using aBCS weak coupling model.I. Sheikin, W. KnafoD. Braithwaite , G. Lapertot, C. Marin (CEA/Gr<strong>en</strong>oble, Gr<strong>en</strong>oble, France),59


METALS, SUPERCONDUCTORS ... 2009Coexist<strong>en</strong>ce of magnetic order and superconductivity in iron pnicti<strong>des</strong>How long range magnetic order can coexist with bulk superconductivityis a c<strong>en</strong>tral question in a number of unconv<strong>en</strong>tionalsuperconductors. Both in the copper oxideand in the ”new” iron pnictide family of high temperaturesuperconductors the superconducting phase is obtained byadding charge carriers into a phase with antiferromagneticorder. Observation of phase coexist<strong>en</strong>ce in such a situationimmediately raises two important questions. The firstone is about the intrinsic character of the coexist<strong>en</strong>ce. Thisquestion is obviously linked to a rather subtle issue in theseoff-stoichiometric materials: to which ext<strong>en</strong>t is chemicalinhomog<strong>en</strong>eity of the samples intrinsic or not, i.e. unavoidableor not? The next important question is: Do the phasesoverlap in space, or do they occupy mutually exclusive volumes?In short, on which l<strong>en</strong>gth scale do the two phasescoexist? This is an equally delicate problem because unambiguousdirect experim<strong>en</strong>tal proofs are in most cases difficultto obtain, ev<strong>en</strong> for true local probes such as nuclearmagnetic resonance (NMR), muon spin rotation (µSR) orscanning tunneling microscopy (STM). As a matter of fact,the debate is still going on in the cuprates. In the ironpnicti<strong>des</strong>, magnetic order (a spin d<strong>en</strong>sity wave state) hasrec<strong>en</strong>tly be<strong>en</strong> found to coexist with superconductivity inseveral (but not all) families. Yet, a global picture of theconditions for this coexist<strong>en</strong>ce in the pnicti<strong>des</strong> is still lacking.We have measured the NMR properties of 75 As nucleiin single crystals of Ba(Fe 1.95 Co 0.05 ) 2 As 2 andBa 0.6 K 0.4 Fe 2 As 2 , both of which show 100% Meissner volumefraction [Juli<strong>en</strong> et al., EPL 87, 37001 (2009)]. Ourresults demonstrate that both samples show the coexist<strong>en</strong>ceof bulk superconductivity with magnetic (SDW) order. Yet,the details appear differ<strong>en</strong>t:- In Ba(Fe 1.95 Co 0.05 ) 2 As 2 , the fact that the NMR signalat the paramagnetic resonance frequ<strong>en</strong>cy vanishes abruptlyand completely below TSDW onset = 56 K indicates that the twophases coexist at the microscopic scale probed by NMR, asituation which is oft<strong>en</strong> referred to as ”homog<strong>en</strong>eous mixing”in the literature. This implies either that both types oforders are simultaneously defined at each Fe site (owing tothe multiple bands pres<strong>en</strong>t at the Fermi level), or that theyare mixed on the scale not greater than one or two latticespacing. A nanoscale coexist<strong>en</strong>ce involving superconductingislands (without magnetic order) of typical size definedby the coher<strong>en</strong>ce l<strong>en</strong>gth ξ ≃ 2.8 nm appears to be unlikely.In this case, some paramagnetic NMR signal from regionsas large as t<strong>en</strong> times the Fe-Fe distance should have be<strong>en</strong>observed.- In Ba 0.6 K 0.4 Fe 2 As 2 , on the other hand, the NMR signalhas decreased but remains finite in the whole temperaturerange, including the superconducting state. Thus, the magneticregions do not occupy the full sample volume. Inthis s<strong>en</strong>se, the coexist<strong>en</strong>ce might be qualified as ”inhomog<strong>en</strong>eous”.Figure 80: Top panel: In-plane resistivities. Bottom panel: NMRsignal int<strong>en</strong>sities (r<strong>en</strong>ormalized by temperature). Excessive signalloss is due to the spin-d<strong>en</strong>sity-wave transition in all (Co-dopedmaterial) or part (K-doped material) of the samplePerhaps unexpectedly, the inhomog<strong>en</strong>eity is considerablystronger in the potassium-doped sample. Actually, the factthat substitutions at the Fe site, unlike substitutions at theCu site in the cuprates, improve conductivity and ev<strong>en</strong> inducesuperconductivity is one of the most remarkable surprisesof these new superconductors. It is difficult to fullyunderstand the Ba 1−x K x Fe 2 As 2 system from the pres<strong>en</strong>tNMR data only. The important inhomog<strong>en</strong>eity/disordercould be due to inhomog<strong>en</strong>eity of K + conc<strong>en</strong>tration and/orto a particularly strong impact of these ions on the localelectronic structure in FeAs layers. No evid<strong>en</strong>ce for phaseseparation could be detected in the K-doped sample, andthe single crystal exhibits 100% Meissner fraction. Wepoint out that T SDW vs. x is extremely steep near x = 0.4.Phase separation or inhomog<strong>en</strong>eous coexist<strong>en</strong>ce could thusoriginate from K-doping inhomog<strong>en</strong>eity around this particularconc<strong>en</strong>tration. Therefore, they might not reflect theproperties at somewhat lower x values. In other words,Ba 1−x K x Fe 2 As 2 should perhaps be simply viewed as a disorderedversion of Ba(Fe 1−x Co x ) 2 As 2 . Anyhow, the coexist<strong>en</strong>ceof magnetic and superconducting phases clearlyemerges as a cornerstone of the iron-pnictide physics.M. Horvatić, C. BerthierM.-H. Juli<strong>en</strong>, H. Mayaffre (<strong>Laboratoire</strong> de Spectrométrie Physique, Université J. Fourier, Gr<strong>en</strong>oble, France), X. D.Zhang, W. Wu, G.F. Ch<strong>en</strong>, N.L. Wang, J.L. Luo (Beijing <strong>National</strong> Laboratory for Cond<strong>en</strong>sed Matter Physics andInstitute of Physics, Chinese Academy of Sci<strong>en</strong>ce, Beijing, China)60


2009 METALS, SUPERCONDUCTORS...High-field metamagnetism in the antiferromagnet CeRh 2 Si 2CeRh 2 Si 2 is a heavy-fermion antiferromagnet which canbe driv<strong>en</strong> to a magnetic instability either by applying pressureor in a high magnetic field. It orders antiferromagneticallyat a second-order phase transition T N = 36 K, afirst-order phase transition occurring at a lower temperatureT 1,2 = 26 K, below which the antiferromagnetic structure ismodified [Graf et al., Phys. Rev. B 57, 7442 (1998)]. Applicationof hydrostatic pressure induces a quantum phasetransition to a paramagnetic Fermi liquid regime at around11 kbar, and unconv<strong>en</strong>tional superconductivity was evid<strong>en</strong>cedin the vicinity of the quantum phase transition,below a critical temperature going up to TSCmax ≈ 0.4 K[Movshovich et al., Phys. Rev. B 53, 8241 (1996)]. Here,we pres<strong>en</strong>t a careful study of the magnetic field-temperaturephase diagram of CeRh 2 Si 2 wh<strong>en</strong> a magnetic field is appliedalong the easy-axis c. This study was made combiningtransport, torque and dilatometry experim<strong>en</strong>ts using thepulsed magnetic fields g<strong>en</strong>erated at the LNCMI-Toulouse.Figure 81 shows a plot of the field-derivative of the torqueversus magnetic field of CeRh 2 Si 2 , at temperatures betwe<strong>en</strong>4.2 and 24 K. The torque signal is proportional to MH sinθ,where M is the magnetization and θ the small angle betwe<strong>en</strong>the magnetic field H and the easy axis c of the sample.The field-induced polarization of the system is accompaniedat 4.2 K by two successive minima in the fieldderivativeof the torque, which are the characteristics oftwo first-order transitions, separated by 0.5 T, at H 2,3 andH c ≃ 26 T. From figure 81, it is clear that the two transitionsH 2,3 and H c merge at about 20 K into a single first-ordertransition H c . In our data, a first-order-like anomaly at H ccan be se<strong>en</strong> up to 23 K, which is characterized by a symmetricpositive anomaly in the field-derivative of the torque.Above 24 K, a second-order-like anomaly has replaced thefirst-order-like anomaly, and the torque versus field data arecharacterized by an asymmetric step-like anomaly in thefield-derivative of the torque.Our torque data are in good agreem<strong>en</strong>t with our transport,thermal expansion, and magnetostriction measurem<strong>en</strong>ts(not shown here), but also with studies performedby Settai et al. [J. Phys. Soc. Jpn. 66, 2260 (1997)], Abeet al. [J. Phys. Soc. Jpn. 66, 2525 (1997)], and Demuer,Sheikin et al. [to be published]. This study permitted todraw the magnetic field-temperature phase diagram of thesystem, indicating the pres<strong>en</strong>ce of three distinct antiferromagneticphases (see figure 82). The possibility of a tetracriticalpoint at around (24 T, 20 K), where the four antiferromagnetictransition lines could merge, was suggestedhere. It should be further checked using continuous highmagnetic fields. The temperature dep<strong>en</strong>d<strong>en</strong>ce of the resistivity(not shown here) was also extracted from our pulsedfield scans. This permitted to show that the quadratic coeffici<strong>en</strong>tA of the resistivity is <strong>en</strong>hanced in a rather large Hwindow, of about 10 T, which contrasts with the additionalsharp <strong>en</strong>hancem<strong>en</strong>t of A through the first-order metamagnetictransitions H 2,3 and H c , which are only separated by0.5 T. Finally, a drop of resistivity observed at H c is compatiblewith the idea of a Fermi surface reconstruction.Figure 81: Magnetic field-derivative of the torque versus magneticfield of CeRh 2 Si 2 , for temperatures T ≤ 24 K and magneticfields along c.Figure 82: Magnetic field versus temperature phase diagram ofCeRh 2 Si 2 , with H ‖ c, obtained from resistivity, torque, and thermalexpansion. The insert focuses on the low-temperature part ofthe phase diagram.W. Knafo, D. Vignolles, B. Vignolle, Y. Klein, C. Jaudet, C. ProustD. Aoki, A. Villaume, J. Flouquet (Commissariat à l’Energie Atomique, Gr<strong>en</strong>oble)61


METALS, SUPERCONDUCTORS ... 2009Field Evolution of Coexisting Superconductingand Magnetic Orders in CeCoIn 5Heavy fermion compound CeCoIn 5 is one of the most intriguingexamples of a manifestation of the coexist<strong>en</strong>ce ofmagnetic and superconducting (SC) orders. In the SC stateof this compound application of a magnetic field (H 0 ) inducesa long range magnetic order (LRO), restricted to asmall high-field low-temperature region of the phase diagramjust below H c2 . What is more, this particular region ofthe phase diagram was initially id<strong>en</strong>tified as the first realizationof the long-sought Fulde, Ferrell, Larkin, and Ovchinnikov(FFLO) state, a superconducting state with a nonzeropair mom<strong>en</strong>tum and a spatially modulated order parameter.However, important questions regarding the tru<strong>en</strong>ature of this SC phase, the details of the magnetic orderand its field dep<strong>en</strong>d<strong>en</strong>ce, and the pot<strong>en</strong>tial driving mechanismsof their coexist<strong>en</strong>ce remain unanswered. Therefore,CeCoIn 5 provi<strong>des</strong> a strikingly rich ground to study thecomplex interplay betwe<strong>en</strong> exotic SC and magnetic degreesof freedom. Experim<strong>en</strong>tally, nuclear magnetic resonance(NMR), as a microscopic probe s<strong>en</strong>sitive to both magneticand SC degrees of freedom, provi<strong>des</strong> a powerful tool for theinvestigation of these puzzles.Here we report detailed low temperature (T ) 115 In NMRmeasurem<strong>en</strong>ts on the three distinct In sites in CeCoIn 5 , forH 0 ||[100] [Koutroulakis et al., Phys. Rev. Lett. in press(arXiv:0912.3548)]. The axially symmetric In(1) is locatedin the c<strong>en</strong>ter of the tetragonal Ce planes, while In(2 ac ) andIn(2 bc ) sites correspond to In atoms located on the lateralfaces (parallel and perp<strong>en</strong>dicular to the applied field, respectively)of the unit cell. In figure 83 the H 0 evolutionof the In(2 ac ) spectra at T ≈70 mK is plotted. Loweringthe field below ≈ 11.7 T establishes magnetic LRO, whichis evid<strong>en</strong>t from the broad<strong>en</strong>ing of the In(2 ac ) line into aspectrum with two extrema/peaks and finite signal weightin betwe<strong>en</strong> them. Such spectra are characteristic of incomm<strong>en</strong>surate(IC) LRO along one spatial dim<strong>en</strong>sion. For9.2T H 0 10.2 T, the spectra of all In sites consist of asingle peak, i.e. no signature of the IC state is observed.However, these spectra remain significantly broader thanthe ones for H 0 9.2 T, where the linewidth of all sites canbe adequately <strong>des</strong>cribed by the spatial distribution of magneticfields resulting from the vortex lattice of an Abrikosov(low-field) SC state (lfSC).By NMR we have thus established that at T ≈ 70mK aphase with static magnetic LRO is stabilized for fieldsabove ≈ 10.2T in the SC state. By analyzing the spectraof the differ<strong>en</strong>t In sites, we deduce that the LRO is an incomm<strong>en</strong>suratespin d<strong>en</strong>sity wave (IC-SDW) with mom<strong>en</strong>tsori<strong>en</strong>ted along the ĉ-axis, indep<strong>en</strong>d<strong>en</strong>t of the in-plane H 0ori<strong>en</strong>tation. We fit the data to simulated spectra for the IC-SDW order with magnitude of the local magnetic mom<strong>en</strong>t(µ 0 ) as a fitting parameter. This allows us to map the detailedfield evolution of the mom<strong>en</strong>t. From the analysis ofthe field dep<strong>en</strong>d<strong>en</strong>ce of the NMR shift we show that this IC-SDW coexists with a novel SC state, that is likely an FFLOphase, characterized by an <strong>en</strong>hanced spin susceptibility.Figure 83: Low temperature NMR spectra of In(2 ac ) for variousH 0 ‖â. The frequ<strong>en</strong>cy scale is defined by subtracting ω 0 , the zeroNMR shift frequ<strong>en</strong>cy. N d<strong>en</strong>otes the normal phase, IC the LROphase, eSC the state with strong spin fluctuations, and lfSC theAbrikosov SC state. The LRO is evid<strong>en</strong>t in the fact that the In(2 ac )line broad<strong>en</strong>s into a spectrum with two extrema. Such spectra arecharacteristic of IC LRO along one spatial dim<strong>en</strong>sion. Red solidlines are simulated spectra for the IC-SDW order.By consideration of the spectral lineshapes and spin decoher<strong>en</strong>cetime of differ<strong>en</strong>t In sites for 9.2T H 0 10.2Tat low-T , we conclude that this corresponds to an ‘exotic’SC (eSC) phase characterized by strong AF fluctuations.This might be a ‘true FFLO’ phase, unperturbed by LROmagnetic order. This phase is separated from the above <strong>des</strong>cribedhigh-field, low-T phase by the 2 nd order phase transitionpreviously id<strong>en</strong>tified at H ∗ ≈ 10.2 T from the NMRlineshift data. Such a two step phase transition from lfSCto FFLO (assuming it exists in eSC) and th<strong>en</strong> to the IC statewas theoretically predicted wh<strong>en</strong> spin fluctuations are considered.The IC magnetism can arise in the FFLO state ina d-wave SC as a consequ<strong>en</strong>ce of the formation of Andreevbound states near the zeros of the FFLO order parameter.The formation of the IC LRO is triggered by a large DOSin these bound states.M. Horvatić, C. BerthierG. Koutroulakis, V. F. Mitrović (Brown University, Provid<strong>en</strong>ce, U.S.A.), G. Lapertot, J. Flouquet (INAC, SPSMS, CEAGr<strong>en</strong>oble, France)62


2009 METALS, SUPERCONDUCTORS...Fermi surface study in the hidd<strong>en</strong> order state of URu 2 Si 2The heavy fermion superconductor URu 2 Si 2 has attractedmuch att<strong>en</strong>tion for the past two deca<strong>des</strong> because of the socalledhidd<strong>en</strong> order (HO) phase below T 0 = 17.5K, wherea tiny magnetic mom<strong>en</strong>t of 0.03µ B with the wave vectorQ 0 = (1,0,0) appears. The associated <strong>en</strong>tropy at T 0 is,however, too large. That is why many theoretical modelshave be<strong>en</strong> proposed, such as, spin- and/or charge-d<strong>en</strong>sitywave, higher orbital ordering, helicity order, etc. Furthermoreit was rec<strong>en</strong>tly reported that a new phase transition ora crossover appears at H ∗ = 23T below 2K [Shishido et al.Phys. Rev. Lett. 102, 156403 (2009)]. Above H ∗ , a newdHvA frequ<strong>en</strong>cy with relatively light effective mass was detectedin a high quality sample. Nevertheless, there are stillundetected Fermi surfaces, considering the large specificheat coeffici<strong>en</strong>ts and carrier numbers. It is important to determinethe electronic states from the microscopic point ofviews. One of the most powerful experim<strong>en</strong>tal probe is thede Haas-van Alph<strong>en</strong> (dHvA) or Shubnikov-de Haas (SdH)effects. Rec<strong>en</strong>tly, we succeeded in growing high qualityURu 2 Si 2 single crystals (RRR > 200) in order to performthe SdH experim<strong>en</strong>ts. Here we report the rec<strong>en</strong>t results ofSdH experim<strong>en</strong>ts using high quality single crystals at highfields up to 34T and at low temperatures down to 30mK.Figure 84(a) shows the magnetoresistance for the curr<strong>en</strong>talong [100] at various field directions in URu 2 Si 2 . Thelarge magnetoresistance and clear SdH oscillation indicatethe high quality of our sample. The kink is clearly detectedfor H ‖ [001] at H ∗ = 24T, which shifts to the higher fieldwith increasing the field angle from [001] to [100]. Theangular dep<strong>en</strong>d<strong>en</strong>ce of H ∗ is shown in Fig. 84(b). H ∗ approximatelyfollows the 1/cosθ-dep<strong>en</strong>d<strong>en</strong>ce. We show infigure 85 the typical SdH oscillation for H ‖ [001] and forthe field tilted 52deg from [001] to [100]. As clearly se<strong>en</strong>in figure 85, the SdH amplitude abruptly increases aboveH ∗ for H ‖ [001], while the SdH amplitude at field angle52deg smoothly increases, following the Lifshitz-Kosevichformula. Below H ∗ , the fast Fourier transform (FFT) analysisshows three kinds of SdH branches, namely α, β andγ. The cyclotron effective masses for H ‖ [001] below H ∗are 12m 0 and 18m 0 for branch α and β, respectively. Althoughthe number of wave is not <strong>en</strong>ough to analyze thedata, the SdH frequ<strong>en</strong>cy for branches α and β shows nochange above H ∗ , however, the cyclotron mass for branchβ seems to decrease above H ∗ . These results clearly indicatethat the electronic state is changed above H ∗ in the HOstate. Further experim<strong>en</strong>ts, such as thermoelectric power,are required to confirm this point.Figure 84: (a)Magnetoresistance at various field directions from[001] to [100] at 30mK in URu 2 Si 2 . (b)Angular dep<strong>en</strong>d<strong>en</strong>ce ofH ∗ , which is defined as a kink of magnetoresistance. The solidline corresponds to the 1/cosθ dep<strong>en</strong>d<strong>en</strong>ce.Figure 85: Typical Shubnikov-de Haas oscillations for the fieldalong [001] and for the field tilted 52deg from [001] to [100].I. SheikinD. Aoki, E. Hassinger, V. Taufour, J. Flouquet (CEA-Gr<strong>en</strong>oble),63


METALS, SUPERCONDUCTORS... 2009High field resistivity measurem<strong>en</strong>ts on single crystalline UPt 2 Si 2Tetragonal UPt 2 Si 2 has rec<strong>en</strong>tly be<strong>en</strong> characterized as amoderately mass <strong>en</strong>hanced antiferromagnet (T N = 32 K),which in various physical properties closely resembles thehidd<strong>en</strong> order material URu 2 Si 2 [Süllow et al., J. Phys. Soc.Jpn. 77, 024708 (2008); Johanns<strong>en</strong> et al., Phys. Rev. B 78,121103 (2008) ; Kim et al., Phys. Rev. Lett. 91, 256401(2003); Amitsuka et al., Physica B 177, 173 (1992) ].are clearly to be se<strong>en</strong>, supporting the notion of the similaritybetwe<strong>en</strong> the two systems. Pres<strong>en</strong>tly, high field magnetizationmeasurem<strong>en</strong>ts at 3 He temperatures are underway toext<strong>en</strong>d the determination of these phase boundaries to verylow temperatures.Similar to URu 2 Si 2 , high field phase transitions at low temperatureshave be<strong>en</strong> observed in UPt 2 Si 2 , that is in fieldsof 30 T to 45 T along the a direction and 20 T to 33 Talong c [Amitsuka]. Rec<strong>en</strong>t high field measurem<strong>en</strong>ts revealadditional structure in the magnetic phase diagram, emphasizingthe close resemblance to URu 2 Si 2 .Based on these findings, the goal of the pres<strong>en</strong>t set of experim<strong>en</strong>tswas to verify and more accurately define the highfield phase boundaries observed in previous resistivity andmagnetization measurem<strong>en</strong>ts. Therefore, high field resistivityexperim<strong>en</strong>ts at low temperatures along the crystallographica and c axes of UPt 2 Si 2 were initiated and carriedout.We have measured the high field resistivity along the crystallographica and c axes in field and temperature sweeps upto 28 T and 40 K. From our data we calculated the differ<strong>en</strong>tialresistivities ∂R/∂B and ∂R/∂T , in which the transitionsappear as local maxima (∂R/∂B) or minima (∂R/∂T ).In the temperature sweeps the transition to the antiferromagnetphase is clearly visible for both directions. In fieldsweeps with B applied along the a axis the high field phaseis not accessible but for B//c the phase boundary to thelowest high field phase occurring at ∼ 25 T below 18 K isvisible.Together with the data tak<strong>en</strong> previously, we construct themagnetic phase diagram of UPt 2 Si 2 , as shown in figure 86.In these diagrams, field induced phases similar to URu 2 Si 2Figure 86: Proposed magnetic phase diagrams for the crystallographica and c directions derived from previous and actual magnetizationand resistivity measurem<strong>en</strong>ts.I. SheikinD. Schulze Grachtrup, S. Süllow (TU Braunschweig, Institute for Physics of Cond<strong>en</strong>sed Matter, Braunschweig, Germany)64


2009 METALS, SUPERCONDUCTORS...Evolution of the Fermi surface of BaFe 2 (As 1−x P x ) 2on <strong>en</strong>tering the superconducting domeThe Fermi surface topology of the iron-pnicti<strong>des</strong> is widelythought to play a key role in determining the type of magneticor superconducting order that occurs in these materialsat low temperature. Measurem<strong>en</strong>ts of the de HaasvanAlph<strong>en</strong> (dHvA) effect provide a unique way of measuringthe Fermi surface of these materials. Prior to thepres<strong>en</strong>t work, measurem<strong>en</strong>t had only be<strong>en</strong> possible in thestoichiometric <strong>en</strong>d members of the various families. However,to gain an understanding of how the bulk Fermi surfaceevolves as the correlation effects responsible for superconductivitybecome strong, it is necessary to measurethe highest T c superconducting samples. With the notableexception of the low T c phosphide material LaFePO, otheriron-pnicti<strong>des</strong> need to tuned, either chemically or with pressurein order for them to become superconducting. Chemicallytuning oft<strong>en</strong> adds disorder, for example replacing Feby Co in the series Ba(Fe 1−x Co x ) 2 As 2 . This decreases dramaticallythe dHvA signal, making it unobservable ev<strong>en</strong> inhigh pulsed fields. Rec<strong>en</strong>tly, it was discovered that substitutingAs for P in the series BaFe 2 (As 1−x P x ) 2 producedhigh T c superconductivity without changing the carrier conc<strong>en</strong>tration(both As and P are in the 3+ state so this is anisoelectric substitution). Importantly, this substitution doesnot appear to produce significant disorder in the conductingplane, making this an excell<strong>en</strong>t candidate system for adHvA study.Measurem<strong>en</strong>ts were made in Toulouse on BaFe 2 (As 1−x P x ) 2samples with three differ<strong>en</strong>t values of x, with T c rangingfrom 12 K to 30 K. These measurem<strong>en</strong>ts were supplem<strong>en</strong>tedwith other data obtained using superconductingmagnets in Osaka (17 T), the hybrid magnet in Tallahassee(45 T), and a resistive magnet in Nijmeg<strong>en</strong> (33 T).Figure 88: Variation of the size of the electron orbits (α andβ) and the effective mass of quasiparticle moving on the β orbitas a function of phosphorous fraction x in BaFe 2 (As 1−x P x ) 2 .The variation of T c with x is also shown. The data show that theelectron Fermi surfaces shrink and the effective mass increasesas x decreases and T c becomes larger. Data for samples withx = 0.64,0.72, and 1.0 were obtained using dc fields in Osaka,Nijmeg<strong>en</strong> and Tallahassee.Band-structure calculations suggest that the Fermi surfaceof these materials consists of quasi-two-dim<strong>en</strong>sional electronand hole sheets. The total volumes of the electron andhole sheets are exactly equal (comp<strong>en</strong>sated metal). In ourexperim<strong>en</strong>t only the electron Fermi surfaces were observed.This follows a tr<strong>en</strong>d found for other iron-phosphi<strong>des</strong> wherethe mean free path on the electron Fermi surface is muchlonger than on the hole sheets.Figure 87: Measured de Haas-van Alph<strong>en</strong> data for samplesof BaFe 2 (As 1−x P x ) 2 . The left panels show raw torque data atT = 1.5 K. The right panels show the oscillatory part of the torqueand the corresponding fast Fourier transforms, for samples withx = 0.41 and 0.56. No oscillations were observed for the highestT c = 30 K sample (x = 0.33).The main conclusion is that the data show that the volumeof the electron sheets (and via charge neutrality also thehole sheets) shrink linearly and the effective masses becomestrongly <strong>en</strong>hanced with decreasing x. Calculationsshow that it is unlikely that these changes are a simpleconsequ<strong>en</strong>ce of the one-electron bandstructure but insteadthey likely originate from many-body interactions. Thesechanges may be intimately related to the high T c unconv<strong>en</strong>tionalsuperconductivity in this system. These results arereported in detail in Shishido et al. arXiv:0910.3634.D. Vignolles, B. Vignolle, C. ProustA. Carrington, A.F. Bangura, A.I. Coldea, P.M.C. Rourke (Bristol University), A. McCollam (HMFL, Nijmeg<strong>en</strong>), H.Shishido, S. Tonegawa, K. Hashimoto, S. Kasahara, H. Ikeda, T. Terashima, Y. Matsuda, T. Shibauchi (University ofKyoto), R. Settai, Y. Ōnuki (University of Osaka)65


METALS, SUPERCONDUCTORS... 2009Angular dep<strong>en</strong>d<strong>en</strong>ce of the Nernst effect in elem<strong>en</strong>tal bismuthThe Fermi surface of bismuth consists of one pocket ofhole-like carriers with an ellipsoid shape whose long axisis along the trigonal direction, and three electron pockets,arrayed symmetrically around the hole ellipsoid (see figure89(a)) for a sketch). The electron pockets are muchmore anisotropic than the hole pocket. It is known thatin two directions the electronic bands are <strong>des</strong>cribed by theDirac Hamiltonian [Wolf, J. Phys. Chem. Solids 25,1057(1964)]. The full volume of the Fermi surface occupies10 −5 of the volume of the Brillouin zone. One consequ<strong>en</strong>ceof this remarkable property is that the quantum limit can bereached for a magnetic field as low as 9 T, ori<strong>en</strong>ted alongthe trigonal axis. It has rec<strong>en</strong>tly appeared that the Nernst effect(the transverse voltage induced by a longitudinal temperaturegradi<strong>en</strong>t, in the pres<strong>en</strong>ce of a magnetic field) is avery s<strong>en</strong>sitive probe of quantum oscillations in the vicinityof the quantum limit. Above 9 T, i.e. beyond the holequantum limit (QL), three unexpected anomalies were se<strong>en</strong>in the Nernst response of bismuth [Behnia et al., Sci<strong>en</strong>ce11, 1729 (2007)]. These anomalies were interpreted as signaturesof many-body effects. However, it has rec<strong>en</strong>tly appearedthat the one-particle spectrum of bismuth is complex,and a small misalignm<strong>en</strong>t off the trigonal axis woulddrastically change the field position of the electron Landaulevels. In abs<strong>en</strong>ce of an angular-resolved study, the additionalNernst anomalies could be explained in one-particlepicture with a small misalignm<strong>en</strong>t [Sharlai Mikitik, Phys.Rev. B 79, 081102(R) (2009)].In order to clarify the origins of these unexpected Nernstanomalies, we studied the angular dep<strong>en</strong>d<strong>en</strong>ce of the Nernsteffect in bismuth. For this purpose, we built our ownthermoelectric single and double rotator set-up based on apiezoelectric positionner (typical angular accuracy: 0.01 ◦ ).The ori<strong>en</strong>tation of the sample in the magnetic field was determinedby Hall probes. Figure 89(b)) pres<strong>en</strong>ts the Nernstvoltage at T = 1.3 K for a magnetic field tilted in the trigonalbinary plane. The typical angular step is 0.5 ◦ . At lowfield, quantum oscillations with a main period of 0.15 T −1 ,corresponding to the hole ellipsoid can be se<strong>en</strong>. Over theangular range investigated here the QL of the hole pocketdoes not change significantly. Above the QL, we can resolvetwo quasi vertical lines in the (B, θ) plane, which aresymmetrical about θ = 0. These lines are more obvious onthe (B, θ) color map of the high magnetic Nernst voltage reportedin figure 89(c)) (deduced from figure 89(b))). Thesetwo lines define a cone which is reminisc<strong>en</strong>t to the cone observedby torque [Li et al, Sci<strong>en</strong>ce, 321, 547 (2008)] andtransport measurem<strong>en</strong>t [Fauqué et al, Phys. Rev. B 79,245124 (2009)]. According to the rec<strong>en</strong>t calculation on theLandau levels spectrum of bismuth performed by [Aliceaand Bal<strong>en</strong>ts, Phys. Rev. B 79, 081102(R) (2009)], this conecorresponds to the 0 + electron Landau level.Figure 89: (a) Sketch of the Fermi surface of bismuth: the holeand the electron pockets are respectively in red and gre<strong>en</strong>. (b)Nernst voltage as a function of B at T = 1.3 K for a magnetic fieldtilted in the trigonal binary plane. θ, the angle betwe<strong>en</strong> the trigonalaxis and the magnetic field direction, varies from −8.4 ◦ to 8.5 ◦ .The curves are shifted for clarity. (c) Color map of the Nernstvoltage betwe<strong>en</strong> 10.5 T and 28 T for a magnetic field tilted in thetrigonal binary plane. (d) Nernst voltage for θ=0 as a function ofthe magnetic field for various temperatures T = 1.3,2.3,3.4,5.5and 8.5 K.In addition to these lines, we can id<strong>en</strong>tify at least three additionallines inside and outside the cone. Each of these linesseems to be characterized by their own angular dispersionin the (B, θ) plane. Figure 89(d)) pres<strong>en</strong>ts the evolution ofthe Nernst response with temperature, for a magnetic fieldori<strong>en</strong>ted along the trigonal direction(θ=0). As se<strong>en</strong> in thefigure the anomalies fade away wh<strong>en</strong> the temperature exceeds3.4 K.In conclusion, our angular-dep<strong>en</strong>d<strong>en</strong>t study reveals that: (i)the Nernst effect can reveal hole and electron Landau levelsspectrum (ii) the unexpected Nernst anomalies cannotbe explained by the electron Landau levels and are characterizedby their own angular dep<strong>en</strong>d<strong>en</strong>ce. The additionalNernst anomalies are unexpected in single-particle theoryand point to collective effects, which are yet to be understood.A.B. Antunes, L. MaloneH. Yang, B. Fauqué, K. Behnia (LPEM/ESPCI, Paris, France)66


2009 METALS, SUPERCONDUCTORS...Magnetic field-induced electronic instability in bismuthIn the pres<strong>en</strong>ce of a reasonably large magnetic field, theelectric resistivity of bismuth is <strong>en</strong>hanced by five orders ofmagnitude with no sign of saturation. This feature, discoveredas early as 1928 by Kapitza, has escaped wide theoreticalatt<strong>en</strong>tion [Abrikosov, J. Phys. A 36, 9119 (2003)].Wh<strong>en</strong> a magnetic field exceeding 9 T is applied along thetrigonal axis of a bismuth crystal, the carriers are confinedto their lowest Landau level. In the case of electron-like carriers,this level has two sub-levels of opposite spins. Holelikecarriers , on the other hand, are spin-polarized. Rec<strong>en</strong>texperim<strong>en</strong>tal studies of bismuth [K. Behnia et al., Sci<strong>en</strong>ce11, 113012 (2009); L. Li et al. Sci<strong>en</strong>ce, 321, 547 (2008);B. Fauqué et al., Phys. Rev. B 79, 245124 (2009)] haveuncovered a number of <strong>en</strong>igmatic field scales beyond thisquantum limit.We have ext<strong>en</strong>ded previous measurem<strong>en</strong>ts of longitudinaland Hall resistivity of bismuth to 55 T. Our study has uncovereda new field scale in the vicinity of 40 T pointing to anunid<strong>en</strong>tified electronic instability. The signatures of electronicreorganization at this field in the experim<strong>en</strong>tal data,namely, a minimum in field-dep<strong>en</strong>d<strong>en</strong>ce of electric resistivity(see figure 90) and a peak in the Nernst response (foundusing the dc hybrid magnet in NHMFL-Tallahassee), are almostas drastic as the crossing of the quantum limit at 9 T.Our angular-dep<strong>en</strong>d<strong>en</strong>t resistivity studies establish that thisfield scale persists ev<strong>en</strong> wh<strong>en</strong> the field is strictly parallel tothe trigonal axis and, thus cannot be attributed to the oneparticle<strong>en</strong>ergy spectrum. Thus, this result constitutes themost solid experim<strong>en</strong>tal evid<strong>en</strong>ce available until now for afield-induced electronic instability caused by electronic interactionsin bulk bismuth.In bismuth, quantum oscillations of resistivity (theShubnikov-de Haas effect) are superimposed on a hugemonotonous background. The main period of oscillation(0.15 T −1 ), clearly visible in dρ/dB plots (figure 90(b)), isassociated with the cross section of the hole ellipsoid. Thepres<strong>en</strong>ce of the 40 T anomaly was checked in five Bi singlecrystals from differ<strong>en</strong>t sources.According to rec<strong>en</strong>t theoretical calculations [Alicea and Bal<strong>en</strong>ts,Phys. Rev. B 79, 241101 (2009); Sharlai and Mikitik,Phys. Rev. B 79, 081102 (2009)], the one-particle spectrumof bismuth for a field ori<strong>en</strong>ted close to the trigonal axis isremarkably complex. This is due to the implications of thecharge neutrality in a comp<strong>en</strong>sated system, the particularFermi surface topology and the relatively large Zeeman <strong>en</strong>ergy.According to these calculations, the field scales ofthe three electron ellipsoids are expected to pres<strong>en</strong>t a verysharp angular dep<strong>en</strong>d<strong>en</strong>ce wh<strong>en</strong> the field is slightly tiltedaway from the trigonal axis. On the other hand, if the fieldis strictly ori<strong>en</strong>ted along the trigonal axis, above B ∼ 10 T,no other field scale is expected in the one-particle picture.We have verified that tilting the field slightly away from thetrigonal axis has little effect on the field position of the 40 Tanomaly. The high-field anomaly is pres<strong>en</strong>t ev<strong>en</strong> wh<strong>en</strong> thefield is parallel to the high-symmetry axis and thus it cannotbe attributed to one of the three sharply anisotropic electronellipsoids.This field-induced electronic reorganization leads to a betterconductivity and an <strong>en</strong>hanced metallic behaviour, insharp contrast to the expected signatures of a d<strong>en</strong>sity-wavetransition. A version of such a transition is widely believedto occur in graphite in a similar ultra-quantum configuration[Yaguchi and Singleton, J. Phys.: Cond<strong>en</strong>s. Matter 21,34 (2009) for a review].Figure 90: Left: Magnetoresistance of three bismuth single crystals.Sample (a) was measured in a dc hybrid magnet and the twoothers in the pulsed magnet at LNCMI-Toulouse. The high-fieldminimum in resistivity occur far beyond the quantum limit. Right:Field-derivative of resistance a s function of B −1 . Quantum oscillationsare visible in addition to the newly discovered field scalemarked by arrows.Figure 91: Longitudinal and Hall resistivity as a function of B −1in a bismuth single crystal for differ<strong>en</strong>t tilt angles. The θ = 0curves are in red. The high-field anomaly shows little variationwith tilt angle.B. Vignolle, C. ProustB. Fauqué, K. Behnia (ESPCI, Paris)67


METALS, SUPERCONDUCTORS... 2009Magnetic oscillations in a linear chain of comp<strong>en</strong>sated orbitsDue to their rather simple Fermi surface, organicmetals provide a rich playground for the investigationof quantum oscillations in physics. In that respect,the most well known example is provided by κ-(BEDT-TTF) 2 Cu(NCS) 2 (where BEDT-TTF stands for bisethyl<strong>en</strong>edithio-tetrathiafulval<strong>en</strong>e)which can be regarded asthe experim<strong>en</strong>tal realization of the Fermi surface consideredby Pippard in the early sixties for his model. In theext<strong>en</strong>ded zone scheme, such a Fermi surface is composedof closed hole orbits and quasi-one dim<strong>en</strong>sional sheets coupledby magnetic breakdown. This kind of Fermi surfaceyields quantum oscillations spectra with numerous frequ<strong>en</strong>cycombinations that cannot be accounted for by thesemi-classical model of Falicov and Stachowiak. This ph<strong>en</strong>om<strong>en</strong>onwhich has g<strong>en</strong>erated great interest is g<strong>en</strong>erally attributedto either the formation of Landau bands and/or oscillationsof the chemical pot<strong>en</strong>tial in a magnetic field.In the case where the effective masses linked to electronandhole-type orbits are the same (m ∗ e = m ∗ h), calculationsdemonstrate that chemical pot<strong>en</strong>tial oscillations vanish forsuch a Fermi surface. More g<strong>en</strong>erally, in the case wherem ∗ e and m ∗ hare differ<strong>en</strong>t, these oscillations are significantlydamped, all the more if the magnetic breakdown field issmall, as evid<strong>en</strong>ced in figure 93.Figure 92: Calculated Fermi surface of the Bechgaard salt(TMTSF) 2 NO 3 in the temperature range below the anion orderingand above the spin d<strong>en</strong>sity wave cond<strong>en</strong>sation, according toKang et al. [EPL 29 635 (1995)]. Solid blue and red lines arecomp<strong>en</strong>sated hole and electron orbits, respectively. This Fermisurface achieves linear chains of comp<strong>en</strong>sated orbits.Contrary to the above m<strong>en</strong>tioned example, the Fermi surfaceof numerous organic metals is composed of comp<strong>en</strong>satedelectron- and hole-type closed orbits, yieldingmany frequ<strong>en</strong>cy combinations as well, as far as ShubnikovdeHaas oscillations are concerned. We have computedthe field and temperature dep<strong>en</strong>d<strong>en</strong>ce of the de Haas-vanAlph<strong>en</strong> oscillations spectra of an ideal two-dim<strong>en</strong>sionalmetal whose Fermi surface achieves a linear chain ofsuccessive electron- and hole-type comp<strong>en</strong>sated orbits.Such a topology is realized e.g. in the Bechgaard salt(TMTSF) 2 NO 3 (where TMTSF stands for tetra-methyltetra-sel<strong>en</strong>o-fulval<strong>en</strong>e)in the temperature range in-betwe<strong>en</strong>the anion ordering temperature and the spin d<strong>en</strong>sity wavecond<strong>en</strong>sation (see figure 92).Figure 93: Field dep<strong>en</strong>d<strong>en</strong>ce of the chemical pot<strong>en</strong>tial for Fermisurface such as in figure 92 for m ∗ e = m 0 and m ∗ h = 2.5m 0 (m ∗ e andm ∗ h are the electron and hole orbit effective mass, respectively; m 0is the free electron mass) at a reduced temperature t = 10 −4 (t = T× k B m 0 A 0 /2π 2 , where A 0 is the unit cell area). b is the reducedmagnetic field (b = B × eA 0 /2π), b 0 is the reduced magneticbreakdown field. The inset compares the chemical pot<strong>en</strong>tial oscillationsfor two electron orbits and two comp<strong>en</strong>sated orbits with,respectively, the same effective masses as in the main panel, in theabs<strong>en</strong>ce of magnetic breakdown (b 0 →∞).It appears from the analysis of the numerical resolutionof Landau levels, including the electron-hole band interaction,that the Lifshits-Kosevich semiclassical formalismcan be applied for the first harmonic, provided magneticbreakdown orbits, although with higher effective masses,are tak<strong>en</strong> into account. The resulting high order terms canlead to appar<strong>en</strong>t temperature-dep<strong>en</strong>d<strong>en</strong>t effective mass forclean crystals in the high B/T limit in the case where onlyone effective mass is considered for the data analysis, as itis usually done. For example, in the abs<strong>en</strong>ce of magneticbreakdown, m ∗ = min(m ∗ e, m ∗ h) in the low field range whilem ∗ = √ m ∗ em ∗ hat high field.On the contrary, strong deviation from the Lifshits-Kosevich behavior is observed for the second harmonic.The main feature of this latter compon<strong>en</strong>t being the zeroamplitude occurring at a B/T value dep<strong>en</strong>ding on the ratioof the two effective masses (m ∗ h /m∗ e), only, indep<strong>en</strong>d<strong>en</strong>t ofthe magnetic breakdown field value.A. AudouardJ.-Y. Fortin (Institut Jean Lamour, Nancy)68


2009 METALS, SUPERCONDUCTORS...Coexist<strong>en</strong>ce of closed orbit and quantum interferometer with the same crosssection in the organic metal β”-(BEDT-TTF) 4 (H 3 O)[Fe(C 2 O 4 ) 3 ]·C 6 H 4 Cl 2The family of quasi-two-dim<strong>en</strong>sional charge transfer saltsβ”-(BEDT-TTF) 4 (A)[M(C 2 O 4 ) 3 ]Solv (where BEDT-TTFstands for bis-ethyl<strong>en</strong>edithio-tetrathiafulval<strong>en</strong>e, A is amonoval<strong>en</strong>t cation, M is a trival<strong>en</strong>t cation and Solv is asolv<strong>en</strong>t) have raised great interest in particular because ityielded, more than t<strong>en</strong> years ago, the first organic superconductorat ambi<strong>en</strong>t pressure with magnetic ions.due to the relatively narrow field range in which these latteroscillations can be observed (B > 20 T).The Lifshitzs-Kosevich formalism accounts for the fieldand temperature dep<strong>en</strong>d<strong>en</strong>ce of both the SdH and dHvAdata over all the explored range. However, a very weak thermaldamping of the Fourier compon<strong>en</strong>t F b , with the highestamplitude, is evid<strong>en</strong>ced for SdH spectra above about 6 K(see figure 95). As a result, magnetoresistance oscillationsare observed at temperatures higher than 30 K. Taking intoaccount the temperature dep<strong>en</strong>d<strong>en</strong>ce of the scattering rate,this feature, which is not observed for dHvA oscillations(recorded up to 15 K), is in line with the coexist<strong>en</strong>ce, at leastin the temperature range around 6 K, of a closed orbit b anda symmetric (i.e. with a zero effective mass) quantum interfer<strong>en</strong>cepath with the same area (keeping in mind that dHvAoscillations are only s<strong>en</strong>sitive to the d<strong>en</strong>sity of states). Thisresult, which cannot be interpreted in the framework of theFermi surface displayed in figure 94(d), points to a Fermisurface reconstruction in this compound. For details, see[Vignolles et al. Eur. Phys. J. B 71 203 (2009)].Figure 94: (a) Field-dep<strong>en</strong>d<strong>en</strong>t interlayer resistance ofβ”-(BEDT-TTF) 4 (H 3 O)[Fe(C 2 O 4 ) 3 ]·C 6 H 4 Cl 2 for θ = 0 ◦ (θ is theangle betwe<strong>en</strong> the field direction and the normal to the conductingplane). (b) Fourier analysis deduced from the oscillatory part ofthe magnetoresistance displayed in the inset. The field range is18-54 T. Marks are calculated with F a = 74 T and F b = 348 T. (c)Magnetic torque at θ = 29 ◦ . Corresponding Fourier analysis aredisplayed in the inset. The field range is 30-53.5 T and 38-53.5 Tbelow and above 9 K, respectively. (d) Textbook case of Fermisurface accounting for the frequ<strong>en</strong>cies a, b and b-a.Magnetoresistance and magnetic torque of the salt with A= H 3 O + , M = Fe 3+ and Solv = C 6 H 4 Cl 2 have be<strong>en</strong> investigatedin pulsed magnetic fields of up to 54 T. Shubnikov-deHaas (SdH) oscillations reveal three basic frequ<strong>en</strong>cies F a ,F b and F b−a , which, in line with band structure calculations,can be interpreted on the basis of three comp<strong>en</strong>sated closedorbits originating from a hole orbit with an area equal to thatof the first Brillouin zone (see figure 94). Only F a and F bare observed in de Haas-van Alph<strong>en</strong> (dHvA) spectra, likelyFigure 95: Temperature dep<strong>en</strong>d<strong>en</strong>ce of the amplitude of the boscillations for dHvA and SdH data. Empty and solid symbolscorrespond to a mean field value of 44.6 T and 30 T/cos(θ), respectively(θ is the angle betwe<strong>en</strong> the field direction and the normal tothe conducting plane). Solid lines are best fits of the Lifshitzs-Kosevichformula. A zero-effective mass and a temperature-dep<strong>en</strong>d<strong>en</strong>tscattering rate are considered for the SdH data in the hightemperature range.D. Vignolles, A. AudouardV.N. Laukhin, E. Canadell (ICMAB, Barcelona, Spain), E.B. Yagubskii (IPCP, Chernogolovka, Russian Federation)69


METALS, SUPERCONDUCTORS... 2009Metal-non-metal transition in the charge transfer salt(BEDT-TTF) 8 [Hg 4 Br 12 (C 6 H 5 Br) 2 ]At room temperature and ambi<strong>en</strong>t pressure, all the membersof the family of charge transfer salts (BEDT-TTF) 8 [Hg 4 X 12 (C 6 H 5 Y) 2 ] (where X, Y = Cl, Br and BEDT-TTF stands for bis-ethyl<strong>en</strong>edithio-tetrathiafulval<strong>en</strong>e) areisostructural. According to band structure calculations,their Fermi surface is composed of one electron and onehole comp<strong>en</strong>sated orbit, coupled by magnetic breakdown(MB). However, ev<strong>en</strong> though a metallic ground-state is observedfor X = Cl, a metal-non metal transition occurs as thetemperature is lowered for X = Br, as displayed in figure 96.(2003), Audouard et al. Euro. Phys. Lett. 71 783 (2005)]),only few MB orbits are observed for X = Br. This is due toa larger MB gap betwe<strong>en</strong> electron and hole orbits in the lattercase, in line with band structure calculations. The mostsali<strong>en</strong>t feature is the sizeable decrease of the effective masslinked to the comp<strong>en</strong>sated orbits observed as the appliedpressure increases (roughly a factor of two in the exploredrange). In addition, the effective mass scales with the coeffici<strong>en</strong>t(A) of the T 2 law. Such a behaviour is reminisc<strong>en</strong>t ofa Brinkman-Rice sc<strong>en</strong>ario which predicts the diverg<strong>en</strong>ce ofthe effective mass as approaching a Mott transition. In thatrespect, no structural phase transition can be inferred fromX-ray data down to 100 K at ambi<strong>en</strong>t pressure, for X = Br.Figure 96: Temperature dep<strong>en</strong>d<strong>en</strong>ce of the interlayer resistivityfor (a) X = Cl and (b) X = Br. Ev<strong>en</strong> though the two compounds areisostructural at room temperature, a metal-non metal transition isobserved for X = Br at low pressure. T 2 dep<strong>en</strong>d<strong>en</strong>ce of the interlayerresistivity at low temperature for (c) the metallic compoundwith X = Cl and (d) the pressure-induced metallic state of X =Br. The Fermi surface for X = Br is displayed in the inset of (b).Electron (red) and hole (blue) orbits are comp<strong>en</strong>sated.We have studied the interlayer magnetoresistance of the twocompounds with Y = Br under applied pressure of up to 1.1GPa. For X = Cl, a metallic ground-state is observed in allthe pressure range explored while for X = Br, a pressureinducedmetallic state is observed at a few t<strong>en</strong>th of GPa.For both compounds, a T 2 variation of the zero-field resistance(ρ = ρ 0 + A×T 2 ), typical of correlated Fermi liquids,is observed in the metallic state. Shubnikov-de Haas (SdH)oscillations are observed for both X = Cl (see figure 97)and X = Br. While many frequ<strong>en</strong>cy combinations, typicalof coupled orbits networks are observed in the former case(for more details see [Vignolles et al. Eur. Phys. J. B 31 53Figure 97: (a) Field-dep<strong>en</strong>d<strong>en</strong>t resistance for X = Cl at 1.1 GPaand (b) corresponding Fourier spectra. Label a stands for the comp<strong>en</strong>satedorbits (see figure 96), the other labels corresponds to eitherfrequ<strong>en</strong>cy combinations or Fermi surface pieces located in--betwe<strong>en</strong> the orbits. (c) The coeffici<strong>en</strong>t (A) of the T 2 law of thezero-field resistivity scales with the square of the effective mass(m ∗ ) deduced from SdH oscillations.D. Vignolles, A. Audouard, F. Duc, M. NardoneR.B. Lyubovskii, R.N. Lyubovskaya (IPCP, Chernogolovka, Russian Federation), E. Canadell (ICMAB, Barcelona,Spain)70


2009 METALS, SUPERCONDUCTORS...Magnetic torque experim<strong>en</strong>ts on the magnetic-field-induced organicsuperconductor λ-(BETS) 2 FeCl 4Layered organic superconductors have upper critical fieldsexceeding the theoretical Pauli limit for superconductivitywh<strong>en</strong> the magnetic field is applied parallel to the layers.Theory predicts th<strong>en</strong> the possibility of a Fulde-Ferrel-Larkin-Ovchinnikov (FFLO) superconducting state[Fulde and Ferrel, Phys. Rev. 135, A550 (1964);Larkin and Ovchinnikov, Sov. Phys. JETP 20, 762(1965)]. Besi<strong>des</strong> κ-(BEDT-TTF) 2 Cu(NCS) 2 , the two dim<strong>en</strong>sionalfield-induced superconductor λ-(BETS) 2 FeCl 4 ,where BETS is bis(ethyl<strong>en</strong>edithio)tetrasel<strong>en</strong>afulval<strong>en</strong>e, is acandidate which fulfils all necessary conditions. Wh<strong>en</strong> themagnetic field is applied parallel to the metallic layers, asuperconducting phase appears above 17 T below 1 K.In our first experim<strong>en</strong>t we focused on the critical field at17 T. Figure 98 shows torque data tak<strong>en</strong> at differ<strong>en</strong>t temperaturesduring field sweeps. Surprisingly, a broad kinklikeanomaly appears only above 22 T indicating the transitioninto the field-induced superconducting state. Below200 mK a pronounced hysteresis appears. The experim<strong>en</strong>tsshow no evid<strong>en</strong>ce for additional phase transitions withinthe superconducting state. The phase diagram clearly differsfrom that reported by Uji et al. A misalignm<strong>en</strong>t of thesample can be ruled out. A possible explanation may befound in the rather rapid cooling conditions in our experim<strong>en</strong>twhich is known to cause anion-disorder effects in 1Dorganic superconductors. The result stimulates further experim<strong>en</strong>tsunder more controlled experim<strong>en</strong>tal conditions.This field-induced superconductivity is well understoodin the framework of the Fischer theory, based on theJaccarino-Peter effect. Uji et al. reported possible FFLOstates at the two critical fields based on dip structures inthe resistivity [Uji et al., Phys. Rev. Lett. 97, 157001(2006) and refer<strong>en</strong>ces therein]. This motivated us to lookfor a thermodynamic phase transition betwe<strong>en</strong> the homog<strong>en</strong>eoussuperconducting phase and the FFLO states bymeans of magnetic torque experim<strong>en</strong>ts using a capacitancecantilever technique. The probe was equipped with a rotator,which allowed us to align the layers parallel to the fielddirection with a precision of 0.001 ◦ . Single crystals of λ-(BETS) 2 FeCl 4 were grown by the standard electrochemicaloxidation technique.Figure 98: Magnet torque of λ-(BETS) 2 FeCl 4 is plotted as afunction of field at differ<strong>en</strong>t temperatures.I. SheikinR. Lortz (The Hong Kong University of Sci<strong>en</strong>ce and Technology, Kowloon, Hong Kong), Y. Nakazawa ( University ofOsaka, Osaka, Japan), B. Zhou, A. Kobayashi, H. Kobayashi (Nihon University, Tokyo, Japan)71


METALS, SUPERCONDUCTORS... 2009Temperature and magnetic field dep<strong>en</strong>d<strong>en</strong>ce of domain wall width and periodof Condon domain structure in AgDiamagnetic instability of electron gas in normal metals underquantizing magnetic field and low temperature is a resultof strong electron correlations induced by the magneticfield. It gives rise to a phase transition with formation ofcomplex domain patterns (Condon domains).hysteresis in magnetization curves, exist<strong>en</strong>ce of persist<strong>en</strong>tcurr<strong>en</strong>ts which results in a discontinuity of magnetic inductionalong the interface boundaries of regular domainpatterns. Still, there remain op<strong>en</strong> fundam<strong>en</strong>tal questionsrelated to the formation of Condon domain phase. As anexample, the important information about the size of thedomains, the domain wall width and surface <strong>en</strong>ergy of theinterface boundaries is still lacking. In our studies [N. Logoboyand W. Joss, Solid State Comm. 149, 2007 (2009)]we offer a way to calculate the expected values of domainwall width and period of the domain structure by means ofmeasurem<strong>en</strong>t of the value of the jump of magnetic inductionat the domain wall δB (figure 99 and figure 100).Figure 99: Temperature dep<strong>en</strong>d<strong>en</strong>ce of the DW width δ (a) andperiod of the domain structure D (b) at the conditions of the experim<strong>en</strong>t[Kramer et al., Phys. Rev. Lett. 95, 267209 (2005)].The solid lines correspond to the theory, the circles are calculatedfrom the temperature dep<strong>en</strong>d<strong>en</strong>ce of the measured jump of magneticinduction at the interface boundaries.The diamagnetic phase transition has received rec<strong>en</strong>tlymuch att<strong>en</strong>tion due to a number of unusual ph<strong>en</strong>om<strong>en</strong>a forthe physics of diamagnetism, e.g. formation of complexbranch structures, strong dep<strong>en</strong>d<strong>en</strong>ce of magnetic phase diagramson Fermi-surface topology, pres<strong>en</strong>ce of diamagneticFigure 100: Magneticfield dep<strong>en</strong>d<strong>en</strong>ce of the DW width δ (a)and period of the domain structure D (b) at the conditions of theexperim<strong>en</strong>t [Kramer et al., Phys. Rev. Lett. 95, 267209 (2005)].The solid lines correspond to the theory, the circles are calculatedfrom the temperature dep<strong>en</strong>d<strong>en</strong>ce of the measured jump of magneticinduction at the interface boundaries.W. JossN. Logoboy (The Racah Institute of Physics, The Hebrew University of Jerusalem, Jerusalem, Israel and The Instituteof Superconductivity, Departm<strong>en</strong>t of Physics, Bar-Ilan University, Ramat-Gan, Israel)72


2009 METALS, SUPERCONDUCTORS...Intrinsic diamagnetic l<strong>en</strong>gth scales of Condon domain phase in BeMagnetic quantum oscillations which are the result of Landauquantization of the quasiparticle spectrum are a powerfultool in investigation of Fermi surfaces of wide spectrumof substances, including traditional normal metals, lowdim<strong>en</strong>sionalsystems and superconductors. The increasein the amplitude of the dHvA oscillations at low temperatureunder quantizing magnetic field gives rise to the magneticinstability with formation of nonuniform diamagneticphase (Condon domains). The low curvature of the quasi-2D ’cigar’-like part of Fermi surface of beryllium results inrelatively high amplitude of dHvA oscillations and makesit favorable to observe the diamagnetic instability in beryllium.We show that the properties of correlated electrons innormal metals at the conditions of diamagnetic instabilitywh<strong>en</strong> the differ<strong>en</strong>tial magnetic susceptibility a =µ 0 max{∂ ˜M/∂B} ≥ 1 ( ˜M is oscillating part of the magnetizationand B is magnetic induction of the sample) can be<strong>des</strong>cribed by the effective <strong>en</strong>ergy functionalthe size and the shape of the sample, and short-range electroninteraction on the scale of r c which gives rise to positive<strong>en</strong>ergy of interface boundaries.Thus, for a plate-like sample of thickness L, the minimizationof total free <strong>en</strong>ergy of periodic domain structureG PDS = G d−d + G σ , containing two terms, e. g. dipoledipole<strong>en</strong>ergy G d−d = (7/π 3 )ζ(3)y 2 0D, where ζ(3) is zetafunction,and surface <strong>en</strong>ergy of separation of two domainsG σ = (2L/D)σ (σ is the surface <strong>en</strong>ergy of a single domainwall), allows to calculate the steady-state period of the domainstructureD = 25/2 π(r c L) 1/2[7ζ(3)] 1/2 (sec 2 y2 02 − a)1/4 . (14)We calculate the expected values of domain wall width andperiod of the domain structure by use of measured valuesof the jump of magnetic induction at the domain wall δB(figure 101).G = − 1 2 K sin2 Θ + 1 2 A(∂ ζΘ) 2 . (12)In Eq. (12) we use a variable Θ = πy/2y 0 where y = 4πkMis a reduced magnetization, k = 2πF/(B a ) 2 = 2π/∆H, F =(F h +F w )/2 is average fundam<strong>en</strong>tal frequ<strong>en</strong>cy of the dHvAoscillations (F h = 970.9 T and F w = 942.2 T are two fundam<strong>en</strong>talfrequ<strong>en</strong>cies corresponding to two extremal crosssectionsof ’cigar’-like Fermi surface of Be), ∆H is dHvAperiod. The uniform magnetization y 0 = y 0 (a) is giv<strong>en</strong> inexplicit form by equation y 0 = asin y 0 . Parameters K andA in Eq. (12) are defined asK = 4asin 2 y 02 (1 − acos2 y 02 ), A = a(2r cy 0 /π) 2 . (13)The first term in RHS of Eq. (12) is analogous to the easyaxiscrystallographic anisotropy (K > 0), while the gradi<strong>en</strong>tterm (ζ is coordinate) accounts for the short-range correlationson the scale of the cyclotron radius r c and correspondsto the exchange interaction in the physics of spinmagnetism. It follows from Eq. (12) that there is a closeanalogy betwe<strong>en</strong> easy-axis anisotropy ferromagnetic sampleand the system which shows the diamagnetic instability.Thus, the problem of the diamagnetic l<strong>en</strong>gth scales can besolved by the standard methods of the physics of magneticmaterials.We assume the exist<strong>en</strong>ce of periodic domain structure withalternative magnetization ±y 0 in neighboring domains. Periodof the domain structure D is defined by competitionbetwe<strong>en</strong> long-range dipole-dipole interaction dep<strong>en</strong>d<strong>en</strong>t onFigure 101: (a) Temperature dep<strong>en</strong>d<strong>en</strong>ce of the domain wallwidth δ = δ(T ) and (b) period of the Condon domain structureD = D(T ) at fixed value of B a = 2.642 T and Dingle temperaturesT D = 1.9 K in beryllium plate-like sample with the width L = 1.8mm. Circles (triangles) repres<strong>en</strong>t the diamagnetic l<strong>en</strong>gth-scalescalculated from the data [G. Solt and V. S. Egorov, Physica B 318,231 (2002)] wh<strong>en</strong> heating (cooling).W. JossN. Logoboy (The Racah Institute of Physics, The Hebrew University of Jerusalem, Jerusalem, Israel and The Instituteof Superconductivity, Departm<strong>en</strong>t of Physics, Bar-Ilan University, Ramat-Gan, Israel)73


METALS, SUPERCONDUCTORS... 200974


2009Magnetic Systems75


2009 MAGNETIC SYSTEMSY b 3+ → Er 3+ up-conversion luminesc<strong>en</strong>ce under high pressure and pulsedmagnetic fieldsEr 3+ -doped materials are ess<strong>en</strong>tial for laser application,displays, infrared detectors as well as in telecommunicationusing it in optical fibre amplifiers or other planar wavegui<strong>des</strong>.Therefore, the understanding of the effect of an externalmagnetic field on the photoluminesc<strong>en</strong>ce (PL) bandsof Er 3+ is important in order to obtain information aboutthe electronic structure, particularly, the Zeeman sublevelstructure forming the excited and ground state manifold.We have investigated the Zeeman splitting of the 4 S 3/2 → 4I 15/2 Er 3+ transition, which is responsible of the gre<strong>en</strong>luminesc<strong>en</strong>ce of high-quality single-crystal thin layers ofKY (WO 4 ) 2 : Er 3+ ,Y b 3+ in pulsed magnetic fields as afunction of hydrostatic pressure by resonant up-conversionspectroscopy (figure 102). The gre<strong>en</strong> Er 3+ PL was resonantlyexcited via up-conversion processes after Y b 3+ andEr 3+ excitation in the near infrared around 980 nm usinga tunable titanium-sapphire laser. Under the applied magneticfield, the <strong>en</strong>ergy resonance betwe<strong>en</strong> the Y b 3+ levelsand the Er 3+ changes by the Zeeman effect. The upconversionprocess can be completely suppressed and therefore,a precise tuning of the laser excitation wavel<strong>en</strong>gth tocomp<strong>en</strong>sate the Zeeman splitting of Y b 3+ ions was necessaryin order to assure the resonance at high magnetic fields.Up-conversion process is a way to transform low <strong>en</strong>ergyphotons into higher <strong>en</strong>ergy photons differ<strong>en</strong>t from secondharmonicg<strong>en</strong>eration which is commonly used in solid-statelasers. The most effici<strong>en</strong>t up-conversion system is that onebased on Er 3+ and Y b 3+ . It is possible to observe, by th<strong>en</strong>aked eye, visible emission from Er 3+ after Y b 3+ excitationin the near-infrared.Figure 103: Pressure effect on the gre<strong>en</strong> photoluminesc<strong>en</strong>ce of4 S 3/2 → 4 I 15/2 Er 3+ transition at two differ<strong>en</strong>t external magneticfields.Figure 102: Low temperature Zeeman splitting of Er 3+ photoluminesc<strong>en</strong>cespectra in KY (WO 4 ) 2 : Er 3+ ,Y b 3+ for a 5.0 T magneticfield applied parallel to the crystallographic b axis correspondingto the lowest lying Kramers’ doublet of the 4 S 3/2 to the splitKramers’ doublets of the 4 I 15/2 ground state. The insets showdetails of some relevant peaks.The results indicate that pressure induces a linear redshiftfor all peaks at the two selected magnetic fields (figure 103).The pressure induced shift rates are almost indep<strong>en</strong>d<strong>en</strong>t ofthe magnetic field making this material suitable as s<strong>en</strong>sor.In fact, the magnetic-field splitting mainly dep<strong>en</strong>ds on thefield int<strong>en</strong>sity and thus can be used as magnetic probes andthe highest <strong>en</strong>ergy peak position which dep<strong>en</strong>ds on bothmagnetic field and pressure can be used in combinationwith the Zeeman splitting to unambiguously determine thepressure and magnetic field.H<strong>en</strong>ce, KY (WO 4 ) 2 crystals doped with Y b 3+ and Er 3+ areexcell<strong>en</strong>t systems for using as probes of high magneticfield and high pressure conditions through spectroscopicproperties of the Er 3+ gre<strong>en</strong> photoluminesc<strong>en</strong>ce via upconversion.The PL spectrum at low temperature consistsof a series of Zeeman split peaks, which are distinctly s<strong>en</strong>sitiveto the magnetic field int<strong>en</strong>sity and pressure. This behaviorallows us to id<strong>en</strong>tify selected peaks by <strong>en</strong>ergy andint<strong>en</strong>sity that provi<strong>des</strong> an unambiguous determination of Band P simultaneously through the peak position E (B, P).The measured shift rates make it suitable for using as doublymagnetic and pressure s<strong>en</strong>sor [Vali<strong>en</strong>te et al., acceptedin High Pressure Research].M. Millot, S. George and J.M. BrotoR. Vali<strong>en</strong>te, J. Gonzalez, F. Rodriguez (DCITIMAC, Santander, Spain), S. Garca-Revilla ( ESI, Bilbao, Spain), Y.Romanyuk (EMPA, Düb<strong>en</strong>dorf, Switzerland) and M. Pollnau (MESA+, Enschede, Netherland)77


MAGNETIC SYSTEMS 2009Nd 3+ crystal-field studies of weakly doped Nd 1−x Ca x MnO 3Manganites RMnO 3 compounds based on lanthani<strong>des</strong> (R)are antiferromagnetic systems with important Jahn-Tellerdistortions. Substitution of lanthani<strong>des</strong> by Ba, Sr, or Caleads to appearance of double exchange interactions, reductionof Jahn-Teller-type distortions and simultaneous observationof metallic and ferromagnetic character with increasingmolar fraction x (R 1−x A x MnO 3 , A = Ba, Sr, orCa). In this work, Nd 3+ ions crystal field (CF) excitationsin Nd 1−x Ca x MnO 3 (x = 0.025, 0.05 and 0.1) singlecrystals have be<strong>en</strong> investigated using infrared transmissionspectroscopy at differ<strong>en</strong>t temperatures and external magneticfields and compared to undoped NdMnO 3 .Our study reveals the pres<strong>en</strong>ce of a magnetic phase separationin the doped samples. As a consequ<strong>en</strong>ce of dopingby calcium, we report the detection of two sets ofCF levels, as already observed in Nd 1−x Sr x MnO 3 [see S.Jandl et al., Phys. Rev. B 71, 024417 (2005) and S.Jandl et al., ibid 72, 024423 (2005)]. One is associatedwith unperturbed sites related to the NdMnO 3 antiferromagnetismwith its typical Zeeman splitting below Neeltemperature, and a second one is linked to perturbed sitesin the vicinity of the Ca 2+ cations where local A-typeantiferromagnetism is suppressed. While the <strong>en</strong>ergy differ<strong>en</strong>cesbetwe<strong>en</strong> the two sets are within the uncertaintyvalues of the CF parameters that <strong>des</strong>cribe the NdMnO 3CF Hamiltonian and predict the CF levels, their detectionstr<strong>en</strong>gth<strong>en</strong>s the role of local probe the rare-earth CF levelsplay in manganite compounds. Finally, under appliedexternal magnetic field, Zeeman splittings are observed inNdMnO 3 and Nd 0.975 Ca 0.025 MnO 3 , while they are maskedin Nd 0.95 Ca 0.05 MnO 3 and Nd 0.9 Ca 0.1 MnO 3 . The latter resultsare due to doping-induced band broad<strong>en</strong>ing and possibletwining.The Zeeman splitting well-resolved at lower doping d<strong>en</strong>sitiesis demonstrated in Fig. 104, where the middle-infraredtransmission spectra of investigated samples tak<strong>en</strong> withoutand with the externally applied magnetic field (parts A andB) are pres<strong>en</strong>ted. For details see, S. Jandl et al., J. Magn.Magn. Mater. 321, 3607 (2009).Figure 104: Transmission spectra showing 4 I 9/2 → 4 I 11/2 Nd 3+transitions in Nd 1−x Ca x MnO 3 at T = 1.8 K: x = 0 (a), x = 0.025(b), x = 0.05 (c) and x = 0.1 (d) measured at (A) B = 0 T andB = 12 T. ∗ indicates the new CF excitations that are due to thedoping. The Zeem<strong>en</strong> splitting is well-resolved at lower conc<strong>en</strong>trations(x = 0 and 0.025) but masked at higher doping d<strong>en</strong>sities.M. OrlitaS. Jandl (University of Sherbrooke, Canada), A. A. Mukhin, V. Yu. Ivanov (G<strong>en</strong>eral Physics Institute of the RussianAcademy of Sci<strong>en</strong>ces, Moscow, Russia), A. Balbashov (Moscow Power Engineering Institute, Moscow, Russia)78


2009 MAGNETIC SYSTEMSMagnetotransport in a disordered Zn 1-x Mn x GeAs 2 alloyMagnetotransport studies in high magnetic fields are a veryeffective tool for studying the interplay betwe<strong>en</strong> the electronicand magnetic properties of magnetic materials. Inthis work the results of the magnetoresistance and Hall effectstudies in Zn 1-x Mn x GeAs 2 (0.053 ≤ x ≤ 0.182) are pres<strong>en</strong>ted.The investigated compound Zn 1-x Mn x GeAs 2 belongsto the II-IV-V 2 group of diluted magnetic semiconductors.Our rec<strong>en</strong>t studies of magnetic properties of thisalloy [L. Kilanski, et al., Acta Phys. Pol. A 114, 1151(2008)] showed that the transition from a Curie-Weiss paramagnetinto a ferromagnetic material with Curie temperaturesexceeding 300 K occurs in this system for x ≥ 0.06.The high Curie temperature observed in this alloy is probablyconnected with the pres<strong>en</strong>ce of nano-sized MnAs grainsin the crystal.The results of Hall effect investigations in the form of magneticfield dep<strong>en</strong>d<strong>en</strong>ce of the off-diagonal resistivity t<strong>en</strong>sorcompon<strong>en</strong>t ρ xy are pres<strong>en</strong>ted in figure 106. It is interestingto note that in the Zn 1-x Mn x GeAs 2 crystals we do notobserve the anomalous Hall effect, a ph<strong>en</strong>om<strong>en</strong>on widelyobserved in ferromagnetic semiconductors. The ρ xy (B)dep<strong>en</strong>d<strong>en</strong>ce in the case of ferromagnetic Zn 1-x Mn x GeAs 2(x ≥ 0.06) crystals showed the pres<strong>en</strong>ce of large nonlinearitiesat temperatures lower than 9 K. The b<strong>en</strong>ding of theρ xy (B) curve is the most promin<strong>en</strong>t in the case of the samplewith the highest conc<strong>en</strong>tration of Mn ions. Such behaviormay indicate the pres<strong>en</strong>ce of two types of conductingcarriers influ<strong>en</strong>cing the carrier transport in this material.It is well established that the magnetic properties of crystalshave a significant influ<strong>en</strong>ce on the electron transport inZn 1-x Mn x GeAs 2 samples with differ<strong>en</strong>t Mn cont<strong>en</strong>t. Apartfrom changes in the basic transport properties such as carrierconc<strong>en</strong>tration and resistivity, we have also observed asignificant differ<strong>en</strong>ces in the high field magnetoresistanceand the Hall effect. The magnetic field dep<strong>en</strong>d<strong>en</strong>ce of theresistivity t<strong>en</strong>sor compon<strong>en</strong>t ρ xx recorded at T ≈ 1.45 K arepres<strong>en</strong>ted in figure 105.In the case of the paramagnetic Zn 0.947 Mn 0.053 GeAs 2 samplewe observe a small negative magnetoresistance saturatingat moderate magnetic fields of about B ≈ 50 kOe. Theorigin of this behavior of the magnetoresistance curve is thespin-disorder scattering of the conducting carriers on theMn magnetic mom<strong>en</strong>ts embedded inside the semiconductorhost. It may be added that the negative magnetoresistance isobserved only at temperatures lower than 5 K. The positivecontribution to the magnetoresistance observed clearly athigher temperatures results from the orbital carrier movem<strong>en</strong>tin the pres<strong>en</strong>ce of the external magnetic field. Thispositive contribution competes at low temperatures with theeffect of spin disorder scattering causing the curves to showa minima.In the case of the two ferromagnetic Zn 1-x Mn x GeAs 2 sampleswith x > 0.06 we observed negative magnetoresistancewith an amplitude much larger than in the case of the paramagneticcrystal. The observed effect is interpreted as agiant magnetoresistance due to the polarization of conductingcarriers inside ferromagnetic grains (similar to that observedin the case of granular ferromagnets). The amplitudeof the giant magnetoresistance is highly compositiondep<strong>en</strong>d<strong>en</strong>t due to changes in the conc<strong>en</strong>tration of magneticinclusions in the material.Figure 105: Magnetoresistance curves obtained at T ≈1.45 K forZn 1-x Mn x GeAs 2 crystals with differ<strong>en</strong>t chemical composition x.Figure 106: Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of the Hall resistivity ρ xymeasured at T ≈ 1.45 K for Zn 1-x Mn x GeAs 2 crystals with differ<strong>en</strong>tchemical composition x.D. K. MaudeL. Kilanski, W. Dobrowolski (Institute of Physics Polish Academy of Sci<strong>en</strong>ce, Warsaw, Poland),S. A. Varnavskiy, S. F. Mar<strong>en</strong>kin (Kurnakov Institute of G<strong>en</strong>eral and Inorganic Chemistry RAS, Moscow, Russia)79


MAGNETIC SYSTEMS 2009Anomalous Hall effect in (Ge,Mn)Te-(Sn,Mn)Te spin-glasslike crystalsThe anomalous Hall effect shows a direct interplay betwe<strong>en</strong>magnetic and electronic properties of solid. Inthis contribution, we show the results of the anomalousHall effect studies in the series of Ge 1-x-y Sn x Mn y Tecrystals with chemical composition 0.090≤x≤0.142 and0.012≤y≤0.115 in the temperature range 1.4≤T ≤200 Kand magnetic fields up to 130 kOe. Rec<strong>en</strong>t investigation ofmagnetic properties of this alloy [Kilanski, et al., J. Appl.Phys. 105, 103901 (2009)] showed the pres<strong>en</strong>ce of the spinglasslikestate with transition temperatures T SG ≤60 K.R S is probably more complex function of both magneticand electrical properties than just chemical compositionof the alloy. It may be noted that the obtained anomalousHall constants are similar to the ones observed in the literaturefor other IV-VI based diluted magnetic semiconductorslike Sn 1-x Mn x Te and Ge 1-x-y Mn x Eu y Te [Brodowska, et al.,Journal of Alloys and Compounds. 423, 205 (2006)].The magnetic field dep<strong>en</strong>d<strong>en</strong>ce of the resistivity t<strong>en</strong>sorcompon<strong>en</strong>t ρ xy for Ge 0.815 Sn 0.091 Mn 0.094 Te crystal at temperaturerange 4.3≤T ≤50 K is pres<strong>en</strong>ted in figure 107. Thesharp increase of ρ xy (B) dep<strong>en</strong>d<strong>en</strong>ce visible in the low fieldregion is the manifestation of the anomalous Hall effect (attemperatures lower than T SG ). The off-diagonal resistivityρ xy (B) is a sum of ordinary R H and anomalous R S contribution<strong>des</strong>cribed by the following equationρ xy = R H B + µ 0 R S M(H), (15)where µ 0 is a magnetic permeability of vacuum. In orderto determine the anomalous Hall constant the isothermalmagnetization curves M(H) were measured at thesame temperatures in which magnetotransport effectswere investigated. The magnetization curves for selectedGe 0.850 Sn 0.119 Mn 0.031 Te crystal are pres<strong>en</strong>ted in figure 108.The M(H) dep<strong>en</strong>d<strong>en</strong>cies (see figure 108) shows nonsaturatingbehavior ev<strong>en</strong> at magnetic fields as high as 100 kOe.The magnetization curves observed at temperatures lowerthan spin-glass freezing temperature showed behavior differ<strong>en</strong>tthan that for spin-glass system, namely the largespontaneous magnetization. The experim<strong>en</strong>tal M(H)curves are more complex than that of a Weiss ferromagnetwhat may be interpreted that short range interactionsplay an important role in this system. The maximum valuesof magnetization obtained in each crystal were slightlysmaller than the estimated using chemical composition ofthe alloy. It indicates, that possibly a fraction of Mn ionsremained in a spin state reducing their magnetic mom<strong>en</strong>t orthere exists antiferromagnetic clusters.The equation 1 was fitted to the experim<strong>en</strong>tal data in orderto extract values of ordinary R H and anomalous R SHall coeffici<strong>en</strong>ts. The obtained values of R S varies betwe<strong>en</strong>crystals with a differ<strong>en</strong>t amount of both alloyingelem<strong>en</strong>ts by about an order of magnitude in the range of2.7×10 −5 cm 3 /C and 30×10 −5 cm 3 /C. The chemical compositionof the alloy has significant effect on the R S i.e. itdecreases with the amount of Sn in the alloy and increasewith the Mn cont<strong>en</strong>t. It must be noted, however that theFigure 107: Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of the off-diagonal resistivityρ xy obtained for selected Ge 0.815 Sn 0.091 Mn 0.094 Te crystal.Figure 108: Magnetetization curves obtained at differ<strong>en</strong>t temperatures(see leg<strong>en</strong>d) for selected Ge 0.850 Sn 0.119 Mn 0.031 Te crystal.A. B. AntunesL. Kilanski, W. Dobrowolski (Institute of Physics Polish Academy of Sci<strong>en</strong>ce, Warsaw, Poland), V. E. Slynko, E. I.Slynko (Institute of Materials Sci<strong>en</strong>ce Problems, Ukrainian Academy of Sci<strong>en</strong>ces, Chernovtsy, Ukraine)80


2009 MAGNETIC SYSTEMSHigh field torque magnetometry on a molecular Dysprosium triangleLanthanide based molecular nanomagnets have be<strong>en</strong> attractingconsiderable att<strong>en</strong>tion due to their interesting magneticproperties. Mononuclear complexes of 4f ions haveshown slow relaxation of the magnetization at very hightemperatures compared to those observed in transition metals.Despite their out of phase ac signal observed above 40K, hysteresis curves were observed only at very low temperatures[Ishikawa et al., Angew. Chem. 117, 2991 (2005)].On cooling, deviations from the Arrh<strong>en</strong>ius law predictedfor single molecule magnet behavior become more important,which indicates that tunnelling plays a crucial role inthe relaxation of the magnetization. It is therefore of crucialimportance to obtain information on the low lying sublevelsof the 4f electronic systems, in order to understand the magnetism,and especially the relaxation mechanisms of thesecompounds.We have performed high field torque magnetometry measurem<strong>en</strong>tson the rec<strong>en</strong>tly investigated molecular Dy triangle[Luzon et al., Phys. Rev. Lett. 100 247205(2008)]. This compound shows an unpreced<strong>en</strong>ted magneticbehaviour having a non-magnetic ground doublet whichoriginates from the noncollinearity of the single-ion easyaxes of the Dy 3+ ions that lie in the plane of the triangleat 120 ◦ one from each other. This gives rise to a peculiarchiral nature of the ground nonmagnetic doublet and toslow relaxation of the magnetization which exhibits abruptaccelerations at the crossings of the discrete <strong>en</strong>ergy levels.The ground (|J = 15/2,m J = ±15/2〉) and the first excited(|J = 15/2,m J = ±13/2〉) doublets, were considered to <strong>des</strong>cribethe <strong>en</strong>ergy levels of the single ion assuming that theother excited states are very high in <strong>en</strong>ergy and do not contributeto the magnetic properties at low temperatures. Thesystem therefore mimics the behaviour of an S=3/2 spin.We have used the spin Hamiltonian approach to <strong>des</strong>cribethe low lying <strong>en</strong>ergy levels. The expression of the Hamiltonianused is,anisotropy in the system. The performed high field torquemeasurem<strong>en</strong>ts at 50 mK <strong>en</strong>abled us to quantify the crystalfield splitting betwe<strong>en</strong> the 15/2 and the 13/2 doubletsin Dy 3+ . Figure 109 (a) shows the measured torque signalat 50 mK up to 32 Tesla for the magnetic field applied atdiffer<strong>en</strong>t angles to the plane of the triangle. A peak in thetorque is evid<strong>en</strong>t at around 28 Tesla. Figure 109 (b) showsthe calculated torque signals for δ = 250 cm −1 , j = 0.064cm −1 , and g = 1.35 at 50 mK, which reproduce fairly wellthe experim<strong>en</strong>tally observed curves. The observed peak inthe torque signal at around 28 Tesla for transverse magneticfields points towards the high anisotropy in the system. Thecrystal field splitting of δ = 250 ± 10 cm −1 is close to thatexpected from previously performed ab initio calculations[Chibotaru et al., Angew. Chem. Int. Ed. 47, 4126 (2008)].In a more g<strong>en</strong>eral picture, this study has contributed to abetter understanding of lanthanide based systems. In particular,we have prov<strong>en</strong> that high field torque magnetometrycan be a good substitute to spectroscopy in systems whichare spectroscopically inactive.Ĥ = − j(Ŝ 1 · Ŝ 2 + Ŝ 2 · Ŝ 3 + Ŝ 3 · Ŝ 1 )− gµ B ∑ B · Ŝ i + δ oi=1,314 ∑ (( 15i=1,32 )2 − Ŝ 2 z i)(16)The first term is the isotropic exchange betwe<strong>en</strong> the Dy 3+ions, the second is the Zeeman term, and the last term<strong>des</strong>cribes the single-ion anisotropy where δ o is the zerofield splitting betwe<strong>en</strong> |J = 15/2,m J = ±15/2〉 and |J =15/2,m J = ±13/2〉 states of each Dy 3+ ion. We have particularychos<strong>en</strong> torque magnetometry as it is a strong tool toinvestigate the anisotropy in high-spin clusters, especiallyin systems which are not accessible by spectroscopy. Apeak in the torque signal occurs at a characteristic fieldwhich dep<strong>en</strong>ds on the temperature as well as the magneticFigure 109: (a) Torque signals for the magnetic field applied atdiffer<strong>en</strong>t angles close to 90 ◦ from the plane of the triangle at 50mK. (b) Similar calculated torque curves with the best fit parameters(δ = 250 cm −1 , j = 0.064 cm −1 , and g = 1.35). The temperatureand anisotropy dep<strong>en</strong>d<strong>en</strong>t peak in the torque signal is evid<strong>en</strong>tat around 28 Tesla. The inset shows the molecular structure of theDy 3 cluster.A. B. Antunes, I. SheikinF. El Hallak, J. van Slager<strong>en</strong>, M. Dressel (University of Stuttgart, Germany), M. Eti<strong>en</strong>ne, J. Luzon, R. Sessoli (Universityof Flor<strong>en</strong>ce, Italy), C. Anson, A. Powell (University of Karlsruhe, Germany)81


MAGNETIC SYSTEMS 2009NMR evid<strong>en</strong>ce for long zero-quantum coher<strong>en</strong>ce in antiferromagneticmolecular wheels NaFe 6 and LiFe 6Molecular magnetic clusters of nanometer size have received<strong>en</strong>ormous attraction because of their spectacularquantum ph<strong>en</strong>om<strong>en</strong>a. A unique class of these clusters arethe antiferromagnetic (AFM) molecular wheels, in whichmagnetic metal ions are assembled in a ring-like structure.The dominant AFM Heis<strong>en</strong>berg interaction J betwe<strong>en</strong> themagnetic metal ions leads to a nonmagnetic S = 0 groundstate and a first excited S = 1 state in zero magnetic field.In strong magnetic fields the Zeeman splitting induces levelcrossings (LCs), where the ground state of the moleculechanges from S = 0, M = 0 to S = 1, M = −1, and furtherto S = 2, M = −2, etc. Due to the hyperfine couplingbetwe<strong>en</strong> the nuclear spin and the Fe III ions, the nuclear relaxationrate T −11is very s<strong>en</strong>sitive to the spin state and thespin dynamics of the ferric wheel. Most NMR studies havebe<strong>en</strong> carried out by means of 1 H NMR, since protons providea very strong signal, and their T −11is s<strong>en</strong>sitive to thedynamics of the Néel vector ⃗n = ∑ 6 i=1 (−1)i ⃗s i . However, amajor drawback is a huge amount of inequival<strong>en</strong>t protonson each ring complicating the analysis of the spin dynamics,especially around the level crossings. In order to overcomethis problem we performed NMR measurem<strong>en</strong>ts onthe nuclei which are located in a single-site position of highsymmetry, in the c<strong>en</strong>ter of the ferric wheel–here 23 Na or 7 Linuclei. Their hyperfine interaction is proportional to the totalspin of the ferric wheel ⃗S = ∑ 6 i=1 ⃗s i leading to importantdiffer<strong>en</strong>ces as far as T −11is concerned.Here we pres<strong>en</strong>t the first c<strong>en</strong>tral alkali NMR study atlow temperature and at high field, focusing on the magneticfield dep<strong>en</strong>d<strong>en</strong>ce at the level crossings [L. Schnelzeret al., submitted to EPL]. NMR measurem<strong>en</strong>ts on 23 Naand 7 Li nuclei were carried out on single crystals of [Na/Li⊂Fe 6 {N(CH 2 CH 2 O) 3 } 6 ]Cl·5CHCl 3·0.5H 2 O (Na/LiFe 6in short). They were performed in 17 and 20 T superconductingmagnets in Gr<strong>en</strong>oble and Karlsruhe. Single crystalswere mounted in the mixing chamber of a dilution refrigeratorfor very low temperatures and in pumped 4 He for measurem<strong>en</strong>tsat 2 K. Figure 110 shows the measured T −11ratesat 220 mK and 2 K. The low temperature measurem<strong>en</strong>ts ofNaFe 6 at 220 mK reveal a strong increase of T1 −1 towardsthe LC at 12 T. The LC is not characterized by an additional<strong>en</strong>hancem<strong>en</strong>t of T1 −1 as expected for proton NMR,but by a small reduction of T1 −1 (inset to figure 110a). Thisis attributed to the ins<strong>en</strong>sitivity of the c<strong>en</strong>tral alkali nucleito the fluctuations of the Néel vector. At 2 K T1 −1 shows abroad maximum around LC and, surprisingly, a reductionby three orders of magnitude of T −11in-betwe<strong>en</strong> the 1 st andthe 2 nd LC. Similar results have be<strong>en</strong> obtained for LiFe 6 ;plotted on a reduced field scale (B/J) the measurem<strong>en</strong>ts onLiFe 6 and NaFe 6 are almost id<strong>en</strong>tical. Measurem<strong>en</strong>ts of23 Na T1 −1 at the first LC, at temperatures down to 80 mK,reveal the exist<strong>en</strong>ce of a very small gap 0.06 K, in spiteof high symmetry of the molecule. This implies the exist<strong>en</strong>ceof a small perturbation reducing the symmetry of themolecule. The most striking ph<strong>en</strong>om<strong>en</strong>a is a spectaculardecrease by three orders of magnitude of T1 −1 occurring inthe middle betwe<strong>en</strong> the first and the second LC.The relaxation data have be<strong>en</strong> <strong>des</strong>cribed by calculating thecorresponding spectral d<strong>en</strong>sity of spin fluctuations by amethod of mom<strong>en</strong>ts. It turns out that the observed strongextinction of relaxation is not at all visible in the int<strong>en</strong>sity ofthe zero frequ<strong>en</strong>cy resonance (the zero mom<strong>en</strong>t), but is <strong>en</strong>tirelydue to its width, calculated as the second mom<strong>en</strong>t m 2 .For the calculation of m 2 we used the secular (i.e., <strong>en</strong>ergyconserving) part of the dipolar intermolecular interaction.Betwe<strong>en</strong> the first and the second LC there is a broad andvery deep minimum of m 2 . In this field range the groundstate is a S = 1 state whereas the first excited state changesfrom S = 0 to S = 2 through a broad anti-LC. Since theminimum of m 2 results from the balance of the matrix elem<strong>en</strong>tsof these states, it ext<strong>en</strong>ds over the same field range asthe anti-LC. It is remarkable that √ m 2 can become smallerby two orders of magnitude than the nuclear Larmor frequ<strong>en</strong>cy.This quite unusual situation leads to the reductionof T1 −1 by three orders of magnitude. One should also realizethat the correlation time τ c = 1/ √ m 2 corresponds tothat of a zero quantum coher<strong>en</strong>ce. τ c can be as long as ≃0.2 µs, which is very unusual for an electronic spin system.Figure 110: (a) Field dep<strong>en</strong>d<strong>en</strong>ce of 23 Na T1 −1 in NaFe 6 atT = 220 mK (white squares) and 2 K (black squares), and (b) 7 LiT1 −1 in LiFe 6 at T = 2 K (black squares) and 1 H T1 −1 (dots). Theresults of the calculations are giv<strong>en</strong> by solid lines. Inset displays azoom on the field dep<strong>en</strong>d<strong>en</strong>ce close to the LC at 220 mK.M. Horvatić, C. BerthierL. Schnelzer, B. Pilawa, M. Marz, H. von Löhneys<strong>en</strong> (Physikalisches Institut, Universität Karlsruhe,Germany)82


2009 MAGNETIC SYSTEMSNuclear magnetic resonance determination of spin-superlattice structureof magnetization plateaus in SrCu 2 (BO 3 ) 2Quantum spin systems are nowadays in the focus of considerableexperim<strong>en</strong>tal and theoretical efforts, in particularfor the magnetic field induced exotic quantum states. Ofspecial interest are interacting systems of Heis<strong>en</strong>berg, antiferromagnetic,S=1/2 spin dimers in a magnetic field whichcloses the gap betwe<strong>en</strong> the singlet and one of three Zeemansplittriplet levels of each dimer. At low temperature, wh<strong>en</strong>only these two states per dimer are relevant, the systemcan be <strong>des</strong>cribed by the corresponding S=1/2 pseudospins,or the equival<strong>en</strong>t hard-core bosons. Interacting dimers areth<strong>en</strong> equival<strong>en</strong>t to a system of interacting bosons where boson(triplet) d<strong>en</strong>sity can be tuned by the magnetic field. Thissystem g<strong>en</strong>erally undergoes a Bose-Einstein cond<strong>en</strong>sation(BEC) and therefore provi<strong>des</strong> an exceptional access for experim<strong>en</strong>talstudies of this ph<strong>en</strong>om<strong>en</strong>on. In the hard-coreboson repres<strong>en</strong>tation the balance of the kinetic and the interaction(repulsion) <strong>en</strong>ergy is determined by the degree offrustration of interdimer spin coupling, where frustrationstrongly reduces kinetic <strong>en</strong>ergy. In this latter case, insteadof being itinerant and undergo BEC, bosons can be localizeddue to mutual repulsion into a charge ordered state,that is a Wigner crystal. Since this state is gapped, the bosond<strong>en</strong>sity will be magnetic field indep<strong>en</strong>d<strong>en</strong>t and the systemwill pres<strong>en</strong>t a plateau of magnetization.Perfect frustration occurs in the geometry of orthogonaldimers in 2D, giv<strong>en</strong> by the Shastry-Sutherland Hamiltonian,and the SrCu 2 (BO 3 ) 2 compound is its first recognizedrealization. The discovery of the magnetization plateaus at1/8, 1/4 and 1/3 of the saturation magnetization in this compoundwas followed by ext<strong>en</strong>sive experim<strong>en</strong>tal and theoreticalinvestigation. In particular, NMR study performed atLNCMI proved that the 1/8 plateau, as predicted, indeedcorresponds to a comm<strong>en</strong>surate spin superstructure. Subsequ<strong>en</strong>tstudies showed that a superstructure persists at highermagnetic field [Takigawa et al., Phys. Rev. Lett. 101,037202 (2008)], and that there are other, yet undiscoveredplateaus. One of these, adjac<strong>en</strong>t to the 1/8 plateau on thehigh field side, was indeed confirmed by the torque measurem<strong>en</strong>ts[Levy et al., EPL 81, 67004 (2008)]. At the sametime appeared several contradictory predictions for the exist<strong>en</strong>ceof many other magnetization plateaus in this system,calling for experim<strong>en</strong>tal verification. However, theoretical<strong>des</strong>cription of SrCu 2 (BO 3 ) 2 is very difficult, because the interdimerinteraction is too strong to be properly <strong>des</strong>cribedby a perturbation theory, while exact numerical methods arelimited to only very small 2D systems.We have therefore continued our NMR investigation to observeevolution of the spin superstructure through magneticfield dep<strong>en</strong>d<strong>en</strong>ce of 11 B NMR spectra in the 27-34 T range,at 0.43 K. From the observed spectra we clearly id<strong>en</strong>tifyplateau phases where the NMR spectra, and thus the spinsuperstructure, is magnetic field indep<strong>en</strong>d<strong>en</strong>t. In additionto the long known 1/8 and 1/4 plateau and the rec<strong>en</strong>tly discoveredplateau adjac<strong>en</strong>t to the 1/8 plateau, a new plateauwas discovered half way up towards the 1/4 plateau (seefigure 111). Betwe<strong>en</strong> these plateaus NMR spectra evolvecontinuously with magnetic field, and no other plateau wasdetected. The same sequ<strong>en</strong>ce of plateaus was confirmedby the new, “differ<strong>en</strong>tial” torque measurem<strong>en</strong>ts, performedat ∼0.1 K. This method determines the magnetization withconsiderably <strong>en</strong>hanced precision, allowing us to find thatthe magnetization of the first three plateaus scales as 1/8: 2/15 : 1/6, which confirms some of the theoreticallyproposed values and exclu<strong>des</strong> others. Detailed analysis ofthe 11 B NMR spectra allows us to make complete determinationof the spin-polarization superstructures. We findthat previously id<strong>en</strong>tified “ext<strong>en</strong>ded triplets” are always arrangedin stripe structures, specific to each plateau, oft<strong>en</strong>differ<strong>en</strong>t from what is proposed theoretically [Takigawa etal., unpublished].Figure 111: The distribution of the internal field at the 11 B sites,obtained by deconvoluting the NMR spectra from the quadrupolesplitting. Pres<strong>en</strong>ted spectra are repres<strong>en</strong>tative of 4 magnetizationplateaus, attributed to fractions 1/8, 2/15, 1/6 and 1/4 of saturationmagnetization.M. Horvatić, C. Berthier, S. Krämer, I. SheikinM. Takigawa, T. Waki, Y. Ueda (ISSP, University of Tokyo, Japan), H. Kageyama (Kyoto University, Japan), F. Mila(EPFL, Lausanne, Switzerland)83


MAGNETIC SYSTEMS 2009Magnetic structure of the half magnetization plateau phase in CdCr 2 O 4CdCr 2 O 4 belongs to the well-known family of cubic Crbasedspinels ACr 2 O 4 (A=Hg, Cd, and Zn) which have attractedmuch att<strong>en</strong>tion because of the highly frustrated pyrochlorelattice formed by their magnetic Cr 3+ (S = 3/2)ions. Furthermore, due to the direct overlap of t 2g orbitalsof neighboring Cr 3+ ions (3d 3 ), the spin Hamiltonianhas dominant isotropic antiferromagnetic nearest neighborinteractions. The resulting strong frustration suppressesthe system from ordering down to a much lower temperaturethan the Curie-Weiss temperature Θ CW . In case ofCdCr 2 O 4 , the system remains paramagnetic up to T N =7.8 K, far below |Θ CW | = 88 K. The ordered state is accompaniedby a cubic to tetragonal structural transition, and isnot a simple collinear antiferromagnet, but an incomm<strong>en</strong>surate(IC) helical magnetic order with a single characteristicwave vector of Q m = (0,δ,1) or (δ,0,1) where δ ∼ 0.09[Ueda et al. Phys. Rev. Lett. 94, 047202 (2005); Chunget al., Phys. Rev. Lett. 95, 247204 (2005)]. Upon applicationof an external magnetic field, CdCr 2 O 4 undergoes aphase transition into a half-magnetization plateau phase atH c1 = 28 T suggesting that each tetrahedron has three upand one down spins (3:1 constraint). Under this restriction,two spin arrangem<strong>en</strong>ts, one with the rhombohedralR3m symmetry and one with the cubic P4 3 32, are possible,dep<strong>en</strong>ding on the sign of the next nearest neighbor interaction.Thanks to the rec<strong>en</strong>t combination of a 30 T portable miniaturepulsed magnet and the world highest flux neutronsource of the Institut Laue-Langevin (ILL) [Yoshii et al.,Phys. Rev. Lett. 103, 077203 (2009)], we have succeededin following the field dep<strong>en</strong>d<strong>en</strong>ce of selected magneticBragg reflections, which allowed to distinguish betwe<strong>en</strong>these two possible magnetic structures. The experim<strong>en</strong>twas carried out on the thermal neutron tripleaxisspectrometer IN22. The single crystal (a thin plate(∼ 4 × 4 × 0.2 mm 3 ) of ∼ 40 mg) was mounted with the[111] and [110] axes in the horizontal scattering plane. Thepulsed measurem<strong>en</strong>ts were performed more than 100 timesat each reflection to obtain reasonable statistics.Figure 112(a) shows the time dep<strong>en</strong>d<strong>en</strong>ce of the elastic neutronscattering int<strong>en</strong>sity measured at the IC magnetic peakof (1.0675, -1.0125, 0.0275) at 2.5 K. The peak int<strong>en</strong>sitygradually decreases to background level and th<strong>en</strong> remainszero betwe<strong>en</strong> 3 and 4.6 ms (H > 28 T) after which the int<strong>en</strong>sityincreases back to the intermediate level but not tothe original int<strong>en</strong>sity because of magnetic domain ori<strong>en</strong>tation.In order to find out where the magnetic int<strong>en</strong>sity ofthe IC peak was transferred to, we performed similar measurem<strong>en</strong>tsat a comm<strong>en</strong>surate Q = (1,-1,0) position. Asillustrated in figure 112(b), wh<strong>en</strong> a magnetic field was applied,no signal was initially observed at (1,-1,0) for 3 msat which point the int<strong>en</strong>sity sudd<strong>en</strong>ly increased due to thefirst-order nature of the field-induced phase transition. Thecomm<strong>en</strong>surate magnetic int<strong>en</strong>sity remained non-zero overexactly the same range of time (and field) over which theIC magnetic signal w<strong>en</strong>t down to zero. Our results indicatethat as CdCr 2 O 4 <strong>en</strong>ters the half magnetization plateaustate, the magnetic structure changes from the IC spiral to acomm<strong>en</strong>surate collinear spin structure with Q m = (1,0,0).Figure 112: Time dep<strong>en</strong>d<strong>en</strong>ce of the magnetic field (solid redlines) and neutron counts (filled circle) measured at (1.0675,-1.0125, 0.0275) and (1,-1,0) reflections at T = 2.5 K.Figure 113: Magnetic field dep<strong>en</strong>d<strong>en</strong>ce of the peak int<strong>en</strong>sity ofthe (2,-2,0) reflections measured at T = 2.5 K with the asc<strong>en</strong>ding(filled circles) and <strong>des</strong>c<strong>en</strong>ding (op<strong>en</strong> circles) field.To distinguish betwe<strong>en</strong> the two possible models, we alsoperformed similar pulsed field measurem<strong>en</strong>ts at (2,-2,0) atwhich point the R3m structure should produce magneticBragg scattering while the P4 3 32 structure would not. AtH = 0 T, nuclear Bragg int<strong>en</strong>sity is observed at (2,-2,0). Asshown on figure 113, the (2,-2,0) int<strong>en</strong>sity does not changeas the system <strong>en</strong>ters the half-magnetization phase. Thus, weconclude that the half-magnetization spin state of CdCr 2 O 4has the P4 3 32 spin structure.F. Duc, P. Frings, B. Vignolle, G.L.J.A. Rikk<strong>en</strong>H. Nojiri, K. Ohoyama, S. Yoshii (Institute for Materials Research, Tohoku University, Japan), M. Matsuda (JAEA,Tokai, Japan), L-P. Regnault (CEA, DRFMC-SPSMS-MDN, Gr<strong>en</strong>oble)84


2009 MAGNETIC SYSTEMSStructural analysis with pulse-l<strong>en</strong>gth exposures up to 30 Tesla at ID06, ESRFAs topical tests of the newly commissioned experim<strong>en</strong>talsetup at ID06, ESRF, synthetic powder samples of high T cNdFeAsO and of a natural atacamite, Cu 2 Cl(OH) 3 , havebe<strong>en</strong> measured in pulsed fields of up to 30 Tesla, usingpulse-simultaneous exposure times of less than 10 ms attemperatures down to 150 K (NdFeAsO) and 6 K (atacamite).temperatures and fields (Rp ∼ 0.06-0.07). The lower panelshows there is a measurable, and isotropic, effect on the inplanecell parameters with applied field. Preliminary analysisof cell parameter have giv<strong>en</strong> us direct information on thelattice strain in the sample. This tak<strong>en</strong> with variable temperatureand field data should allow us to establish how the anycoupling parameters at the transition are field-affected. Theinternal parameters would give information on characteristicstructural features; such as bond l<strong>en</strong>gths and perhapsmore critically, bond angle behaviour under variable fieldand temperature.Figure 114: Lattice distortion in NdFeAsO. The top panel shows,in blue, the variation in b/a, or the level of in-plane orthorhombicdistortion and in red the level of pseudo-tetragonal [2c/(a + b)]distortion at all temperatures and fields of 3 - 30 T . The lowerpanel indicates the effect on in-plane cell parameters at a fixedtemperature of 90 K, while augm<strong>en</strong>ting pulse str<strong>en</strong>gth to 30 T.The gre<strong>en</strong> line shown indicates an increasing tr<strong>en</strong>d of 0.04 ÅT −1 .The two samples offer differ<strong>en</strong>t chall<strong>en</strong>ges; not only froma point of view of disturbing their inher<strong>en</strong>t magnetic propertiesat reduced temperature, but also from our ability toextract reliable structural information from powder sampleswith contrasting symmetries and structural complexities.For NdFeAsO, it is evid<strong>en</strong>t from figure 114 that lattice distortionmarkers show most variance in the range of measuredtemperatures betwe<strong>en</strong> 120−205 K. Above and belowthese points there is little scatter, <strong>des</strong>pite the same numberof data at each temperature and equival<strong>en</strong>t quality fits at allFigure 115: Rietveld refined, to R Bragg = 0.06, structure of atacamiteat T = 7 K, B = 30 T from 7 ms data collection on mar345image plate.The second study was <strong>des</strong>igned to test the limits ofwhat structural analysis would be possible; using an altogethermore complicated orthorhombic structure, at basetemperatureof the cryostat and with our pulse-l<strong>en</strong>gth limitedexposure times. Again here, the aim would be to determineinternal structural parameters to estimate if it wouldbe possible to extract any affect of high-field applicationon the frustration of the Kagomé-like lattice. We havebe<strong>en</strong> successful in refining atacamite to R Bragg of 0.06 atsub 10 K, with field str<strong>en</strong>gths of up to 30 Tesla and pulselockedexposure times. Figure 115 shows the refined structure.Detailed analysis of the full dataset will determineif any field-induced frustration can give rise to a tractableresponse at these extreme conditions, though with experi<strong>en</strong>cegained in setup, control and running this demandingmeasurem<strong>en</strong>t; we are confid<strong>en</strong>t that these methods offerconsiderable scope for future in situ diffraction research.F. DucT. Roth, C. Detlefs, W. A. Crichton (ESRF, Gr<strong>en</strong>oble, France), S. Margadonna (University of Edinburgh, U.K.)85


MAGNETIC SYSTEMS 2009Magnetization at low temperatures and high magnetic fields on LuFe 2 O 4LuFe 2 O 4 is thought to be a multiferroic [Ikeda et al. Nature436, 1136-1138 (2005)], with a novel ferroelectric mechanism,based on charge order. The electrically active Fe withaverage val<strong>en</strong>ce of 2.5+ is contained in trigonal Fe-O doublelayers, a highly frustrated arrangem<strong>en</strong>t. Below ∼ 320 Kthe Fe val<strong>en</strong>ces order, resulting in the double layers becomingpolar, appar<strong>en</strong>tly with an antiferroelectric stacking ofthe polarization of the individual double layers [M.Angst etal. Phys. Rev. Lett. 101, 227601 (2008)].The frustration also effects the spin ordering occurring below240 K [Christianson et al. Phys. Rev. Lett. 100,107601 (2008)]. Several indications for magnetoelectricityhave be<strong>en</strong> observed, though the microscopic details ofthis coupling remain to be elucidate. Apart from magnetoelectriccoupling, the magnetism in LuFe 2 O 4 has also attractedatt<strong>en</strong>tion due to a giant magnetic coercivity, rec<strong>en</strong>tlyattributed a freezing of nano-scale pancake-like (Ising) ferromagneticdomains. In low fields we have observed magnetictransitions of sharpness and clear 3D spin order. Bymagnetization, spectroscopic, neutron and synchrotron experim<strong>en</strong>tswe id<strong>en</strong>tified a further transition at 170 K, involvinga disruption of magnetic order and a structural distortionwhich can be tuned by a magnetic field.In our experim<strong>en</strong>t at the LNCMI with a 10MW-magnet weperformed hysteresis loops with H||c and a magnetic fieldup to 22 T, within a temperature range betwe<strong>en</strong> 60 K andhelium base temperature of 3 K. All the magnetization datawas measured with the extraction method. These measurem<strong>en</strong>tswere done after cooling down the sample in a zerofield (ZFC). From this ZFC we were able to obtain a virgincurve of the magnetization. The hysteresis loop at basetemperature (inset figure 116) shows a plateau in its virgincurve at a magnetic field of 15T, what is in good agreem<strong>en</strong>twith the data from optical reflectance contrast [Xu etal. Phys. Rev. Lett. 101, 227602 (2008)]. At this valuethe transition is not complete and it remains up to a valueof about 20T until the crystal structure is switched (fromhexagonal to monoclinic) and the magnetization is saturated.We observe only one step in the virgin magnetizationcompared to [Iida et al. Physica B 155 307, (1989)] whereseveral occur. This is may be due to a better crystal qualitywith less differ<strong>en</strong>t grains. From the in loop magneticbehaviour we were able to complete the magnetic phase diagramfor LuFe 2 O 4 for low temperatures, as shown in figure117, where it is shown that there is a coexist<strong>en</strong>ce betwe<strong>en</strong>a ferromagnetic (FM) phase and a antiferromagnetic(AFM) phase at low temperatures.We also measured the magnetization in as high fields as feasibleperp<strong>en</strong>dicular to the c-axis. In this part of the experim<strong>en</strong>tthere was no indication of a lacking of the magnetocrystallineanisotropy. This means that the magnetic mom<strong>en</strong>tsare all aligned in c-direction.Figure 116: Magnetic field dep<strong>en</strong>d<strong>en</strong>ce from the magnetizationwith H||c in LuFe 2 O 4 at differ<strong>en</strong>t temperatures. All measurem<strong>en</strong>tswhere tak<strong>en</strong> in zero field cooling (ZFC).Figure 117: Low temperature H-T phase diagram for H||c inLuFe 2 O 4 determined from data shown in figure 116 (arrows indicatethe direction of the transition as a function of the appliedfield).A. B. AntunesJ. de Groot, M. Angst (Forschungsz<strong>en</strong>trum Jülich GmbH, 52428 Jülich, Germany)86


2009 MAGNETIC SYSTEMSEnhancem<strong>en</strong>t magnetic mom<strong>en</strong>t in the single phase nanostructure Gd 3 Fe 5 O 12Rare earth iron garnets (REIG) are promising candidatesfor use in high performance microwave and electrochemicaldevices owing to its high resistivity, high Curie temperature,and high chemical stability and possess uniquemagnetic, optical, thermophysical and mechanical properties.Gd 3 Fe 5 O 12 (R 3+3 c[Fe 3+2 ] a (Fe 3+3 ) dO 2−12h) particles weresynthesized in polycrystalline form by the solid-state reactiontechnique from a mixture of α−Fe 2 O 3 and Gd 2 O 3 innominal compositions of 5 : 3. The X-ray diffractogramsshow that all the milled Gd 3 Fe 5 O 12 garnet particles retaintheir single phase structure (Ia3d space group). The averagegrain size decreases with milling and reaches 29 nm forthe 40 hours milled sample. The 57 Fe Mössbauer spectrawere recorded at 300 K and 77 K for the differ<strong>en</strong>t samples.There is no evid<strong>en</strong>ce for the pres<strong>en</strong>ce of Fe 2+ chargestate. On increasing the milling time, one observes the progressiveoccurr<strong>en</strong>ce of a c<strong>en</strong>tral quadrupolar feature at both300 K and 77 K, in addition to three magnetic sextets withdecreasing int<strong>en</strong>sity but increasing line width compared tothat of the bulk. The quadrupolar feature has to be decomposedat both temperatures into two broad line quadrupolardoublets: the pres<strong>en</strong>ce of ferric and ferrous species isth<strong>en</strong> id<strong>en</strong>tified. The Fe 2+ cont<strong>en</strong>t linearly increases withthe milling time (figure 118).The measured magnetization (M) for the as-prepared GdIGis found equal to 15.9 µBmol −1 at 4.2 K. Wh<strong>en</strong> the grainsize is reduced below 100 nm, the M is strongly appliedfield dep<strong>en</strong>d<strong>en</strong>t and no saturation is observed ev<strong>en</strong> underthe highest applied field of 320 kOe (figure 119). In the170 − 320 field range the magnetization curves of the differ<strong>en</strong>tmilled samples are very well (within 1%) <strong>des</strong>cribedby the approach law M = M sat (1 − b/H 2 ). According toNéel the b coeffici<strong>en</strong>t is determined by the magnetocrystallineanisotropy and giv<strong>en</strong> by b = 8K 2 /105(M sat ) 2 .18.For the 35h milled sample M sat is only equal to 14 µBmol −1and remains much smaller than the bulk value. The socalculatedvariation of K is reported in figure 120 versusthe Fe2+ cont<strong>en</strong>t where a large increase of K is observedwh<strong>en</strong> the milling time increases. The modified formulaeof our GdIG particle is giv<strong>en</strong> by Gd 3+3(Fe 3 3(1−r) + Fe2+ 3r )[Fe 3 2(1−s) + Fe2+ 2s ] O2− 12−2.5ptaking into account the pres<strong>en</strong>ceof oxyg<strong>en</strong> vacancies related to the Fe 2+ cont<strong>en</strong>t (p). Assumingthat only the Fe 3+ contribute to the ferrite magnetizationr and s values were calculated using the p and M satvalues deduced from the Mössbauer spectra and high fieldbehavior analysis respectively. The particular behavior ofthe 35h milled samples is th<strong>en</strong> explained by the fact thanthe octahedral site contains the largest part of Fe 2+ ion. W<strong>en</strong>ote that (i) the T comp values of the nanogarnets are few degreeshigher than that of the bulk; (ii) However, the Curietemperature (T C ) of the various sized nanocrystalline GdIGsamples are found to be significantly higher than that of thebulk.Figure 118:Figure 119:Figure 120:Fe 2+ cont<strong>en</strong>t versus the milling time.Isothermal magnetization curves at 4.2K.Anisotropy constant versus the Fe 2+ cont<strong>en</strong>t.M. GuillotC. N. Chinnasamy, B. Latha, T. Sakai, S. D. Yoon, C. Vittoria, V. G. Harris, (C<strong>en</strong>ter for Microwave Magnetic Materialsand Integrated Circuits, Northeastern University, Boston). J. M. Gr<strong>en</strong>eche (LPEC, Universit du Maine, Le Mans).87


MAGNETIC SYSTEMS 2009Effect of the M/Co substitution on magnetocrystalline anisotropy andmagnetization in SmCo 5−x M x compounds (M=Ga; Al)The RCo 5 compounds have be<strong>en</strong> discovered a few deca<strong>des</strong>ago but are still attracting much interest in order to understandtheir exceptional intrinsic magnetic properties. Theinflu<strong>en</strong>ce of substitution of p elem<strong>en</strong>ts (Al, B, Ga...) forCo on the magnetic properties of the RCo 5 type phases isalso an active field of research nowadays. The samples formagnetization measurem<strong>en</strong>ts were processed from powderswith a particle size smaller than 25 µm. The powder wasori<strong>en</strong>ted at room temperature using an ori<strong>en</strong>tation field oftypically 10 kOe and fixed in slow setting epoxy resin. Themagnetic field was applied either parallel or perp<strong>en</strong>dicularto the alignm<strong>en</strong>t direction. According to the X-ray analysis,the CaCu 5 type structure of the RCo 5 is preserved upon substitutionof Ga and Al for Co in the SmCo 4 Al and SmCo 4 Gacompounds. According to the neutron diffraction resultson these isotype compounds, the Al and Ga atoms havea pronounced prefer<strong>en</strong>ce for the Co 3g atomic position inthe hexagonal CaCu 5 structure. For both SmCo 4 Al andSmCo 4 Ga, at room temperature, the easy magnetization directioncoinci<strong>des</strong> with the c-axis of the hexagonal lattice.Ga and Al for Co substitution induce a large reduction ofthe Curie temperature from typically 900 K to 1000 K forthe RCo 5 to around 500 K only for the RCo 4 Al or RCo 4 Gaphases. The RCo 4 M phases containing M=Ga and Al havesimilar Curie temperature.As can be se<strong>en</strong> from the isothermal curves in figures 121and 122, the use of high magnetic field is required dueto the large magnetocrystalline anisotropy of the samples.The spontaneous magnetization has be<strong>en</strong> determined froma linear extrapolation of the M(H) curve to zero appliedfields. The saturation magnetization has be<strong>en</strong> obtainedfrom extrapolation of the M(H) curve with H parallel tothe alignm<strong>en</strong>t direction and larger than 20 T according toM(H) = M sat + a/H2. The replacem<strong>en</strong>t of one Co atomby one Ga or Al atom induces a strong decrease of the saturationmagnetization from 8.46 µB/formula unit at 4 K toonly about 4 µB/f.u. Such dramatic decrease of the Co magnetizationis consist<strong>en</strong>t with earlier reported results on isotypecompounds. SmCo 5 is well known for it exceptionallylarge magnetocrystalline anisotropy µ 0 H a ∼ 52 T at 4 K.The anisotropy field can be estimated by the field at whichthe two magnetization curves will merge for the two differ<strong>en</strong>tori<strong>en</strong>tations. The anisotropy is found to be largerfor the Ga than for Al containing compounds; 89 T and83 T respectively. An effective magnetocrystalline coeffici<strong>en</strong>thas be<strong>en</strong> derived from the anisotropy field accordingto the relation H a = 2K e f f /M s . The values found for theSmCo 4 Al and SmCo 4 Ga are 16.3 and 19.3 MJ/m 3 respectively,that is to say of the same order of magnitude thanfor the SmCo 5 . Consequ<strong>en</strong>tly, the huge anisotropy field observedfor the SmCo 4 Al and SmCo 4 Ga result from largeanisotropy constant and a strong decrease of the saturationmagnetization respectively. The pres<strong>en</strong>ce of Al or Ga hasbe<strong>en</strong> reported to significantly reduce the Co sublattice contributionto the magnetocrystaline anisotropy in the YCo 4 Alor YCo 4 Ga isotype compounds. Thus we conclude thatthe huge anisotropy field reported here for SmCo 4 Al andSmCo 4 Ga results from a reinforcem<strong>en</strong>t of the Sm contributionto the magnetocrystalline anisotropy in comparison tothe SmCo 5 phase. Further studies are in progress to investigatethe thermal dep<strong>en</strong>d<strong>en</strong>ce of the magnetic features oftheses phases.Figure 121: Isothermal (4.2K) high field magnetization curve ofSmCo 4 Al recorded parallel to the easy magnetization direction inorder to obtain the spontaneous magnetization M spon . Inset; determinationof the saturation magnetization M sat .Figure 122: Isothermal hysteresis cycle recorded at 4 K on ori<strong>en</strong>tedSmCo 4 Al wh<strong>en</strong> applying the magnetic field perp<strong>en</strong>dicularto the alignm<strong>en</strong>t direction (c axis).M. GuillotA. Laslo, C.V. Colin, O. Isnard (Institut Néel, CNRS and Université Joseph Fourier)88


2009 MAGNETIC SYSTEMSInvestigation of the intrinsic magnetic properties of the ThCo 4 B compoundWe have meaured the intrinsic magnetic properties ofThCo 4 B to investigate the influ<strong>en</strong>ce of a tetraval<strong>en</strong>t elem<strong>en</strong>tsuch as Th on the magnetic properties of the Co sublatticein comparison to the already well investigated trival<strong>en</strong>trare-earth containing isotype compounds. The compoundis single phase (CeCo4B structure) with two differ<strong>en</strong>t crystallographicsites for thorium (1a and 1b), two other sitesfor cobalt (2c and 6i) and one site for the boron atom (2d)(figure 123). Magnetic measurem<strong>en</strong>ts were carried out inthe temperature range 4.2 − 300 K in a continuous magneticfield up to 230 kOe. No single crystals of ThCo4Bwas available, thus the samples were sieved down to a particlesize smaller than 25 µm. The powder was mixed withepoxy resin and subsequ<strong>en</strong>tly aligned at room temperatureusing an ori<strong>en</strong>tation field of typically 10 kOe. The saturationmagnetization has be<strong>en</strong> obtained from extrapolation ofthe M(H) curve with H parallel to the alignm<strong>en</strong>t directionaccording to the following equation M(H) = M sat + a/H 2 .As se<strong>en</strong> in figure 124 ThCo 4 B orders ferromagneticallyat 301 K temperature much smaller than that of isotypeRCo 4 B (R is a rare-earth elem<strong>en</strong>t or yttrium).Assuming that T c results only from Co-Co exchange interactionsthe Co 4 B compound exhibit rather large exchangeinteraction betwe<strong>en</strong> Co neighbors corresponding to an exchangefield of 175 T. Both neutron diffraction experim<strong>en</strong>tsand electronic band structure calculations indicate the exist<strong>en</strong>ceof a large Co magnetic mom<strong>en</strong>t at the Co 2c position.For this site the magnetic mom<strong>en</strong>t 1.8 µB/formula unit isfound to be typically the same as those observed in Cometal or in well known RCo 5 type compounds, thus indicatingthat unlike the Co 6i site, the Co 2c site is almost ins<strong>en</strong>sitiveto the pres<strong>en</strong>ce of Th. This confirms the significantdiffer<strong>en</strong>ce in the magnetic behavior of the two inequival<strong>en</strong>tCo magnetic sites in ThCo 4 B. The Co 2c site has a largemagnetic mom<strong>en</strong>t and localized character whereas the Co 6isite displays a nearly ferromagnetic state with a large degreeof delocalization. As can be se<strong>en</strong> from figure 125 hugemagnetocrystalline anisotropy is observed for the ThCo 4 Bcompound. The estimation of the 4 K anisotropy field givesa value of about 47 T. This large value can be consideredas surprising if one keeps in mind that the YCo 4 B isotypecompound exhibit a spin reori<strong>en</strong>tation transition resultingfrom the competition of the Co 2c and Co 6i inequival<strong>en</strong>tatomic positions. The RCo 4 B type compounds arestructurally deriving from the RCo 5 type structure whereboth Co sites are competing in terms of magnetocrystallineanisotropy, the Co 2c and Co 6i preferring an alignm<strong>en</strong>t alongthe c-axis and within the basal plane respectively. However,as in ThCo 4 B the Co 6i magnetic mom<strong>en</strong>t is close tozero, its contribution to the magnetocrystalline anisotropyis expected to decrease significantly also. The ThCo 4 B unusuallylarge magnetocrystalline is related to the large Co 2ccontribution.Figure 123: Crystal structure of ThCo 4 B (Th atoms are occupyingthe sites labelled R).Figure 124: Thermal evolution of isofield magnetization curvesrecorded at the indicated temperatures.Figure 125: Magnetization isotherms of ThCo 4 B recorded atT = 4.2 with the field applied parallel and perp<strong>en</strong>dicular to theeasy magnetization direction.M. GuillotO. Isnard, V. Pop, H. Mayot, J.C. Toussaint (Institut Néel, CNRS and Université Joseph Fourier)89


MAGNETIC SYSTEMS 2009Magnetic properties of Y 0.7 Er 0.3 Fe 2 (H, D) 4.2 compounds up to 35 TRFe 2 Laves phases can absorb hydrog<strong>en</strong> or deuterium upto 5H(D)/mol and this absorption modifies significantly thestructural, magnetic and electronic properties. The YFe 2 D xdeuteri<strong>des</strong> are ferromagnetic with an increase of the meanFe mom<strong>en</strong>t and a decrease of T C for x ≤ 3.5 D/mol. Forx = 4.2, the monoclinic compound is ferromagnetic at lowtemperature, th<strong>en</strong> undergoes a sharp first order magnetovolumictransition towards an antiferromagnetic structure at84 K. Surprisingly this transition is very s<strong>en</strong>sitive to the Hfor D substitution, which increases the mean Fe mom<strong>en</strong>t at4.2 K and shifts the transition temperature extrapolated atzero field T M0 to 131 K (by 50%). Since the cell volumeof the hydride is 0.78% larger than the deuteride, this giantisotope effect has be<strong>en</strong> related to the strong dep<strong>en</strong>d<strong>en</strong>ce ofthe itinerant electron metamagnetic behavior (IEM) behavioron the volume of one of the Fe sites among eight whichhas a differ<strong>en</strong>t number of H(D) neighbors.Thermomagnetization curves deduced from cooling underlow magnetic field (300 Oe) for Y 0.7 Er 0.3 Fe 2 H 4.2 andY 0.7 Er 0.3 Fe 2 D 4.2 respectively show sharp transitions atT MO = (107±2) K and (61±1) K respectively. These transitiontemperatures were found equal to 131 and 84 K inthe YFe 2 hydride and deuteride. The higher T MO valuefor the ferromagnetic YFe 2 H 4.2 hydride is attributed toa larger cell volume. However, in Y 0.7 Er 0.3 Fe 2 H 4.2 andY 0.7 Er 0.3 Fe 2 D 4.2 the exchange couplings betwe<strong>en</strong> the differ<strong>en</strong>tmagnetic atoms may also influ<strong>en</strong>ce the transitiontemperatures. This is confirmed by the thermomagnetizationcurves (figures 126 and 127) where a large increaseof T MO is observed together with a metamagnetic behavior.The transition field (HTR) is determined from themaximum of (dM T /dH). For Y 0.7 Er 0.3 Fe 2 H 4.2 the transitionis observed in the 4.2 − 40 K and 125 − 175 K temperaturesranges On the contrary the transition exists inthe 4.2 − 55 K and 80 − 175 K temperature ranges forY 0.7 Er 0.3 Fe 2 D 4.2 . In the 4.2 − 40 K range the (HTR) valuesare id<strong>en</strong>tical. However, wh<strong>en</strong> the temperature increasesa large isotopic effect is revealed by the temperature variationof HTR (figure 128).The transition field increases linearlyversus temperature but with a smaller HTR/T slopefor the deuteride (2.48 kOe/K) compared to the hydride(2.58 kOe/K). These values are nevertheless larger than forYFe 2 H 4.2 (1.34 kOe/K) and YFe 2 D 4.2 (1.37 kOe/K), showingan additional influ<strong>en</strong>ce of the Er substitution. This suggeststhat the Y for Er substitution modifies the structuraland magnetic properties of the hydri<strong>des</strong> and deuteri<strong>des</strong>: (i)The cell volume of the hydride is 0.8% larger than the correspondingdeuteride; (ii) A spin reori<strong>en</strong>tation of Er mom<strong>en</strong>tis induced at low temperature, indep<strong>en</strong>d<strong>en</strong>tly to the H/Disotope effect; (iii) The values of T M0 are smaller than inthe YFe 2 H 4.2 and YFe2D 4.2 compounds, but remain s<strong>en</strong>sitiveto the isotope influ<strong>en</strong>ce. The s<strong>en</strong>sitivity of T M0 to thechange of volume confirms the magnetovolumic characterof the transition. (iv) The B/T slopes are differ<strong>en</strong>t for thehydride and deuteri<strong>des</strong>, whereas there were similar in th<strong>en</strong>on substituted compounds.Figure 126: Thermomagnetization of Y 0.7 Er 0.3 Fe 2 (H, D) 4.2 .Figure 127:D) 4.2 .Figure 128:Isothermal magnetization of Y 0.7 Er 0.3 Fe 2 (H,Transition field versus temperature.M. GuillotV. Paul-Boncour, T. Leblond (CMTR, ICMPE, CNRS and Univ. Paris XII, Thiais)90


2009 MAGNETIC SYSTEMSField-induced transitions in RECo 0.50 Mn 0.50 O 3 (RE = Dy, Eu)One interesting family of perovskites is RE(TM,Mn)O 3 inwhich the Mn atom has be<strong>en</strong> partially substituted by atransition-metal elem<strong>en</strong>t TM like Co giving rise to Mn 4+ -Co 2+ ferromagnetic interactions. In addition, if the RE elem<strong>en</strong>tbears a large magnetic mom<strong>en</strong>t, th<strong>en</strong> the RE sublatticemay interact with the ordered TM-Mn sublattice [Peñaet al., J. Magn. Magn. Mater. 312, 78 (2007); Antuneset al., J. Europ. Ceram. Soc. 27, 3927 (2007)]. Inthis work we pres<strong>en</strong>t the magnetic properties of bulk ceramicsamples EuCo 0.50 Mn 0.50 O 3 and DyCo 0.50 Mn 0.50 O 3 .Nickel-containing samples of similar composition (Ni/Mn= 0.50/0.50) are measured for comparison. Samples wereprepared by solid state synthesis from the correspondingsubmicronic powder oxi<strong>des</strong>. They were characterized byX-ray diffraction showing pure perovskite orthorhombicstructure (Pbnm). Magnetic measurem<strong>en</strong>ts were performedon specim<strong>en</strong>s cut from ceramic bulks.ZFC curve follows a similar behaviour as the Eu case, thatis canted antiferromagnetism since the magnetic propertiesof the Co-Mn sublattice predominate. Wh<strong>en</strong> the sampleis field cooled the Co-Mn sublattice orders at T C = 85 K,a lower temperature as the Eu-case because of the smallerionic radius of the Dy ion compared to Eu.The magnetization loop is shown in figure 130(a) forEuCo 0.50 Mn 0.50 O 3 sample. We notice five steep transitionson the hysteresis curves. The magnetization valuemeasured at 20 T is lower than the theoretical value(M S = 3.87 µ B ) if we consider all the spins of Mn 4+and Co 2+ aligned and no contribution from Eu 3+ . ForEuNi 0.50 Mn 0.50 O 3 there are no step-like transitions. Themeasured value of the magnetization at 20 T is also lowerthan the calculated value of 3.35 µ B if all spins of transitionmetals are aligned on the field direction. This suggeststhat Eu 3+ in these systems is a classical case of VanVleck magnetism. For DyCo 0.50 Mn 0.50 O 3 (figure 130(b))we can see two field transitions (near 2 T and 5 T) andthe magnetization measured at 20 T reaches the theoreticalvalue (M S = 6.76 µ B ) if we consider a ferrimagneticmodel of two sublattices (rare earth and transition metalones) fully aligned, one in opposition to the other. For theDyNi 0.50 Mn 0.50 O 3 sample we do not see any field-inducedanomaly on the hysteresis curves up to 20 T.Figure 129: Thermal dep<strong>en</strong>d<strong>en</strong>ce of the ZFC-FC magnetizationfor EuCo 0.50 Mn 0.50 O 3 and DyCo 0.50 Mn 0.50 O 3 measured at0.025 T.Temperature dep<strong>en</strong>d<strong>en</strong>ce of the magnetization is shown infigure 129 for EuCo 0.50 Mn 0.50 O 3 and DyCo 0.50 Mn 0.50 O 3 .Samples were first cooled under no magnetic field, th<strong>en</strong>the static field of 0.025 T was applied and samples allowedwarming until 300 K (ZFC). Th<strong>en</strong>, they were subsequ<strong>en</strong>tlycooled under the same static field (FC). ZFC branch forEu sample shows that, upon warming, the Co-Mn sublatticeorders in an antiferromagnetic state with a small ferromagneticcompon<strong>en</strong>t due to non-linearity of the spins. Thelow magnetic mom<strong>en</strong>t of Eu and the low external field appliedto the sample, result in almost no contribution fromEu. During the FC procedure, the transition metal sublatticeorders ferromagnetically at T C = 130 K. For the Dysample we can notice that the ZFC curve starts from a finitevalue at 2 K and decreases to almost zero wh<strong>en</strong> thetemperature increases. This is just due to the Curie-Weissbehaviour of Dy 3+ that follows 1/T law, typical of freespinnon-correlated mom<strong>en</strong>ts. For higher temperatures, theFigure 130: Magnetization loop at2.5K for (a) EuCo 0.50 Mn 0.50 O 3 (insert: EuNi 0.50 Mn 0.50 O 3 ) and(b) DyCo 0.50 Mn 0.50 O 3 (insert: DyNi 0.50 Mn 0.50 O 3 ).A. B. AntunesO. Peña (Sci<strong>en</strong>ces Chimiques de R<strong>en</strong>nes, Université de R<strong>en</strong>nes 1, R<strong>en</strong>nes, France), C. Moure, A. Moure (Electrocerámicas,Instituto de Cerámica y Vidrio, CSIC, Madrid, Spain)91


MAGNETIC SYSTEMS 2009High magnetic field study in chromium-based Mn 1−x Cd x Cr 2 S 4 thiospinelsMaterials with spinel AB 2 X 4 structure are widely studiedbecause of outstanding physical properties, e.g. halfmetallicityand colossal magnetoresistance. Among thesematerials, the MnCr 2 S 4 thiospinel pres<strong>en</strong>ts a collinear ferrimagneticstructure at 65 K and a Yafet-Kittel transitionat ∼ 6 K toward a triangular non collinear state [Tsurkanet al., Phys. Rev. B 68, 134434 (2003)]. Application ofvery high magnetic fields produces a reori<strong>en</strong>tation of themom<strong>en</strong>ts toward a ferromagnetic state.We investigate here a solid solution obtained by partial substitutionof magnetic Mn by non-magnetic Cd. Sampleswere prepared from high-purity elem<strong>en</strong>ts, sealed in evacuatedquartz ampoules, using I 2 as transport ag<strong>en</strong>t. Ampouleswere slowly heated up to 800 ◦ C over a period of1 week. The resultant was reground, pelletized and firedat 900 ◦ C for 3 days. Samples were characterized by X-raydiffraction. Patterns were fully indexed in the Space GroupFd3m, with no secondary phases observed within the limitsof the experim<strong>en</strong>tal detection. Magnetic measurem<strong>en</strong>tswere performed on specim<strong>en</strong>s cut from ceramic pellets.The ordered regime was investigated through ZFC/FC magnetizationcycles performed under low applied field (figure131). Samples were first cooled under non-magneticfield and th<strong>en</strong> warmed from 2 up to 300 K under the appliedfield of 0.01 T (ZFC mode). Once in the paramagnetic state,samples were th<strong>en</strong> cooled down to the lowest temperatureof 2 K under the same applied field (FC mode).into a stronger overall ferromagnetism [Barahona et al., J.Alloys Comp. 480, 291 (2009)].Figure 132: Magnetization at giv<strong>en</strong> temperatures for theMn 1−x Cd x Cr 2 S 4 solid solution.In order to obtain a better knowledge concerning spins reori<strong>en</strong>tation,magnetization measurem<strong>en</strong>ts were performedat fixed temperatures in fields up to 20 T (figure 132). Datashow a progressive loss of the antiferromagnetic interactionsbetwe<strong>en</strong> A and B sublattices, favouring the parallelalignm<strong>en</strong>t of mom<strong>en</strong>ts pointing into the same direction, thatis, the ferromagnetism of the Cr 3+ network. To be noticedthat the threshold field for the mom<strong>en</strong>ts realignm<strong>en</strong>tis 5 times smaller (H C ∼ 6 − 8 T) than the one reported forpure MnCr 2 S 4 . However, for all samples, magnetizationsdo not attain full saturation of free spins at 20 T (see figure133).Figure 131: ZFC/FC magnetization for Mn 1−x Cd x Cr 2 S 4 solidsolution (ZFC : op<strong>en</strong> symbols ; FC : filled symbols).In the par<strong>en</strong>t compound MnCr 2 S 4 , the Cr 3+ and Mn 2+networks are ferromagnetic but point in opposite direction,creating a ferrimagnetic state, while in the solid solution(Mn 1−x Cd x )Cr 2 S 4 , the antiferromagnetic interactionbetwe<strong>en</strong> the Mn and Cr networks is progressively lost wh<strong>en</strong>the cont<strong>en</strong>t of non-magnetic cadmium increases, resultingFigure 133: Normalized magnetization at 4 Kfor Mn 1−x Cd x Cr 2 S 4 . The normalization was done with respectto effective magnetic mom<strong>en</strong>t calculated from high temperaturedata of figure 131 fitted to Curie-Weiss law (not shown).A. B. AntunesP. Barahona (Instituto de Ci<strong>en</strong>cias Básicas, Universidad Católica del Maule, Talca, Chile), A. Galdamez, V. Manriquez(Departam<strong>en</strong>to de Química, Facultad de Ci<strong>en</strong>cias, Universidad de Chile, Santiago, Chile), C. M. Campos, O. Peña(Sci<strong>en</strong>ces Chimiques de R<strong>en</strong>nes, Université de R<strong>en</strong>nes 1, R<strong>en</strong>nes, France)92


2009 MAGNETIC SYSTEMSMagnetic properties of ErCo x Mn 1−x O 3 perovskitesA spin reversal ph<strong>en</strong>om<strong>en</strong>on in perovskite manganitesABO 3 may appear wh<strong>en</strong> the rare-earth elem<strong>en</strong>t, having alarge magnetic mom<strong>en</strong>t (e.g. Gd, Er), interacts with theMn 3+ -Mn 4+ sublattice. This has be<strong>en</strong> found in manganitespartially substituted at the A-site by alkaline earth elem<strong>en</strong>ts.B-site substitutions also drastically modify the physicochemicalproperties of these materials, since for each dival<strong>en</strong>ttransition metal introduced in the lattice, a Mn 3+ ionwill transform into Mn 4+ . If the substitute is Co, the solidsolution may ext<strong>en</strong>d over a large range of conc<strong>en</strong>trationssince cobalt may adopt a 2+ and a 3+ oxidation states, dep<strong>en</strong>dingon the synthesis conditions. In these materials, thetotal magnetization changes its sign wh<strong>en</strong> field-cooled dueto a negative polarization of the rare-earth mom<strong>en</strong>t in thepres<strong>en</strong>ce of the internal field created by the ordered manganesesublattice [Peña et al., J. Magn. Magn. Mater. 310,159 (2007)].The isothermal magnetization shows two interesting features:(i) an intersection of the decreasing and increasingbranches of the magnetization loop at low fields, related tothe spin reversal <strong>des</strong>cribed above; (ii) a step-like increase athigh fields wh<strong>en</strong> the applied magnetic field increases [Peñaet al., J. Magn. Magn. Mater. 312, 78 (2007)]. Thesetwo anomalies have be<strong>en</strong> observed only in the Er-Co-basedsystem, for materials close to the ErCo 0.50 Mn 0.50 O 3 composition(figure 134).Figure 135: High field magnetization for ErCo x Mn 1−x O 3 samplesnormalized for the value at 15 T.Important results were obtained: (a) the high field transitionshifts towards higher applied fields wh<strong>en</strong> temperaturedecreases; (b) the high field transition shifts towards higherapplied fields wh<strong>en</strong> the Co/Mn conc<strong>en</strong>tration changes fromthe particular 50/50 ratio; (c) the magnetization does notsaturate at the highest applied field, but the ferromagneticloop <strong>en</strong>ds up at about 10 T; (d) no abrupt jumps are observedfor temperatures above 3 K; (e) magnetic relaxationis observed just before the transition occurs (figure 136).Magnetization loop for the ErCo 0.50 Mn 0.50 O 3 com-Figure 134:position.Figure 136: Magnetization as a function of time forErCo 0.50 Mn 0.50 O 3 . Insert: fit to a logarithmic behaviour.Furthermore, the high-field transition is of a dynamical naturesince both its amplitude and position dep<strong>en</strong>d on thesweep-rate of the applied-field. To get a deeper insight ofthis anomaly, high-field magnetization measurem<strong>en</strong>ts wereperformed at 4 K. (figure 135).Based on these results, several sc<strong>en</strong>arios are possible, suchas, dynamical movem<strong>en</strong>ts of domain walls, magnetic relaxationof ferromagnetic clusters, metamagnetic-like interactionsbetwe<strong>en</strong> Er 3+ and Co 2+ -Mn 4+ mom<strong>en</strong>ts.A. B. AntunesO. Peña (Sci<strong>en</strong>ces Chimiques de R<strong>en</strong>nes, Université de R<strong>en</strong>nes 1, R<strong>en</strong>nes, France), C. Moure (Electrocerámicas, Institutode Cerámica y Vidrio, CSIC, Madrid, Spain), S. de Brion (Institut Néel, Gr<strong>en</strong>oble, France)93


MAGNETIC SYSTEMS 2009Ferromagnetic domains in nanosized erbium perovskitesCooperative ph<strong>en</strong>om<strong>en</strong>a constitute an important researcharea because of many applications at the frontiers of chemistry,physics and electronics. Perovskites manganiteshave received growing att<strong>en</strong>tion because of mixed-val<strong>en</strong>ceMn 4+ /Mn 3+ and resulting magnetoresistance effect. Wepreviously reported interesting results in Er(Co,Mn)O 3 dueto an antiferromagnetic interaction betwe<strong>en</strong> Er and |Co,Mn|sublattices, producing a reversal of the magnetic mom<strong>en</strong>tand formation of ferromagnetic domains. An avalanchemechanism occurs under moderate magnetic fields (∼35 kOe), leading to the rotation of the domains in one ormore steps, dep<strong>en</strong>ding on the rate of variation of the appliedfield and on the grains formation [Peña et al., J. Magn.Magn. Mater. 312, 78 (2007)].In order to investigate the influ<strong>en</strong>ce of the micro-structurewe have elaborated nanosized materials and correlated themagnetic response to the grains size and to boundaries percolation.ErCo 0.50 Mn 0.50 O 3 compound was prepared at700 ◦ C by a citrate method and further calcined at increasingtemperatures. Samples were characterized by X-raydiffraction both before and after the sintering conditions,confirming the pres<strong>en</strong>ce of a pure perovskite orthorhombicPbnm structure and phase purity was checked by <strong>en</strong>ergydispersive analysis. The micro-structure, characterizedby scanning electron microscopy, consists of homog<strong>en</strong>eousspherical grains of 20 − 30 nm diameter for as-preparedsample synthesized at 700 ◦ C, which progressively growwith increasing sintering temperature, attaining 100 − 200nm and a very good percolation at 950 ◦ C, that is, wh<strong>en</strong>grains fuse together and grain barriers almost disappear.Magnetic measurem<strong>en</strong>ts were performed on the startingmaterial and sintered pellets.temperatures of 950 ◦ C and above, that is, wh<strong>en</strong> grain barrierst<strong>en</strong>d to disappear. We correlate this sudd<strong>en</strong> jump withthe reori<strong>en</strong>tation of ferromagnetic domains. At the sametime, the critical field H c decreases with increasing annealingtemperature suggesting that ferromagnetic domains rotatemore easily inside a large homog<strong>en</strong>eous grain since nobarriers are pres<strong>en</strong>t.To confirm the reori<strong>en</strong>tation ph<strong>en</strong>om<strong>en</strong>on, we have performedsubsequ<strong>en</strong>t runs at 2 K, measuring the full M(H)loop. The starting bulk corresponds to a piece of the pelletsintered at 950 ◦ C. This piece was th<strong>en</strong> crushed into finepowder (sieved at 80 µm) and let free to rotate under theaction of the applied field. In a third run, this same powderwas homog<strong>en</strong>eously dispersed inside a drop of liquefiedvacuum grease, th<strong>en</strong> froz<strong>en</strong> at 2 K in order to blockany rotation of the fine particles, and performed a M(H)loop. Finally, the gel-type solution was heated at 350 K insidethe cryostat, and a 50 kOe field was applied. The gelwas th<strong>en</strong> cooled under the same static field down to 2 K,with all domains ori<strong>en</strong>ted parallel to the applied field. Figure138 shows the full M(H) loop under these 4 differ<strong>en</strong>texperim<strong>en</strong>tal set-ups.Figure 138: M(H)-loops measured under 4 differ<strong>en</strong>t conditionsfor ErCo 0.50 Mn 0.50 O 3 sample calcined at 950 ◦ C.Figure 137: Positive part of magnetization loops at T = 2 K forgiv<strong>en</strong> calcination temperatures (in ◦ C).Figure 137 pres<strong>en</strong>ts part of the M(H)-loops for selectedpellets. Below an annealing temperature of about 950 ◦ C,the magnetization increases smoothly with increasing field,until an inflexion point occurs at about 40 kOe. This inflexionpoint transforms into a sudd<strong>en</strong> jump at H c , for sinteringIt can immediately be noticed that the most significantchange in the magnetization loop concerns the height of thejump, which increases by about 60% in the ori<strong>en</strong>ted powderwith respect to the bulk ceramics. It is also evid<strong>en</strong>t that,wh<strong>en</strong> the particles are homog<strong>en</strong>eously dispersed and not allowedto rotate (run 3), the magnetization jump is smoothedout and becomes just an inflexion point. In conclusion, wehave unambiguously shown that grains size and percolationare the most important mechanisms in the rotation of magneticdomains in this material.A. B. AntunesC. M. Campos, O. Peña (Sci<strong>en</strong>ces Chimiques de R<strong>en</strong>nes,Université de R<strong>en</strong>nes 1, R<strong>en</strong>nes, France), G. Pecchi (Facultadde Ci<strong>en</strong>cias Químicas, Universidad de Concepción, Concepción, Chile)94


2009Biology, Chemistry and Soft Matter95


2009 BIOLOGY, CHEMISTRY AND SOFT MATTERConcerted spin crossover and symmetry breaking yield three thermally- andone light-induced crystallographic phases of a novel molecular materialSpin crossover (SC) complexes have be<strong>en</strong> widely studiedover the last deca<strong>des</strong>: the reversible low-spin(LS) ⇄ high-spin (HS) switching triggered by a changein temperature or by light irradiation, has attractedmuch interest for pot<strong>en</strong>tial applications in informationstorage. A new SC material [Fe II H 2 L 2−Me ][PF 6 ] 2 ,1 where H 2 L 2−Me d<strong>en</strong>otes bis[((2-methylimidazol-4-yl)methylid<strong>en</strong>e)-3-aminopropyl] ethyl<strong>en</strong>e diamine, hasbe<strong>en</strong> synthesized.Figure 139 shows the variation of the χ M T product of 1,evid<strong>en</strong>cing a two-step SC process. The INT ⇄ LS step c<strong>en</strong>teredaround 97 K shows a thermal hysteresis loop of 6 Kwidth, characteristic of a first order transition. Wh<strong>en</strong> 1 wasirradiated with gre<strong>en</strong> light, a quantitative light-induced excitedspin state trapping effect (LIESST) was clearly observed.Wh<strong>en</strong> the irradiation was stopped, two steps relaxationto the fully LS state was observed upon increasing T.Figure 139: Temperature dep<strong>en</strong>d<strong>en</strong>ce of the χ M T product oncooling () th<strong>en</strong> warming mode () and after irradiating the sampleat 10 K with a 532 nm laser light. ()at sweeping rate of 1 Kmin-1The crystal structures of 1 were determined by singlecrystalXRD. In the HS state (250 K, P22 1 2 1 ), the averageFe-N bond l<strong>en</strong>gth 〈Fe-N〉 = 2.190 Å is typical of an HSFe II site with six N donors. The crystal structure is madeof hydrog<strong>en</strong> bonded cation layers and anion layers in the(a,b) plane (Figure 140a). In the INT phase, an orderingof spin-states occurs among the Fe II sites, as a cell doublingalong the crystalline axis. The space group decreasesto the non-isomorphic monoclinic subgroup P2 1 : there aretwo non equival<strong>en</strong>t cation sites (Figure 140b), one mainlyHS (〈Fe1-N〉 = 2.13(1) Å) and the other one is mainly LS(〈Fe2-N〉 = 2.04(1) Å). The ordering in the INT phase resultsin the LS-HS-HS-LS pattern. Below 97 K, in the LSphase (P2 1 2 1 2 1 ), the unit cell has changed to (4a,b,c) andinclu<strong>des</strong> two indep<strong>en</strong>d<strong>en</strong>t LS cations per unit cell (〈Fe1-N〉= 2.012 Å = 〈Fe2-N〉) (Figure 140c). Because of the symmetrybreakings, a related distortion of each molecule occurs,accompanied with slight tilts as well as displacem<strong>en</strong>tsof the ions.A novel structural reorganization occurs upon g<strong>en</strong>erationof the PIHS state: the P22 1 2 1 space group is the same asin the HS phase but with differ<strong>en</strong>t translation symmetry.The structure inclu<strong>des</strong> two indep<strong>en</strong>d<strong>en</strong>t complex cationsper unit cell (Figure 140d) with Fe-N bond l<strong>en</strong>gths typicalof HS Fe II sites (〈Fe1-N〉 = 2.17(1) Å and 〈Fe2-N〉 =2.18(1) Å). This is the first-case of photoinduced SC involvingsymmetry breaking while previous report demonstratedisostructural reorganization. The occurr<strong>en</strong>ce of four differ<strong>en</strong>tphases with differ<strong>en</strong>t symmetries is unique and shouldbe related to the strong intermolecular interactions and tothe specific packing of anion and cation layers.Figure 140: Projection of the crystal packing in the HS phase(a), for the INT phase (b), the LS state (c) and PIHS (d). [HS(blue) and LS (red) sites] Additional projections along the multipliedcrystals axis on the right show the motions of the ions.N. BréfuelL. Toupet, E. Collet (University of R<strong>en</strong>nes), H. Watanabe, K. Tanaka (University of Kyoto, Japan), J.-P. Tuchagues (Universityof Toulouse), N. Matsumoto (University of Kumamoto, Japan)97


BIOLOGY, CHEMISTRY AND SOFT MATTER 2009Magnetostructural correlations in Tetrairon(III) single-molecule magnetsSlow magnetic relaxation in molecular systems is a livelyresearch area which spans the interface betwe<strong>en</strong> chemistry,physics and material sci<strong>en</strong>ce. This ph<strong>en</strong>om<strong>en</strong>on is observedin two main families of compounds: single-molecule magnets(SMM) and single-chain magnets (SCM). The persist<strong>en</strong>ceof magnetization in such systems is limited to lowtemperature (below about 4.2 K), but can be in principleexploited for applications in the field of magnetic storageand information processing. Tetrairon(III) complexes withformula [Fe 4 (L) 2 (dpm) 6 ],are providing a growing class ofSingle Molecule Magnets displaying unpreced<strong>en</strong>ted syntheticflexibility and ease of functionalization ( Hdpm =2,2,6,6 − tetramethyl-heptane-3,5-dione).Here we report on three novel derivatives prepared byusing as bridging ligands p<strong>en</strong>taerythritol monoethers,H 3 L = R’-O-CH 2 C(CH 2 OH) 3 with R’=allyl (1), (R,S))-2-methyl-1-butyl (2), and S-2-methyl-1-butyl (3) along witha new polymorph the complex containing 11-(acetylthio)-2,2-bis(hydroxymethyl) undecan-1-ol ligands (4b) [Gregoliet al., Chem. Eur. J. 15, 6456 (2009)]. High-Frequ<strong>en</strong>cyEPR (HF-EPR) spectra have be<strong>en</strong> collected, at two frequ<strong>en</strong>cies(190 and 230 GHz) and several temperatures betwe<strong>en</strong> 5and 30 K, on polycrystalline samples of the four complexesin order to determine the zero-field splitting (zfs) parametersin the ground spin state. The spectra obtained show thetypical behavior of systems with an S = 5 ground spin statecharacterized by an easy-axis type anisotropy (D < 0):H = µ 0 B.g.S + DS 2 z + E(S 2 x − S 2 y) + B 0 4 O0 4 (17)where O 0 4 is a Stev<strong>en</strong>s operator, while D, E and B0 4 arethe crystal field parameters defining the anisotropy of thesystem. Setting an isotropic Landé factor g = 2.0, the bestsimulations of experim<strong>en</strong>tal spectra were obtained with thefollowing parameters (in cm −1 ): D = −0.417, E = 0.015,B 0 4 = +1.3 × 10−5 for (1a), D = −0.435, E = 0.009,B 0 4 = +0.9 × 10−5 for (1b), D = −0.449, E = 0.030,B 0 4 = +2.4 × 10−5 for (2), D = −0.442, E = 0.0312,B 0 4 = +1.65 × 10−5 for (3) and D = −0.412, E = 0.006,B 0 4 = +1.8 × 10−5 for (4b)(figure 1). (1a) and (1b) standfor the two structurally inequival<strong>en</strong>t molecules pres<strong>en</strong>t inthe cell of crystal (1). Experim<strong>en</strong>tal and calculated spectrafor complex (2) at 230 GHz are displayed in figure 141.In (1-3) and (4b), and in other six isostructural compoundspreviously reported, a remarkable correlation is found betwe<strong>en</strong>the axial zfs parameter D and the helical pitch γof the propeller-like structure (figure 142). γ is definedas the average dihedral angle betwe<strong>en</strong> the mean Fe4 planeand the three FeO 2 Fe ”bla<strong>des</strong>”.The relationship is directlydemonstrated by (1), which features both structurally andmagnetically inequival<strong>en</strong>t molecules in the crystal. Thetwo polymorphs of (4) ((4a,b)) span the whole range ofanisotropies for [Fe 4 (L) 2 (dpm) 6 ] complexes, suggestingthat crystal packing effects may be largely responsible forthe observed structural and magnetic differ<strong>en</strong>ces.The dynamics of the magnetization in the four complexeshas be<strong>en</strong> investigated by AC susceptometry, and the resultsanalyzed by master-matrix calculations. The large rhombicityof (2) and (3) is found responsible for the fast magneticrelaxation observed in the two compounds. However, complex(3) shows an additional faster relaxation mechanismwhich is unaccounted for by the set of spin-Hamiltonianparameters determined by HF-EPR.Figure 141: HF-EPR experim<strong>en</strong>tal (bold) and simulated powderspectra recorded at 230 GHz on derivative (2).Figure 142: Axial anisotropy D versus helical pitch γ for thetwelve Tetrairon(III) propellers so far characterized. The redpoints correspond to the four derivatives discussed here. The solidline correspond to the best fit for the derivatives featuring twotripodal ligands.A.L. Barra, P. NeugebauerA. Cornia, L. Gregoli, C. Dianeli (University of Mod<strong>en</strong>a, Italy), R. Sessoli (University of Flor<strong>en</strong>ce, Italy)98


2009Applied Superconductivity99


2009 APPLIED SUPERCONDUCTIVITYMagnetic field behaviour of ex-situ processed MgB 2 multifilam<strong>en</strong>tary wiresIn order to make MgB 2 useful not only for dc but also for acapplications further conductor developm<strong>en</strong>t and optimizationare still needed, in particular to reduce the ac lossescaused by magnetic hysteresis in the MgB 2 core, filam<strong>en</strong>tcoupling and eddy curr<strong>en</strong>ts flowing through the metallicmatrix. In this context research work should be focused onmultifilam<strong>en</strong>tary strands with a large number of very finefilam<strong>en</strong>ts, twisted filam<strong>en</strong>ts and non-magnetic and high resistivitysheath.We have focused our work on obtaining multifilam<strong>en</strong>taryconductors with a large number of very fine filam<strong>en</strong>ts. Inthis context, the powder’s granulometry can play a crucialrole. In this experim<strong>en</strong>t we have prepared two MgB 2 startingpowders which are either not milled (NM) or milled(M) with differ<strong>en</strong>t granulometries (NM= 1.5 µm and M=450 nm) and by the ex-situ powder in tube (PIT) methodwe have realized multifilam<strong>en</strong>tary wires with 19, 91 and361 filam<strong>en</strong>ts and an average size of each filam<strong>en</strong>t of 279,110 and 30 µm respectively. In figure 143 the cross sectionsof the three wire types are shown.We have studied the relationship betwe<strong>en</strong> grain and filam<strong>en</strong>tsize in terms of transport properties. The measuredcritical curr<strong>en</strong>t d<strong>en</strong>sities (J C ) for the samples with NM powderand M powder are reported in figure 144. The criticalcurr<strong>en</strong>t d<strong>en</strong>sity improves with milling for all samples asreported in our previous work [A. Malagoli et al J. Appl.Phys. 104, 103908 (2008)]. Focusing on the behaviour ofthe not milled samples, passing from 19 to 91 filam<strong>en</strong>ts aremarkable critical curr<strong>en</strong>t d<strong>en</strong>sity degradation is evid<strong>en</strong>t,that is partially recovered going to 361 filam<strong>en</strong>ts. On thecontrary for the milled samples 19M and 91M have almostid<strong>en</strong>tical critical curr<strong>en</strong>t d<strong>en</strong>sity - a slightly better behaviourin field being observed in 91M. Wh<strong>en</strong> the number of filam<strong>en</strong>tsincreases up to 361, critical curr<strong>en</strong>t d<strong>en</strong>sity decreasesstaying though above the 361NM.Such a behaviour of the critical curr<strong>en</strong>t d<strong>en</strong>sity in field cannotbe explained or well understood simply considering theeffects of milling. In these complex conductors several factorshave to be tak<strong>en</strong> into account which have an effect onthe transport properties: the starting granulometry of theMgB 2 powders, the cold deformation force and the final filam<strong>en</strong>tsize. Therefore, in the final analysis, the capabilityof these conductors to transport high critical curr<strong>en</strong>ts cruciallydep<strong>en</strong>ds on a proper balance of these parameters. Inthis work we have obtained the best ratio filam<strong>en</strong>t size/grainsize on a 91 filam<strong>en</strong>ts wire with an average filam<strong>en</strong>t size ofabout 110 µm and a powder starting average grain diameterof about 450 nm. A finer MgB 2 granulometry seems to b<strong>en</strong>eeded to realize very thin filam<strong>en</strong>ts (10−30 µm) with highcritical curr<strong>en</strong>t d<strong>en</strong>sity.Figure 143: Images of differ<strong>en</strong>t cross sections through the wireswith 19, 91 and 361 filam<strong>en</strong>ts respectively.Figure 144: Transport critical curr<strong>en</strong>t d<strong>en</strong>sity (J C ) for differ<strong>en</strong>tmilled (M) and not milled (NM) samples measured up to magneticfields of 13 T using a wide bore resistive magnet and a Heliumbath cryostat (T = 4.2 K).E. MossangA. Malagoli, G. Romano, M. Vignolo, C. Ferdeghini, M. Putti (CNR-INFM LAMIA, G<strong>en</strong>ova, Italy), S. Brisigotti, G.Grasso, A. Tumino (Columbus Superconductors S.p.A., G<strong>en</strong>ova, Italy)101


APPLIED SUPERCONDUCTIVITY 2009Superconductivity of C and TiC doped multi-filam<strong>en</strong>tary MgB 2 wiresRec<strong>en</strong>tly a great deal of both fundam<strong>en</strong>tal and technical researchhas be<strong>en</strong> carried out on carbide-doped MgB 2 dueto its high upper critical field (H c2 ) which pres<strong>en</strong>ts considerableinterest for the fabrication of practical magnets, especiallythe GM-cryocooled MRI magnet. For <strong>en</strong>gineeringapplications, it is necessary to make MgB 2 superconductorsinto multi-filam<strong>en</strong>tary wires or tapes. The in-situ and exsitupowder-in-tube (PIT) processes have become the dominantor standard methods due to their commercial pot<strong>en</strong>tialfor large-scale and low-cost production of MgB 2 wires andtapes.Figure 145: Cross section of the differ<strong>en</strong>t multi-filam<strong>en</strong>tMgB 2 /NbCu wires.In this work, various multi-filam<strong>en</strong>t MgB 2 /NbCu roundwires with carbon or TiC doping have be<strong>en</strong> fabricated byin-situ PIT method at the Northwest Institute for NonferrousMetal Research (NIN). The typical diameter of the finalwire is 1 mm. The MgB 2 coil was fabricated using thewind and react method with a 1.5 m long wires and a heattreatm<strong>en</strong>t at 680 ◦ C for 1.5 h. The transport critical curr<strong>en</strong>tof the MgB 2 coils was measured with magnetic fields upto 10 T at various temperatures using a standard four probemethod. The critical curr<strong>en</strong>t d<strong>en</strong>sity, J c , of the coil was calculatedfrom the measured critical curr<strong>en</strong>t I c divided by thecross sectional area of the MgB 2 core.Figure 145 shows the 6-, 12- and 36-filam<strong>en</strong>taryMgB 2 /NbCu wires with amorphous carbon doping. Thevolume of MgB 2 in whole wires is around 20%, 14% and14%, respectively. Figure 146 shows the transport criticalcurr<strong>en</strong>t d<strong>en</strong>sity J c values as a function of applied field at20 K for the multi-filam<strong>en</strong>tary MgB 2 coils with amorphouscarbon or TiC doping. The 6-filam<strong>en</strong>t wires with carbondoping has the largest J c , as high as 4.5×10 4 A/cm 2 at 2 T.The large value of J c in this sample may be due to the goodgrain connectivity and strong flux pinning force. This resultindicates that carbon doping is b<strong>en</strong>eficial for the fabricationof high performance long l<strong>en</strong>gth multi filam<strong>en</strong>tary MgB 2wires.Figure 146: Transport critical curr<strong>en</strong>t d<strong>en</strong>sity of differ<strong>en</strong>t multi–filam<strong>en</strong>tary MgB 2 coils at T = 20 K.Figure 147 shows the result of the transport J c versus Hmeasurem<strong>en</strong>ts at temperatures from 4.2 to 30 K measuredfor 6-filam<strong>en</strong>t wires with carbon doping. This value islower than the best values found in the literature, but webelieve that the transport J c could be improved by optimizingvarious processing parameters.In summary, the J c of multi-filam<strong>en</strong>tary long l<strong>en</strong>gth MgB 2wires were <strong>en</strong>hanced by amorphous carbon doping. Thehighly reactive amorphous carbon can easily substitute intothe lattice of MgB 2 ev<strong>en</strong> with a heat-treatm<strong>en</strong>t at lower temperature.On the other hand, the lower heat-treatm<strong>en</strong>t temperatureresults in a smaller MgB 2 grain size, which introduceda high d<strong>en</strong>sity of flux-pinning c<strong>en</strong>ters.Figure 147: Transport critical curr<strong>en</strong>t d<strong>en</strong>sity of a 6-filam<strong>en</strong>tMgB 2 coil at various temperatures.E. MossangQ.Y. Wang, G. Yan (Northwest Institute for Non-Ferrous Metal Research, Xi’an, China), A. Sulpice (Institut Neel,Gr<strong>en</strong>oble102


2009 APPLIED SUPERCONDUCTIVITYPhthalocyanine doping to improve critical curr<strong>en</strong>t d<strong>en</strong>sities in MgB 2 tapesCarbohydrates show a promin<strong>en</strong>t capability in the criticalcurr<strong>en</strong>t, J c − B, <strong>en</strong>hancem<strong>en</strong>t of MgB 2 . It is claimed thatthese materials can decompose at relatively low temperature,and g<strong>en</strong>erate a lot of reactivate carbon atoms beforethe MgB 2 phase formation. The reactivate carbon atomsand small sized impurities are favorable for good superconductingproperties of MgB 2 . Compared to nano-sized C orSiC, carbohydrate doping can achieve a uniform dispersionwithin the MgB 2 matrix. As the insulated MgO particles arevery harmful to the MgB 2 grain connectivity, oxyg<strong>en</strong>-freecarbon compounds, which will not produce MgO by reactionwith MgB 2 , are preferable to use as MgB 2 dopants.In this work, we tried phthalocyanine (C 32 H 18 N 8 ), whichhas carbon 72.8-76.6%, nitrog<strong>en</strong> 21.1-22.3%, and no oxyg<strong>en</strong>cont<strong>en</strong>t, as MgB 2 doping material. The relationshipsbetwe<strong>en</strong> the critical curr<strong>en</strong>t properties, crystallinity, irreversibilityfield (H irr ) and upper critical field (H c2 ) werestudied as a function of the doping level of phthalocyanine.Figure 148 shows the field dep<strong>en</strong>d<strong>en</strong>ce of transport J cat 4.2 K for undoped and phthalocyanine-doped MgB 2 /Fetapes. Clearly, the in-field J c properties of MgB 2 tapes weremuch improved by the phthalocyanine doping, suggestingthat H c2 was <strong>en</strong>hanced. The best J c − B properties were obtainedin 2.2 wt% phthalocyanine-doped samples. At 4.2 Kand 10 T, a J c value higher than 1.6 × 10 4 A cm −2 wasachieved, which is almost an order of magnitude higherthan that for pure ones. On the other hand, wh<strong>en</strong> the phthalocyaninedoping amount increased to 3 wt%, the J c valuesstarted to decrease, while the field dep<strong>en</strong>d<strong>en</strong>ce was almostnot affected. This suggests that the excess phthalocyanineaddition will have a negative effect on the grainconnectivity and thus the coupling of MgB 2 grains, dueto the non-superconducting and g<strong>en</strong>erally insulating secondphases introduced by phthalocyanine addition.Figure 148: Transport J c − B properties of Fe-sheathed undopedand doped tapes heated at 800 ◦ C for 1 hour. The measurem<strong>en</strong>tswere performed in magnetic fields parallel to the tape surface at4.2 K.The normalized temperature dep<strong>en</strong>d<strong>en</strong>ce of H c2 and H irrfor all samples is shown in figure 149. Although the actualcarbon cont<strong>en</strong>ts in phthalocyanine-doped samples aresmall, the H c2 and H irr values of MgB 2 have be<strong>en</strong> greatly<strong>en</strong>hanced. For example, the H c2 and H irr of the 3 wt%phthalocyanine-doped sample at 24 K are 8.7 and 6 T, respectively,which is markedly higher than those of the undopedsamples.Figure 149: Normalized temperature dep<strong>en</strong>d<strong>en</strong>ce of H irr and H c2for undoped and phthalocyanine-doped samples sintered at 800 ◦ C.H c2 and H irr were defined as H c2 = 0.9R (T c ) and H irr = 0.1R (T c )from the R versus T curve.E. MossangX. Zhang, Y. Ma, D.Wang, , Z. Gao, L. Wang, Y. Qi (Institute of Electrical Engineering, Chinese Academy of Sci<strong>en</strong>ces,Beijing, China) S. Awaji, K. Watanabe (Institute for Materials Research, Tohoku University, S<strong>en</strong>dai, Japan)103


APPLIED SUPERCONDUCTIVITY 2009Critical curr<strong>en</strong>t measurem<strong>en</strong>ts on Bi-2212High critical temperature superconductors (HTS) op<strong>en</strong> extremelyinteresting perspectives for high magnetic field applicationssuch as high field magnets for NMR or SMES,nuclear fusion, or future colliders. The demand is high for25−50 T magnets which is beyond the possibilities offeredby low critical temperature superconductors, i.e. Nb 3 Sn.The possibility of precisely measuring the rather elevatedcritical curr<strong>en</strong>ts of superconductors in a high magnetic field<strong>en</strong>vironm<strong>en</strong>t is crucial for the developm<strong>en</strong>t of HTS magnets.(l<strong>en</strong>gth 30 mm) can be se<strong>en</strong> in figure 1. The results havebe<strong>en</strong> checked by performing cross characterizations at theSACM, CEA Saclay.Complete characterization of Bi-2212 and YBaCuO wiresand tapes at high magnetic fields and low temperatures(from 4.2 to 80 K) can be performed using this new VTI,which will be a very useful tool for the studies of HTS inthe frame of the SUPER-SMES project.Interest for Bi-2212 round wire for high magnetic field applicationsincreased rec<strong>en</strong>tly due to the wires outstandingperformance concerning their intrinsic transport properties.The critical curr<strong>en</strong>t d<strong>en</strong>sity is higher than 1000 MA/m 2at 4.2 K and 45 T. Equally the second g<strong>en</strong>eration (2G)of YBaCuO coated HTS conductors, show very promisingperformances in terms of critical curr<strong>en</strong>ts under very highmagnetic fields. In addition, their mechanical properties areexcell<strong>en</strong>t for the ion beam assisted deposition (IBAD) route.The mechanical performances are of great importance forvery high field magnets. Significant progress has also be<strong>en</strong>achieved in terms of l<strong>en</strong>gths, to the point where it it is nowpossible fabricate HTS magnets. The possibility to operateat higher temperatures than 4.2 K improves considerablythe stability of the magnet due to the rapid increase of thespecific heat at higher temperatures. The stability is one ofthe limitations of LTS magnets in term stored magnetic <strong>en</strong>ergyper unit mass. On the other hand the protection of themagnet is much more difficult since the propagation velocitiesare low, leading to a difficult detection of any qu<strong>en</strong>ch.HTS magnet protection has be<strong>en</strong> id<strong>en</strong>tified as an issue fortheir developm<strong>en</strong>t.The HTS wires (BiSrCaCuO PIT or YBaCuO coated conductor)are produced by Nexans or other providers (suchas OST). The typical cross section of the tapes is 4 ×0.1/0.2 mm 2 and a diameter of 1 mm for the round wires.The critical curr<strong>en</strong>t is of the order of ∼ 500 A in theself-field at 4.2 K. In the frame of the ANR “SUPERSMES” contract, a new Variable Temperature Insert hasbe<strong>en</strong> built in collaboration betwe<strong>en</strong> LNCMI and the NéelInstitute. The available space has be<strong>en</strong> optimized to maximizethe sample l<strong>en</strong>gth: a 34 mm long sample can betested in the 39 mm diameter field bore. An investigationof the sample anisotropy is possible, since the sample canbe rotated through 90 ◦ . Critical curr<strong>en</strong>ts are measured atthe LNCMI under fields up to 20 T. The sample holderhas be<strong>en</strong> <strong>des</strong>igned to <strong>en</strong>able measurem<strong>en</strong>ts on a VAMASlikecoil sample. Preliminary measurem<strong>en</strong>ts performed onBi-2212 VAMAS sample (l<strong>en</strong>gth 1 m) and short samplesFigure 150: (a) Transport I c versus magnetic field at differ<strong>en</strong>ttemperatures in parallel ori<strong>en</strong>tation for a VAMAS Bi-2212 tape.(b) Transport I c versus magnetic field at differ<strong>en</strong>t temperatures inparallel ori<strong>en</strong>tation for a short Bi-2212 sample.E. Mossang, F. Debray, J.P. Domps, S. DufresnesP. Brosse-Maron, O. Exshaw, P. Gandit, L. Porcar, P. Tixador (Institut Néel, CNRS, Gr<strong>en</strong>oble, France), J.M. Rey(DSM-DAPNIA-SACM, CEA Saclay, France)104


2009Magneto-Sci<strong>en</strong>ce105


2009 MAGNETO-SCIENCEChanges in the microstructure resulting from a high cooling rate in Fe-xC-Mnalloys in strong magnetic fieldThe impact of magnetic field on the microstructures obtainedafter rapid cooling is observed in Fe-xC-1.5wt%Mnsteels with x = 0.2 and 0.3 wt%C. The experim<strong>en</strong>ts aredone in a furnace in which alloys are water cooled in magneticfield from the aust<strong>en</strong>ite state [T.Garcin et al., Pat<strong>en</strong>t955380, 2009]. After holding at 1173K for 5min, the poweris switched off and the sample is qu<strong>en</strong>ched. More than200 K/s is obtained by water qu<strong>en</strong>ching betwe<strong>en</strong> 1173 Kand 373 K. The Figure show the SEM micrographs afterqu<strong>en</strong>ching under 0T and 16T.These modifications in the resulting microstructure by theapplication of a static magnetic field may be interestingwh<strong>en</strong> a mixture of ferrite, bainite and mart<strong>en</strong>site is <strong>des</strong>ired.Figure 1(a) shows the 0.2wt%C steel gra<strong>des</strong> cooled under0T and 16T. In the 0T sample, the microstructure is composedof a mixture of bainite (α B ) and mart<strong>en</strong>site(α’). Bainiteis a two-phase structure that contains ferrite-cem<strong>en</strong>titeregions formed from the eutectoid decomposition of aust<strong>en</strong>ite(γ). Mart<strong>en</strong>site is a product of diffusionless transformationand can occur in the form of thin, l<strong>en</strong>ticular plateswhich oft<strong>en</strong> ext<strong>en</strong>d right across the par<strong>en</strong>t gamma grains, oras packets of approximately parallel, fine laths whose sizeis g<strong>en</strong>erally smaller than that of the γ grains. Only severalislands of allotriomorphic ferrite are observed in the structure.The allotriomorphic ferrite (α) grows rapidly alongthe aust<strong>en</strong>ite grain boundary (which is an easy diffusionpath) but thick<strong>en</strong>s more slowly. Application of 16T leads toa considerable increase in the allotriomorphic ferrite fractionalong the prior aust<strong>en</strong>ite grains boundaries. In addition,a large amount of Widmansttt<strong>en</strong> ferrite (α W ) is detected bythe pres<strong>en</strong>ce of thin-wedge plates which have grown fromthe prior aust<strong>en</strong>ite grain boundaries.Figure 1(b) shows the 0.3wt%C steel gra<strong>des</strong> cooled under0T and 16T. In the 0T sample the microstructure iscomposed of a mixture of bainite and mart<strong>en</strong>site. No allotriomorphicferrite is observed probably due to the relativelyhigh carbon cont<strong>en</strong>t in alloy. Wh<strong>en</strong> the transformationoccurs under 16T, the microstructure is predominantlymart<strong>en</strong>site but also has allotriomorphic ferrite, Widmansttt<strong>en</strong>ferrite, bainite and ev<strong>en</strong> pearlite. The mart<strong>en</strong>site structurecan be here referred to as lath mart<strong>en</strong>site which consistsof mart<strong>en</strong>site needles with differ<strong>en</strong>t but well-definedori<strong>en</strong>tations. Notice that the spherical shape of pearlitecolonies is obvious in this sample because of the lack ofimpingem<strong>en</strong>t with other pearlite colonies. Vickers hardnessmeasurem<strong>en</strong>ts have be<strong>en</strong> performed for the differ<strong>en</strong>t alloyscomposition after thermomagnetic treatm<strong>en</strong>t. The applicationof a strong magnetic field results in a g<strong>en</strong>eral decreasein the hardness values. This reduction of hardness is relatedto the <strong>en</strong>hancem<strong>en</strong>t of the ferrite precipitation in the alloystreated under static magnetic field.Figure 151: SEM micrographs showing the structure after waterqu<strong>en</strong>ching under 0 and 16 T for the Fe-0.2C-1.5Mn (a) and forFe-0.3C-1.5Mn (b)(wt%). Original magnification 4000x, 4% nitaletching sample.F. DebrayT. Garcin, S. Rivoirard, R. Morgunov, E. Beaugnon, (CRETA, CNRS, Gr<strong>en</strong>oble, France)107


MAGNETO-SCIENCE 2009Study of the influ<strong>en</strong>ce of magnetic forces on the mass transferof paramagnetic particles in electrochemistryThe context of our work is the characterization of the magneticforces which influ<strong>en</strong>ce the processes of mass transferin electrochemistry. It appears experim<strong>en</strong>tally that in thepres<strong>en</strong>ce of a magnetic field in solutions, where a gradi<strong>en</strong>tof conc<strong>en</strong>tration of paramagnetic ions is pres<strong>en</strong>t, ev<strong>en</strong> if theaction of Lor<strong>en</strong>tz forces is not effective, a driving force actingon the solution will arise. This force, referred to as theconc<strong>en</strong>tration gradi<strong>en</strong>t force, is oft<strong>en</strong> writt<strong>en</strong>,−→ B 2−→ ∇CF m = χ m , (18)2µ 0where χ m (m 3 /mol) is the molar magnetic susceptibility,B(T) the magnetic flux d<strong>en</strong>sity, C(mol/m 3 ) the bath conc<strong>en</strong>trationand µ 0 (Hm −1 ) the permeability of vacuum. Theexperim<strong>en</strong>t was performed using a 10 MW resistive magnetwhich g<strong>en</strong>erates a homog<strong>en</strong>eous a magnetic field of 6 T ina 286 mm diameter. The experim<strong>en</strong>tal device is a rectangularchannel with platinum electro<strong>des</strong> on the upper and lowerwalls, betwe<strong>en</strong> which a voltage drop is applied (figure 152).The channel is closed with insulating walls to eliminate theedge effects. The cell is immersed in an electrolytic bathprepared with an equimolar solution of 0.05 mol/m 3 Ferriferro-cyanide with 0.5 mol/m 3 and K 2 SO 4 as the supportingelectrolyte. The temperature condition was about 17 ◦ Cand an Ag/AgCl refer<strong>en</strong>ce electrode was used to control theelectro<strong>des</strong> pot<strong>en</strong>tial.of the boundary layer. As a result, an additional mechanismof transport of the solution is g<strong>en</strong>erated. Correspondingly,the limiting curr<strong>en</strong>ts of reactions proceeding in the electrochemicalsystem will become a function of the appliedmagnetic flux d<strong>en</strong>sity. The influ<strong>en</strong>ce of magnetic field onthe evolution of the mean limiting curr<strong>en</strong>t d<strong>en</strong>sity is plottedusing logarithmic coordinates in figure 153. We can showsthat for the two mo<strong>des</strong>, anodic and cathodic, the limitingcurr<strong>en</strong>t d<strong>en</strong>sity follows a law in B 2/3 . Note that this lawstarts at 0.5 T for the anodic mode and at 2 T for the cathodicmode due to the paramagnetic forces which drivesa more important flow than the gravity. This ph<strong>en</strong>om<strong>en</strong>ologicalbehaviour was observed by many authors [Waskaas,Acta Chimica 50, 516 (1996)], Rabahand et al., Journal ofElectroanalytical Chemistry 571, 85 (2004)].Figure 152:Experim<strong>en</strong>tal configuration.The results were obtained by the polarographic method.Wh<strong>en</strong> the two electro<strong>des</strong> located on the faces of the channelare submitted to a voltage drop, controlled by a pot<strong>en</strong>tiostat,an electric curr<strong>en</strong>t is imposed and in the pres<strong>en</strong>ce ofan homog<strong>en</strong>eous magnetic field, the gradi<strong>en</strong>t of paramagneticions due to electrode reaction will cause a redistributionof velocities in the bath which th<strong>en</strong> acts on the depthFigure 153: Evolution of the limiting curr<strong>en</strong>t d<strong>en</strong>sities with thework electrode (WE) in the (a) cathodic mode and (b) anodicmode.F. DebrayD. Baaziz, A. Alemany, (EPM-SIMAP Laboratory, Gr<strong>en</strong>oble, France), D. Kalache (Fluids Mechanics Laboratory,University of USTHB, Algiers)108


2009 MAGNETO-SCIENCELarge Alfvén Waves in liquid sodiumAlfvén waves are hydromagnetic waves involving fluid velocityand magnetic field. They are a key ph<strong>en</strong>om<strong>en</strong>onin many geophysical and astrophysical area, such as theEarth’s liquid core, the magnetosphere, solar wind and interstellarplasma dynamics. They are difficult to observe inexperim<strong>en</strong>ts but it would be useful to reach a state of interactingAlfvén waves as a key example of weak turbul<strong>en</strong>ce.Here, we use liquid sodium (figure 154). Compared togalinstan (gallium/indium/tin liquid metal alloy) it is a betterelectrical conductor (ohmic dissipation of Alfvén wavesis reduced) and its d<strong>en</strong>sity is much less (h<strong>en</strong>ce Alfvénwaves are faster). The geometry of the liquid sodium cavityis a cylinder of diameter 10 cm and of l<strong>en</strong>gth 20 cm.This was inserted in an available diameter of 16 cm witha maximum value of 16 T. 7 coils are placed around thiscylinder at regular intervals along the l<strong>en</strong>gth. In addition, aso-called ‘emission’ coil is placed at one <strong>en</strong>d of the cylinderto provide a magnetic excitation of Alfvén waves. This is ashort electrical pulse curr<strong>en</strong>t producing a poloïdal magneticfield. The Alfvén wave can th<strong>en</strong> be observed on the signalof the 7 measuring coils. The characteristic dim<strong>en</strong>sionlessLundquist number (propagation time divided by dissipationtime) changed from a maximum of 60 with galinstanto around 500 with liquid sodium. H<strong>en</strong>ce we expect to observeAlfvén waves very clearly. In figure 155, the arrivalof an Alfvén wave is recorded at the <strong>en</strong>d of the cylindricalcavity, while it was produced at the other <strong>en</strong>d by a pulsein a coil. On the left-hand side, one can see the electricalpulse (black curve) followed by the arrival of a main oscillationwith a shorter delay wh<strong>en</strong> the applied B is stronger,according to the Alfvén propagation time. On the righthandside, time is made dim<strong>en</strong>sionless using the theoreticaltime of propagation of an Alfvén wave from one <strong>en</strong>d of thecylinder to the other: all arrivals collapse around a dim<strong>en</strong>sionlesstime of unity. In figure 156, the 7 measured signalsare shown. It is possible to follow the signal from the <strong>en</strong>dwhere it was created to the other <strong>en</strong>d. There is however anadditional compon<strong>en</strong>t to the signal which is the signatureof structural vibrations. The linearity of the response signal(figure 157) shows however that the excitation is not yetlarge <strong>en</strong>ough to reach a turbul<strong>en</strong>t state.Figure 155: Propagation of an Alfvén wave recorded on the coilfarthest from the ‘emission’ coil for differ<strong>en</strong>t int<strong>en</strong>sities of magneticfield. Same plot using the dim<strong>en</strong>sionless time scale based ontheoretical Alfvén speed.Figure 156:a pulse.The 7 signals of the 7 coils are plotted together, afterFigure 154: These photographs show the process of filling thecontainer with sodium, the bare setup and finally the setup withinits thermal insulator equipped with pressure and temperature s<strong>en</strong>sors.Figure 157: Linear response of electromotive force with respectto the int<strong>en</strong>sity of the excitation pulse. Energy losses during reflections.F. DebrayTh. Alboussiere, P. Cardin, P. La Rizza, J.P. Masson, H.C. Nataf, F. Plunian, N. Schaeffer, D. Schmitt(LGIT/CNRS/OSUG/UJF, Gr<strong>en</strong>oble)109


MAGNETO-SCIENCE 2009Magnetohydrodynamic effect on electrodeposition of nickel alloys-catalysts forhydrog<strong>en</strong> evolutionElectrodeposition is strongly affected by the addition ofnivellant ag<strong>en</strong>ts or bright<strong>en</strong>ers in the electrolytic bath.Many electroactive species can be used to modify the characteristicsof the deposits. However, the pres<strong>en</strong>ce of organiccompounds in the baths gives alloys whose properties withrespect to the corrosion resistance are degraded considerably[Meguro et al. J. Electroch. Soc. 147 3003 (2000)].The magnetic forces g<strong>en</strong>erated by the passage of a curr<strong>en</strong>tin the pres<strong>en</strong>ce of a magnetic field create additional convectionwhich affect the morphology of the deposits.field influ<strong>en</strong>ces deposition by g<strong>en</strong>eration of additional convectionclose to the electrode surface and by reduction ofthickness of diffusion layer near cathode surface.In theory, the size of the grain of the deposits is a functionof the speed of nucleation and growth of the nucleus;the more numerous nucleuses are, the lower is the grainsize. A magnetic field applied parallel to the surface of theelectrode g<strong>en</strong>erates convection (magnetohydrodynamic effector MHD) of the electrolyte; it results in a laminar flowon the surface of the electrode which reduces the diffusionlayer and increases the conc<strong>en</strong>tration gradi<strong>en</strong>t. This resultsin change in the size of the grains. In principle, the grainsize is a function of the nucleation rate and the growth ofthe nuclei: the more the nuclei the smaller is the resultinggrain size.The influ<strong>en</strong>ces of magnetic field on composition, structureand morphology of Cu-Ni alloys have be<strong>en</strong> investigated.The XRD diffraction pattern of deposited alloys ispres<strong>en</strong>ted in figure 158. Alloys show a fcc structure ofCu 0 .81Ni 0 .19. There is no differ<strong>en</strong>ce in the alloy structurewith increasing applied magnetic field while the grainsize of Cu-Ni deposit decreases. This could be explainedby the g<strong>en</strong>eration of additional convection close to the electro<strong>des</strong>urface by the MHD effect. At the same time th<strong>en</strong>ickel cont<strong>en</strong>t of the alloy is increased with increasing appliedmagnetic field. This could be explained by magneticfield action on the hydrog<strong>en</strong> evolution. Nickel electrodepositionis always accompanied by viol<strong>en</strong>t hydrog<strong>en</strong> evolution.Wh<strong>en</strong> a magnetic field is applied the size of hydrog<strong>en</strong>bubbles is smaller and they are more rapidly removed fromsurface of the electrode. In this way the nickel partial curr<strong>en</strong>teffici<strong>en</strong>cy is increased and nickel cont<strong>en</strong>t of the alloy ishigher. The magnetic field also influ<strong>en</strong>ces the morphologyof Cu-Ni alloys. Hydrog<strong>en</strong> evolution <strong>en</strong>hanced by the appliedmagnetic field leads to a smooth surface of the alloys(figure 159). However, this effect is visible only for appliedmagnetic field of 6 T or more.In conclusion, a magnetic field changes the morphologyand grain size of deposited alloys. There is no influ<strong>en</strong>ceof applied magnetic field on structure of deposit. MagneticFigure 158: XRD diffraction pattern of Cu-Ni alloys depositedwith superimposed magnetic field parallel to the surface of electrode.Figure 159: Morphology of Cu-Ni alloys deposited with superimposedmagnetic field parallel to the surface of electrode.F. DebrayP. Zabinski, R. Kowalik, A. Jarek (AGH University of Sci<strong>en</strong>ce and Technology, Krakow, Poland)110


2009 MAGNETO-SCIENCEDiffusion behavior of Al/Cu diffusion interface under a high magnetic fieldThis work has investigated the effect of a 16 T magneticfield on the diffusion behavior of the Al/Cu diffusion interface.Figure 160 shows that the interface morphology ofthe Al/Cu diffusion couple heated to 615 ◦ C and held for5 hours, and th<strong>en</strong> solidified with and without a 16T magneticfield. It can be observed that the surface of the samplefabricated in the case of no magnetic field [figure 160(a)] isirregular. This may be attributed to formation of Marangoniconvection so that natural flow has forced the liquid out ofthe Cu crucible. Wh<strong>en</strong> a 16 T magnetic field is applied, aregular surface forms which can be attributed to the dampingof the Marangoni convection and natural flow.Figure 161 shows micrographs and aluminum conc<strong>en</strong>trationprofiles obtained by measuring the cont<strong>en</strong>t of Al atdiffer<strong>en</strong>t positions as a function the distance from the copperside to the aluminum side of the intermediate layers atthe Cu/Al diffusion interface fabricated with and without a16 T magnetic field. The Cu/Al interface consists of fourintermediate layers with a thin irregular edge and three flatlayers. The conc<strong>en</strong>tration profiles indicate that the compositionof every layer is constant. This is consist<strong>en</strong>t with thephase diagram (according to the phase diagram and EPMAanalysis, the intermediate layers are Cu 3 Al 2 (δ), Cu 12 Al 9(ξ2), CuAl (η2) and CuAl 2 (θ), respectively).In addition, wh<strong>en</strong> the sample is placed in a magnetic field,it will become magnetized. For the materials with differ<strong>en</strong>tmagnetic property, the magnetization is differ<strong>en</strong>t; for theAl/Cu diffusion interface fabricated under high magneticfield, the magnetization of the Cu and Al is differ<strong>en</strong>t. As aconsequ<strong>en</strong>ce, a gradi<strong>en</strong>t of the magnetic field is formed andthe magnetic force is produced at the interface betwe<strong>en</strong> theCu and Al. This force may retard the diffusion of the Alatom to the Cu crucible and cause a change in the shape ofthe liquid interface (forms a convex surface).Figure 160: Effect of a 16 T magnetic field on the diffusion andthe formation of microstructure in the Aluminum/Copper diffusioncouple heated to 615 ◦ C and held for 5 hours, and th<strong>en</strong> solidified(a) with B = 0 T and (b) with B = 16 T.This shows that an application of a high magnetic field hasnot affected the phase composition of the diffusion layers;however, the magnetic field has decreased the depth of thediffusion layers suggesting that the magnetic field has retardedthe diffusion. This may be attributed mainly to twoeffects of the magnetic field. Firstly, the damping of theconvection and secondly, the formation of a magnetic force.It is well known that magnetic field damps the flow and undera 16 T magnetic field, the convection may be dampedtotally. The effect of the flow on the diffusion has be<strong>en</strong>widely investigated and it is g<strong>en</strong>erally accepted that flow<strong>en</strong>hances the diffusion. Thus, wh<strong>en</strong> a high magnetic fieldis applied during the diffusion process, the diffusion will beretarded owing to the damping of the convection, resultingin a decrease of the depth of the intermediate layers.Figure 161: Micrograph of the intermediate layers in the Al/Cudiffusion couple heated to 700 ◦ C and held for 0.5 hours and th<strong>en</strong>solidified with and without a magnetic field of B = 16 T as indicated.F. DebrayY. Fautrelle (SIMAP, EPM, CNRS, Gr<strong>en</strong>oble), X. Li (University of Shanghai, Shanghai)111


MAGNETO-SCIENCE 2009112


2009Magnet Developm<strong>en</strong>t and Instrum<strong>en</strong>tation113


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONHigh field helix developm<strong>en</strong>tThe highest continuous magnetic fields at LNCMI are obtainedusing helix inserts surrounded by large Bitter coils.The 14 helix insert was made available on a regular basisto researchers in September 2006 and g<strong>en</strong>erates 32 T in a34 mm diameter bore. An upgraded version was developedand tested successfully in July 2007 at 34 T. A new versionwas constructed and tested at 35 T in March 2009. Aftertwo weeks of running we <strong>en</strong>countered an anomalous heatingof helices 9 and 10. This was proved to be related witha material imperfection (small cracks)on one of the helicesduring the production process. As a consequ<strong>en</strong>ce, the 34 Tinsert was again into operation until the normal summerstop of the high field facility (<strong>en</strong>d July). The 35 T insertwas reinstalled in September and has since be<strong>en</strong> used undersevere NMR running conditions (continuous high fields formany hours) without problem (figure 162).In parallel we have <strong>des</strong>igned and constructed two new50 mm inserts, one is a 12 helix insert directly derived fromthe 14 helix insert and the other is a first attempt to combinea c<strong>en</strong>tral radially cooled helix (cooling betwe<strong>en</strong> thepitches with a set of 9 longitudinally cooled helices (coolingwithin the annular spacing betwe<strong>en</strong> adjac<strong>en</strong>t helices).Both versions should produce magnetic fields in excess of31 T. One of the two inserts will be in operation in 2010,the second one in 2011. The priority will be defined in thefirst quarter of 2010 dep<strong>en</strong>ding on the results of the tests ona dedicated 40 bar hydraulic loop.The performances of the 35 T magnet are summarized intable 1. The insert produce 25 T in a very compact manner(outer copper radius of 186 mm. The power is 11.5 MWfor an inlet water temperature of 14 ◦ C. An insert capable of26 T with the same power (with some loss of homog<strong>en</strong>eity)has be<strong>en</strong> optimized by changing only the 4 innermost helices.It will be tested dep<strong>en</strong>ding on the high field facilityplanning during 2010. The surrounding two Bitter stacksproduce an additional 10 T with a power of 10 MW forthe same inlet temperature of 14 ◦ C. This value correspondsroughly to a mean condition over the year for inlet temperature(from 10 ◦ to 20 ◦ ) dep<strong>en</strong>ding on the season and onthe type of experim<strong>en</strong>ts (“sweepers” or “sitters”). Consequ<strong>en</strong>tlythe power at a giv<strong>en</strong> magnetic field can be = ±5%dep<strong>en</strong>ding on both the period over the year and the type ofexperim<strong>en</strong>ts. A common work program is underway in thelaboratory to optimize the cost of such high field experim<strong>en</strong>ts.InsertoutsertType of coil 14 helices 2 Bitter StacksInner radius (mm) 19.3 200Outer radius (mm) 186 500Power (MW) 11.6 10.2Inlet temperature ◦ C 14 14Electric curr<strong>en</strong>t (A) 29835 29835Field contribution (T) 25.14 9.86Table 1: Main specifications of the 35 T magnet.Figure 162: A cut through view of a 14 helix insert. The warmbore available for users is 34 mm.C. Auternaud, F. Debray, J. Dumas, M. Kamke, J. Matera, C. Mollard, R. Pfister, B. Pardo, D. Ponton, J. Spitznagel,C. Trophime, E. Verney, N. Vidal, S. VeysJ.M Tudela (SERAS, CNRS, Gr<strong>en</strong>oble)115


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009Magnets for neutron and x-ray scattering and absorption experim<strong>en</strong>tsThe maximum magnetic field available today in a split configurationis 15 T (at ILL, HZB in Berlin, Spring 8 inOsaka and few other places). The magnet conception isbased on Nb 3 Sn superconducting cable technology. Forhorizontal field configuration without specific radial access,commercial superconducting sol<strong>en</strong>oids are availableup to 20 − 22 T. The European Synchrotron Radiation Facility(ESRF), and the Institut Laue Langevin neutron facility(ILL) int<strong>en</strong>d to put into operation high field magnetsadapted for neutron scattering, x-ray scattering and x-rayabsorption experim<strong>en</strong>ts. During 2008 a <strong>des</strong>ign study forthe implem<strong>en</strong>tation of dc high magnetic fields was led byESRF and ILL in collaboration with the LNCMI. The studyaddresses the three critical technical aspects of the project:the cooling and electrical power capacities of the Gr<strong>en</strong>oblesite, and the magnet <strong>des</strong>igns. Magnet <strong>des</strong>igns were based onthe availability of a power of 35 MW in the magnet. Twomain <strong>des</strong>igns have be<strong>en</strong> considered:1 - A horizontal field magnet suitable for back scatteringand absorption experim<strong>en</strong>ts. The <strong>des</strong>ign is derived from the35 T in 34 mm vertical field magnet in operation at LNCMI.The more compact <strong>des</strong>ign has an outer diameter of copperless than 400 mm and gives a magnetic field of 31 T in a34 mm for a power of 22 MW and an inlet temperature of20 ◦ C. It uses exclusively a set of 14 helices powered by acurr<strong>en</strong>t of 36000 amperes. The second version (figure 163)uses in addition a stack of outer Bitter plates. Each of thetwo magnets are supplied by a curr<strong>en</strong>t of 36000 amperes,the total power reaching 33 to 35 MW for 40 T. Further optimizationwill be carried out on the Bitter stack to optimizethis value.2 - A split magnet <strong>des</strong>ign. In this configuration, the effici<strong>en</strong>theat transfer required for split magnets is obtained usingradial channels arranged betwe<strong>en</strong> the magnet turns. Consequ<strong>en</strong>tly,the innermost windings are better cooled thanwh<strong>en</strong> using traditional longitudinally cooled windings. Additionally,the main cooling water flow is parallel to themid-plane and offers a larger flexibility for the <strong>des</strong>ign ofthe mechanical devices necessary to withstand the attractingforces existing betwe<strong>en</strong> the two halves of the magnet.Each magnet half is made of 4 helices arranged conc<strong>en</strong>trically.The outer diameter of the outer helices is smallerthan 400 mm. Using this <strong>des</strong>ign it was possible to optimizea magnet that could reach 30 T in a split configuration.Classical Colburn type correlation can be used for thethermo-hydraulic modeling to determine the heat transfercoeffici<strong>en</strong>ts <strong>des</strong>pite the fact that the hydraulic diameter ofthese channels are of the order of 0.15 to 0.6 mm. The mainmodeling effort has focused on withstanding the attractingforces betwe<strong>en</strong> the two halves of the magnet. The maximumadmissible primary total stress in a normal duty situationis 880 MPa. Calculations show that the sector shapesolution for split magnet assembling that leaves a 10 mmair gap with an associated 2 × 3 ◦ take off angle, would sustainthe attractive force betwe<strong>en</strong> the two half magnets up toa field of 28.8 T with 7 port accesses of 36 ◦ . Higher gapand or higher port angle could be obtained to satisfy userneeds by changing the contact part thickness resulting in adecrease of B and of the attracting forces. For neutrons,the ports are replaced by four aluminum rings. The symmetryof this structure allows to reach a higher field, 30 T,for the same primary total stress. Critical issues of the <strong>des</strong>ignsuch has high curr<strong>en</strong>t d<strong>en</strong>sities on the inner windingswere studied by mean of the construction and test of prototypes.Electromagnetic and thermo-mechanical numericalsimulations were conducted in order to propose mechanical<strong>des</strong>igns capable of holding the attractive forces betwe<strong>en</strong> thetwo halves of the split magnet.To reinforce and secure these ambitious <strong>des</strong>igns, complem<strong>en</strong>taryhydraulic and electromagnetic studies will be performedat the LNCMI during the period 2010 to 2012within a new partnership with the ESRF and the ILL in theframe of the EMFL FP7 program.Figure 163: A 40 T horizontal magnet with a conical access atleast equal to 2×10 ◦ . The warm bore available for users is 34 mm.F. Debray, J. Dumas, S. Labbe-Lavigne, R. Pfister, C. Trophime, N. VidalJ. Giraud (LPSC, CNRS, Gr<strong>en</strong>oble), F. Wilhelm (European Synchrotron Radiation Facility, Gr<strong>en</strong>oble), M. Enderle(Institut Laue Langevin, Gr<strong>en</strong>oble)116


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONA new cooling loop for thermo-hydraulic magnet studiesHeat fluxes <strong>en</strong>countered in high field magnets can be ashigh as 500 W/cm 2 with submillimetric cooling channels.Consequ<strong>en</strong>tly, heat transfers are, together with the materials,a key issue for magnet optimization.The LNCMI has a long term collaboration with the <strong>Laboratoire</strong><strong>des</strong> Ecoulem<strong>en</strong>ts Geophysiques et Industriels (LEGI,CNRS INPG). Most of the experim<strong>en</strong>ts performed were todetermine either the threshold of cavitation in the coolingchannel or the heat transfer coeffici<strong>en</strong>t in a well defined geometry[Reynaud et al., Int. Journal of heat and mass transfer,48, 3197,(2005)]. Nevertheless, the hydraulic coolingloop was limited with a maximum pressure loss of 13 barswhich is roughly half of the pressure loss through our highfield magnets. In addition, high heat fluxes could not bereached on the test section.In 2008 and 2009, LNCMI and LEGI in the frame of theircollaboration have upgraded an existing 40 bars hydrauliccooling loop to study high field magnet thermo-hydraulics.The hydraulic cooling loop (photograph in figure 164) isnow operational for two main kinds of experim<strong>en</strong>ts. One isthe continuation of the precise modelling of heat transfer ina single flat thin channel. Figure 165 shows the related testsession that is now under construction for this purpose. Itis forese<strong>en</strong> to hold a pressure of 40 bars and to characterizethe heat transfer with a velocity up to 40 m/s and heattransfer of at least 100 W/cm 2 , with a variable width of thechannel from 0.2 to 1 mm.Figure 164:assembly.View of the 40 bar hydraulic cooling loop underThanks to the high hydraulic power available on the newhydraulic cooling loop (80 KW instead of 2 KW for the oldhydraulic cooling loop) it is now possible to study directlythe thermo-hydraulics of an <strong>en</strong>tire coil or a group of criticalcoils (helix or Bitter) up to a flow rate of 15 l/s. Thefirst study will concern the flow distribution of the radiallycooled helix that will be used at the c<strong>en</strong>ter of the new highfield 50 mm, 31 T magnet. Consequ<strong>en</strong>tly, an aluminiummodel has be<strong>en</strong> prepared and will be tested at the <strong>en</strong>d of theyear 2009 and it will help to detect possible weak pointsin the very constrained hydraulic <strong>des</strong>ign without using thehigh field facility for this purpose.This work has be<strong>en</strong> partially supported by the ESRF upgradeprogramm and is supported now by the EuromagnetII FP7 program. In this context an <strong>en</strong>gineer, B. Pardo,has be<strong>en</strong> hired in October 2009 and will focus on thermohydraulicmodelling and comparisons with experim<strong>en</strong>taldata. The main goal of this study is to establish a numericalmodel of the radially cooled helix in order to optimizethe geometry of cooling channels. The work will permit to<strong>en</strong>hance the thermo-hydraulics performance of the magnet.Figure 165: A exploded view of the new hydraulic test section tomodel the heat transfers in one channel. Heat flux will be higherthan 100 W/cm, velocity up to 40 m/s and the thickness of thechannel can be changed without dismantling the apparatus. Itis expected to be operational mid 2010. Water flows from leftto right, the thickness of the channel can be varied from 0.2 to0.6 mm. The heaters are located in the red block equipped with aflat heat flux s<strong>en</strong>sor.C. Auternaud, F. Debray, J.Dumas, M. Kamke, J. Matera, R. Pfister, B. Pardo, C. Trophime, E. Verney, N. VidalM. Deleglise (SERAS, CNRS, Gr<strong>en</strong>oble), JP Franc and M. Riondet (LEGI CNRS, INP, UJF, Gr<strong>en</strong>oble)117


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009Pulsed <strong>en</strong>ergy supplyThe 14 MJ capacitor bankThe 14 MJ capacitor bank (see figure 166) has functionedwithout any major problems. The financial contributionby the European Union based on the number of performedpulses requires a stricter accounting system for the use ofthe g<strong>en</strong>erator. A simple logging system was already inoperation. The arrival of Jean-Pierre Nicolin, a professionalinformatics <strong>en</strong>gineer, permitted us to implem<strong>en</strong>t afull-featured database containing coils, users, pulses andother relevant data. He developed a system that inclu<strong>des</strong>controlled access based on a password. Implem<strong>en</strong>ting thisin the Siem<strong>en</strong>s Step7 software was possible but not straightforward,nevertheless, one can now load the user-rights andpassword via a file containing all the accepted proposals.use with the old control unit for the 150 kJ bank. The useof this c<strong>en</strong>tral unit severely limits the versatility of the 1 MJbank since it can only be used at a repetition rate of 1 (full<strong>en</strong>ergy) pulse every 20 minutes and the commutation optionis not operational. Due to the professional informaticssupport we were able to greatly improve and stabilize thesoftware interface betwe<strong>en</strong> the old (150 kJ) c<strong>en</strong>tral moduleand the outside world (direct user interface or controlvia the ESRF “SPEC” system). An interface with the samelook and feel (but partly based on differ<strong>en</strong>t hardware) isnow being writt<strong>en</strong> for the new (1 MJ) c<strong>en</strong>tral module. Theassembly of the c<strong>en</strong>tral module is reaching completion, butdue to unforese<strong>en</strong> long delivery times of the optically firedthyristors (a delay of 1 year to get a viable offer with a deliverytime of 40 weeks!) we will be obliged to cannibalizethe 150 kJ unit (i.e. the thyristor stack of the 150 kJ unitwill be dismounted and temporarily used in the 1 MJ unit).The final test of the c<strong>en</strong>tral (charging) unit is forese<strong>en</strong> forJanuary 2010.Figure 166:basem<strong>en</strong>t.A view of the 14 MJ, 24 kV, 65 kA g<strong>en</strong>erator in theFigure 167: The developed in-house, rapid commutation switch,for changing automatically the polarity of the field.The construction of a 1 MJ transportable capacitorbankDriv<strong>en</strong> by the success and the frequ<strong>en</strong>t use of the transportable150 kJ bank (ILL, ESRF) we decided to build a1 MJ capacitor bank. This new unit is not only a higher<strong>en</strong>ergy version of the 150 kJ g<strong>en</strong>erator but it has two ess<strong>en</strong>tialmodifications. First of all it will have the possibilityto work with two polarities, and secondly the chargingand the commutation (see figure 167) will take only a fewminutes and will be controlled completely by a computerintegrated in the c<strong>en</strong>tral charging unit. For budgetary reasonsit was decided to first build the two storage modulessince they could in principle be <strong>en</strong>ergized by the existingcharger unit (at the exp<strong>en</strong>se of a long charging time). Sincethe first quarter of 2009 the two capacitor modules are inOutlookThe most important and urg<strong>en</strong>t investm<strong>en</strong>t is a moderatelysized (∼ 6 MJ) capacitor bank with a short pulse. Thisequipm<strong>en</strong>t will permit us to <strong>en</strong>ergize coils in the 80 T rangewithout making compromises in the <strong>des</strong>ign. It is forese<strong>en</strong>that the installation will be built as two completely indep<strong>en</strong>d<strong>en</strong>t3 MJ units. Each unit will consist of a mediumsize container. The use of containers has two advantages: ifrequired one can use more than 1 MJ at remote sites (ILL,ESRF, etc.) and secondly the delivery and use of the 6 MJg<strong>en</strong>erator can start before the ext<strong>en</strong>sion of the building hasbe<strong>en</strong> finalized. The forese<strong>en</strong> use of several g<strong>en</strong>erators imposesa review and a profound modification of the groundingstrategy. This long due modification needs to be finalizedin 2010.P. Frings, B. Griffe, J.-P. Nicolin, T. Schiavo118


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONPulsed high-field coilsThe production of user coilsAlso in 2009 the copper-zylon coils remain the workhorseof the laboratory. The production of these coils has nowbecome standard; parts are parameterized and can be producedin 2 weeks on the computerized milling machine,the actual winding takes less than a week and testing a fewdays. Since most of the time parts are in stock and at least4 members of the team have the experi<strong>en</strong>ce to wind a coil,a standard coil can be produced in 10 days. Moreover, thepolicy is to have at least one standard coil in stock, in orderto avoid as far as possible any delay for users after a(finally unavoidable) coil failure. A first glidcop zylon coilwas tested up to 72 T and is now available for users duringthe time the 1 MJ transportable g<strong>en</strong>erator is available.Giv<strong>en</strong> the success of this small-volume, short-pulse prototype,we have constructed a longer pulse (t max = 33 ms,t total = 200 ms ) 72 T coil which can be <strong>en</strong>ergized by the14 MJ g<strong>en</strong>erator. This magnet has be<strong>en</strong> successfully testedand is now available to users on a perman<strong>en</strong>t basis.Figure 168:XXL coilSpecial coilsIn 2009 a special coil for optical experim<strong>en</strong>ts (BMV) wasdeveloped and successfully tested in house and to the highestfield at our colleagues in Dresd<strong>en</strong>. This coil (nicknamedXXL - see figure 168) is an up-scaled version of the X-coil. This coil produced 300 T 2 .m and is an improvem<strong>en</strong>tof 1100% compared to the former X-coils. The split coil,specially <strong>des</strong>igned for synchrotron X-ray experim<strong>en</strong>ts, wasfinally tested inside its cryostat after some problems due tothe complicated integration of the coil-body with the liquidnitrog<strong>en</strong> cryostat. Last, but not least, a mini-coil madefrom Cu-stainless wire was produced by Jérome Béard andhe was able to break with this coil (used as an insert in astandard 60 T coil) the record field of the Toulouse laboratorythat now stands at 81 T. This test was partly made tovalidate our multi-coil <strong>des</strong>ign code that was used to <strong>des</strong>igna large two-coil magnet (ARMS4).Technical developm<strong>en</strong>tsMost of the time in coil winding is sp<strong>en</strong>t on applying thezylon reinforcem<strong>en</strong>t, therefore we decided to improve thezylon spinhead by making it more reliable (new frictionbrakes) and easier to maintain (the spinhead modules canbe exchanged in 2 minutes, to be cleaned and maintained).Since the main progress in coil performance has to comefrom progress in materials it is of utmost importance tostudy the materials used in coil construction under realisticconditions (cryog<strong>en</strong>ic temperature and high mechanicalloads). To test the effici<strong>en</strong>cy of the fibre reinforcem<strong>en</strong>t wedecided to continue the explo-vessel studies (as first developedin at the Universiteit van Amsterdam). Unfortunatelyonce the setup was running (using the high-pressure rig atthe Clar<strong>en</strong>don Laboratory in Oxford) and 30 pressure vesselshad be<strong>en</strong> produced, it turned out that this installationwas not longer available to us due to changing priorities inOxford. Another high-pressure rig was id<strong>en</strong>tified in Franceand we expect to restart the explo-vessel tests before the<strong>en</strong>d of the year. These tests will be used to determine forthe first time the properties of zylon reinforcem<strong>en</strong>t underrealistic conditions, study the influ<strong>en</strong>ce of various impregnatesand impregnation methods, and last but not least toinvestigate other high-str<strong>en</strong>gth fibres that could be used as afall back solution in case zylon would not be available anymore.Apart from the mechanical str<strong>en</strong>gth of the conductorand the fibre reinforcem<strong>en</strong>t the quality of the isolation underhigh mechanical load at cryog<strong>en</strong>ic temperature is of greatimportance to have coils with a long lifetime. In order totest various types of insulations we developed an isolationtest on wires applying realistic loads to the isolation. Thisinstallation has started to work and the first results will beavailable before the <strong>en</strong>d of the year.OutlookThe success of pulsed fields combined with large-scale neutronand X-ray sources has created a demand for more timeat high magnetic fields per 24 hour period. This will be realizedby improving the duty cycle of the coils by increasingthe pulse duration (to prolong lifetime) combined with a reductionof the cool down time. Some test with liquid nitrog<strong>en</strong>based on techniques used up to now in dc fields lookedvery promising (cool down times of only a few minutes). Itis likely that by implem<strong>en</strong>ting these techniques in our coilswe can gain at least a factor of t<strong>en</strong> in the duty cycle.J. Béard, J. Billette, P. Frings, F. Giquel , J.-M. Lagarrigue, J. Mauchain119


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009High str<strong>en</strong>gth conductors for pulsed magnetsR&D of high str<strong>en</strong>gth composite conductors- for B > 80 T in the coilin/coilex system: the developm<strong>en</strong>tof Cu/SS wires, for the coilin, with 60% of stainless steel(UTS(77 K)>1550 MPa) and a cross section of 2.00×1.25mm 2 allowed us to reach 81 Tesla (the LNCMI record) inspring 2009.- Cu alloys for magnets with optimized curr<strong>en</strong>t distribution:conductors made of copper alloys like GlidCop(CuAl 2 O 3 ) or CuAg (with low silver cont<strong>en</strong>t 0.08%) havebe<strong>en</strong> processed by industrial companies to be combinedwith Zylon fibers in the user’s magnet with optimized reinforcem<strong>en</strong>tdistribution.Ultra-high str<strong>en</strong>gth nanocomposite Cu/Nb conductorsThe developm<strong>en</strong>t of reinforced conductors, with high electricalconductivity and high str<strong>en</strong>gth, is ess<strong>en</strong>tial to provid<strong>en</strong>on-<strong>des</strong>tructive high pulsed magnetic fields over 80 Tesla:the best compromise is obtained with copper-based continuousnanofilam<strong>en</strong>tary wires (UTS = 2 GPa and ρ =0.6 µΩcm at 77 K). The fabrication process of thes<strong>en</strong>anocomposite wires is based on severe plastic deformation(SPD) applied by accumulative drawing and bundling,leading to a multi-scale copper matrix containing up toN = 85 4 (∼ 50×10 6 ) continuous and parallel niobium nanotubes[Vidal et al., Scripta Mat., 60, 171 (2009)].In 2007, the extrusion of the nanocomposite conductorshas be<strong>en</strong> stopped at the “C<strong>en</strong>tre de Recherche” of TRE-FIMETAUX because of its closure. We decided to pursueour developm<strong>en</strong>t in collaboration with the CEA/LTMEX inSaclay where a 575 tons extrusion press is available.Developm<strong>en</strong>t of a new co-axial CuNbCuNb nanocompositewiresA new nanocomposite structure has be<strong>en</strong> <strong>des</strong>igned with asuperposition of Nb and Cu nanotubes (figure 169). Weadded nanometric phases remembering that the extraordinarystr<strong>en</strong>gth<strong>en</strong>ing of the co-cylindrical structure is relatedto: (i) an increase of Cu-Nb interfaces surface acting asdislocations barriers; (ii) a rapid and controlled access tonanometre scale where size effect operates on the plasticitymechanisms; (iii) the contribution of an additional reinforcingphase: the Cu-f nanofibers embedded in the Nbnanotubes behave as whiskers with strong size dep<strong>en</strong>d<strong>en</strong>ce.A conductor containing 85 3 Nb nanowhiskers, Cu nanotubesand Nb nanotubes, embedded in a copper matrixhas be<strong>en</strong> obtained. This Cu/Nb/Cu/Nb system is thereforemore effici<strong>en</strong>t than Cu/Nb filam<strong>en</strong>tary and Cu/Nb/Cu cocylindricalsystems for high-str<strong>en</strong>gth applications in magnets(figure 170): it exhibits a controlled microstructureand an effici<strong>en</strong>t str<strong>en</strong>gth<strong>en</strong>ing in the nanocomposite zones,where size and also geometry play major roles.Figure 169: Co-axial conductors: (a) N = 85; (b) N = 85 3 .Figure 170: Ultimate t<strong>en</strong>sile str<strong>en</strong>gth of co-axial CuNbCuNb andco-cylindrical CuNbCu nanocomposite wires versus diameter.The improvem<strong>en</strong>t of the drawing conditions led us to applythe same procedure for the optimization of the extrusionconditions. In the framework of the NANOFILMAGproject, funded by the ANR and involving the PHYMAT,two CEA laboratories (DAPNIA, LTMEX), and an industrialpartner (Alstom/MSA), a program has be<strong>en</strong> defined tooptimize the extrusion conditions. The aim is the prev<strong>en</strong>tionof fractures during the extrusion step of the ADB processand the scale-up of the size of the nanocomposite billets.A Ph.D stud<strong>en</strong>t, J.B Dubois, is involved in the projectand shares his activity betwe<strong>en</strong> LNCMI and PHYMAT.In addition, in-situ neutron diffraction (POLDI-PSI) and exsitulaboratory x-ray diffraction experim<strong>en</strong>ts (PHYMAT-Poitiers, ESRF) have be<strong>en</strong> performed for differ<strong>en</strong>t heattreatm<strong>en</strong>ts to study the formation of the texture. Textureand microstructure in the copper after heat treatm<strong>en</strong>tspres<strong>en</strong>t radical differ<strong>en</strong>ces dep<strong>en</strong>ding on the size of the consideredcopper channels [to be published].F. Lecouturier, N. Ferreira, L. B<strong>en</strong>dichou, J.M. Lagarrigue, J.B. DuboisL. Thilly, P.O R<strong>en</strong>ault (PHYMAT, Poitiers, France), H. van Swyg<strong>en</strong>hov<strong>en</strong>, S. van Petegem (POLDI-Paul ScherrerInstitut, Switzerland), P. Olier (CEA-DEN-LTMEX, Saclay, France), C. Berriaud (CEA-IRFU-SACM, Saclay)120


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONMegagauss magnetic field g<strong>en</strong>erationThe year 2009 marks the first g<strong>en</strong>eration of a magneticfields in excess of 100 T at the Toulouse pulsed magnetfacility. The field has be<strong>en</strong> obtained with a Megagauss g<strong>en</strong>erator(1 Megagauss = 100 Tesla) making use of capacitordriv<strong>en</strong>single-turn coils to produce field pulses on a microsecondtimescale. The installation, originally developedat the Humboldt University in Berlin, betwe<strong>en</strong> 1993 and1997, has be<strong>en</strong> transferred to LNCMI-Toulouse in 2006.an improved cryostat permitting experim<strong>en</strong>ts at liquid-Hetemperature is underway.Prior to its recommissioning the g<strong>en</strong>erator has undergone amajor revision including the replacem<strong>en</strong>t of crucial compon<strong>en</strong>tsof the charge/discharge-circuit (60 kV charging supply,high-voltage switches) and the adaptation of remotecontroland security functions. In the second half of 2009the installation has be<strong>en</strong> tested at moderate charging voltagesof up to 35 kV with 80 % of the nominal capacitance(16 out of 20 capacitors available). These tests have giv<strong>en</strong>rise to the curr<strong>en</strong>t 100 T field record. The field trace isshown in figure together with a simple test measurem<strong>en</strong>t ofthe Faraday rotation in CdS sample.This technique for g<strong>en</strong>erating magnetic field is <strong>des</strong>tructive,in the s<strong>en</strong>se that the coil explo<strong>des</strong> outwards and has to bereplaced after each pulse. However, the setup can be surroundedby an absorbing material (wood) which retains coilfragm<strong>en</strong>ts, and notably prev<strong>en</strong>ts any fragm<strong>en</strong>ts bouncingback. This means that the sample, and cryostat are not <strong>des</strong>troyedduring the pulse. Replacing the coil is a simpleoperation which can be performed quickly, and without removingthe sample or cryostat. This makes this techniquesfor g<strong>en</strong>erating magnetic fields practical from the point ofview of the user since many field shots are possible per day.Indeed, operation is simpler than a classical nitrog<strong>en</strong> cooledpulsed magnet since it is not necessary to wait for the coilto cool after each shot. The price to pay however, is theextremely short pulse, with only around 1µs available fordata acquisition at the maximum of the pulse.Starting from January 2010 the g<strong>en</strong>erator will be operated atfull capacitance and initially with moderate charging voltagesnot exceeding 45 kV. This will permit the g<strong>en</strong>erationof fields in excess of 150 T with little or no risk of insulationfailure. At this point the g<strong>en</strong>erator will be used forfirst sci<strong>en</strong>tific experim<strong>en</strong>ts making use of an optical setupfor transmission measurem<strong>en</strong>ts in the mid-infrared rangethat has also be<strong>en</strong> installed in 2009. The construction ofFigure 171: (a) Magnetic field g<strong>en</strong>erated with a 12×12 mm 2 single-turncoil (inner diameter × axial l<strong>en</strong>gth) at a charging voltageof 35 kV. (b) Expanded view of the top of the magnetic field pulse.(c) Preliminary data of the Faraday rotation in a CdS sample todemonstrate the feasibility of the system for sci<strong>en</strong>tists.P.Y. Solane, F. Durantel, O. Portugall121


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009SEISM: A 60 GHz electron cyclotron resonance (ECR) ion source prototypeLinked to the EURISOL and EURO-ν projects (Designstudies for the second g<strong>en</strong>eration of exotic nuclei acceleratorand the future neutrino factory in Europe), the beta beamproject aims to use the β decay of radioactive ions to produc<strong>en</strong>eutrinos beams. Within the Beta Beam work package(WP4), the ECR task is dedicated to the <strong>des</strong>ign of advancedmagnetic structures to be used in the ECR ion source technology.LPSC has proposed to develop a high frequ<strong>en</strong>cy(60 GHz) pulsed ion source prototype for the beam preparation.A first ion source prototype was <strong>des</strong>igned, basedon a cusp magnetic structure using the polyhelix coil technologyand was named SEISM for Sixty gigahertz Electroncyclotron resonance Ion Source using Megawatt magnets.Here we report progress in the construction of the prototypeand preparation for the first magnetic field measurem<strong>en</strong>tsscheduled in beginning 2010. This work has be<strong>en</strong>carried in the framework of an existing collaboration betwe<strong>en</strong>LPSC and LNCMI.Simulations of the polyhelices have be<strong>en</strong> carried out to finalizethe <strong>des</strong>ign. The temperature field in a coil dep<strong>en</strong>dingon the cooling water flow and on the geometry of the coil insulatorshas be<strong>en</strong> investigated. The geometry and the numbersof insulators (glass fiber) to be positionned betwe<strong>en</strong>each turn of an helice has be<strong>en</strong> specified in order to minimizethe pressure drop, maximize surface cooling and tosustain the 30 tons compression without any copper deformationthat could lead to short-circuit.The maximum electrical power needed is about 6 MW. Awater flow rate of ∼ 30 l/s in the two sets of coils is necessary.Thus, the average coils temperature varies from 80 to180 ◦ C while the peak temperature locally reaches 330 ◦ C.In these conditions, the maximum hoop stress in the coilsis 280 MPa, far below the copper alloy limit of elasticity(360 MPa). At full curr<strong>en</strong>t, the two sets of coils repel eachother with a force of 300 kN. The CAD mechanical <strong>des</strong>ignof the magnetic structure, taking in account all these data,was performed at LPSC. Figure 172 repres<strong>en</strong>ts a cut viewof the source. All mechanical parts will be ready for assemblingin December 2009.Figure 173: On-site implantation scheme for the magnetic fieldmeasurem<strong>en</strong>t at half-int<strong>en</strong>sity. Hydraulic circuit is parallel to M5existing circuit, electrical cables are connected in series with M5magnet.Figure 172: (a) External CAD <strong>des</strong>ign of the ion source prototype,(b) internal view of the curr<strong>en</strong>t and deionized water courses.M5 site was chos<strong>en</strong> as a temporary implantation site for themagnetic field validation at half-curr<strong>en</strong>t. Wh<strong>en</strong> suppliedwith 15 kA, each set of helices (injection set and extractionset) consumes only 0.75 MW of power from the curr<strong>en</strong>tsupply unit. Due to impedance tuning, the prototypeshould be electrically connected in series with an existing10 MW magnet, using flexible power cables. Water flowsof 24 l/s and 22 l/s at a pressure of 20 bars are respectivelyrequired at the injection and extraction. M5 hydraulic circuitwas modified in August 2009 in order to derive about50 l/s from the 150 l/s flow and a parallel hydraulic circuit isnow being installed (figure 173). The incoming water flowwill be controlled with tuneable valves and ultrasonic flowmeters. Hall probes will be mounted on step motor jacks inorder to establish a precise magnetic field map (1mm step).The test b<strong>en</strong>ch is planned to be upgraded with a high voltageplatform and a 28 GHz radiofrequ<strong>en</strong>cy emitter to allowa first characterization of the plasma at the <strong>en</strong>d of year 2010.These activities will be funded within the EURO-ν program(2008 - 2010).C. Trophime, F. Debray, J. Dumas, J. Matera, R. Pfister, N. VidalM. Marie-Jeanne, L. Latrasse, T. Lamy, T. Thuillier, C. Fourel, J. Giraud (LPSC, Gr<strong>en</strong>oble, France)122


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONTowards developing a high T c superconducting magnetHigh critical temperature superconductors (HTS) op<strong>en</strong> extremelyinteresting perspectives for high field applicationssuch as high field magnets for NMR, SMES or physicalinvestigations [J. Schwartz et al., IEEE trans. on Appl. Superc.,18,pp. 70, (2008)]. The demand is high for 25, 30 andev<strong>en</strong> 50 T magnets and is beyond the possibilities offeredby low critical temperature superconductors, for exampleNb 3 Sn. The superconducting solutions for very high fieldsmeet the requirem<strong>en</strong>ts for sustainable developm<strong>en</strong>t.Rutherford cable. These data show that the wires withstandthe cabling process and that they are magnetically isotropic.It will be possible to test the HTS magnets in liquid/gascooling or conduction cooling.Rec<strong>en</strong>tly, the interest for Bi-2212 round wire has be<strong>en</strong> reinforcedfor high field applications [Sh<strong>en</strong> et al., Appl. Phys.Lett. 95, 152516, (2009)] These wires show very high performancein terms of critical curr<strong>en</strong>ts at ultra high fields,at least on short samples. The main issue with Bi-2212 remainsthe heat treatm<strong>en</strong>t, which should be very preciselycontrolled. The melting temperature plays a crucial part andshould be within a window of one or two degrees to obtainthe required highest critical curr<strong>en</strong>ts d<strong>en</strong>sities. Ev<strong>en</strong> morerec<strong>en</strong>tly, the second g<strong>en</strong>eration (2G) HTS conductors, theYBaCuO coated conductors, show also very exciting performancesin terms of curr<strong>en</strong>t capacities under very highfields whereas their mechanical properties are excell<strong>en</strong>t forthe IBAD route. The mechanical performance is of greatimportance for very high field magnets. Substantial advanceshave be<strong>en</strong> achieved with the 2G HTS and they hav<strong>en</strong>ow reached a stage, in terms of l<strong>en</strong>gths, where it is possibleto use them in real devices.Several laboratories in Gr<strong>en</strong>oble (IN, LNCMI, CRETA andG2Elab) have begun works on HTS magnets. IN andG2Elab have built and successfully tested an importantHTS magnet (800 kJ) operating at 20 K in the context of aDGA project. The pres<strong>en</strong>t works are carried out in the contextof a European Project ”EuCARD” and an ANR project”SUPER-SMES”. The purpose is to study the most suitableHTS materials and develop the technology for veryhigh field and high performance HTS magnets for SMES(storage) or high <strong>en</strong>ergy physics (magnets for accelerators)purposes. An id<strong>en</strong>tified issue with HTS magnets is theirprotection and studies have begun both from simulation andexperim<strong>en</strong>tal points of view. In the developm<strong>en</strong>t program,the critical characteristics remain the fundam<strong>en</strong>tal data required.Advanced characterization tools have be<strong>en</strong> developed,in particular to obtain the critical characteristic underhigh fields at variable temperatures and variable field ori<strong>en</strong>tations.After delicate adjustm<strong>en</strong>ts, the system works perfectly.Figure 174 shows the sample holder and the newcryostat under construction to test HTS coils at variabletemperatures in two LNCMI high field magnets. Figure 175shows two PIT Bi-2212 short samples round wires criticalcharacteristics. These wires are extracted from a NexansFigure 174: Sample holder and variable temperature cryostat.Figure 175: Bi-2212 I c (B) performance for round wires.F. Debray, J. P. Domps, E. Mossang, S. DufresnesP. Brosse-Maron, J. P. Leggeri (Institute Neel, Gr<strong>en</strong>oble), J. M. Rey (CEA, IRFU, Saclay), P. Tixador (INP, Gr<strong>en</strong>oble)123


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009Status report of the 42+ Tesla hybrid magnet projectFor a giv<strong>en</strong> electrical power installation, the highest continuousmagnetic fields are obtained with hybrid magnets, i.e.the combination of a resistive inner coil with a superconductingouter one. The base-line for the coil sub-assembliesof the hybrid magnet under construction at LNCMI-G, isgiv<strong>en</strong> in table together with magnetic field contributions.One of the particularities of this <strong>des</strong>ign is to use poly-helixcoil for the innermost part of the resistive insert. The fieldproduced by the poly-helix and Bitter coils are planned tobe further increased, typically up to 36 − 37 T, for the upgradephase of this project.Hybrid compon<strong>en</strong>tsField (baseline)14 series connected helix coils 24.5 T2 series connected Bitter coils 9 T1 superconducting pancake coil 8.5 TTable 2: Subparts of the 42+ Tesla hybrid magnet.The already existing infrastructure of the hybrid magnet hasfixed the maximum dim<strong>en</strong>sions of the superconducting coil,which are listed in table 2 together with the other main parameters.A schematic view of the cryog<strong>en</strong>ics circuits isshown in figure 176. A new helium liquefier producing upto 130 l/h is necessary for the hybrid magnet project as theestimated consumptions in equival<strong>en</strong>t liquid He at 4.5 Kwith and without magnet <strong>en</strong>ergisation are equal to 100 l/hand 65 l/h respectively.Ext<strong>en</strong>sive tests performed in collaboration with the CEA-Saclay and industrial partners have allowed the validationof the conceptual study as well as the preparation of theindustrialization processes.CharacteristicsValuesInner/outer radius550/913 mmHeight1400 mmInductance3 HNominal curr<strong>en</strong>t (8.5 T)7100 AStored Energy76 MJOperating Temperature1.8 KTable 3: Main parameters of the superconducting coil.Figure 176:: Simplified cryog<strong>en</strong>ic process flow diagramThe specification of the superconducting Rutherford Cableon Conduit Conductor (RCOCC) has be<strong>en</strong> prepared and reviewed.The call for t<strong>en</strong>der was issued and the contract forthe production of all unit l<strong>en</strong>gths of the Nb-Ti/Cu Rutherfordcable (∼ 11 km) was signed at the <strong>en</strong>d of 2009.W. Joss, R. Pfister, P. Pugnat, L. RonayetteC. Berriaud, A. Daël, P. Fazilleau, B. Hervieu, F.P. Juster, C. Mayri, J.M. Rifflet (CEA-Saclay, Gif-sur-Yvette, France)A. Bourquard, D. Bresson, (Alstom, Belfort, France)124


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONMeasuring the vacuum magnetic birefring<strong>en</strong>cePreviously we reported measurem<strong>en</strong>ts of birefring<strong>en</strong>ces assmall as 10 −16 with our experim<strong>en</strong>tal apparatus. During thelast year we have worked on the optimization of the signalto noise ratio.Our activity can be divided into five main themes.Vacuum system : in order to understand the ultimate pressurethat we are able to reach and the possibly systematiceffects that can occur, we have characterized the nature ofthe residual gases in our vessel using a Residual Gas Analyzerduring the <strong>en</strong>tire pumping process. Because of theconductivity of the vacuum pipe passing through the magnetcryostat, the lower limit for the pressure that we canreach with our ionic pumps is of about 10 −8 mbar. We needa lower residual pressure. We are curr<strong>en</strong>tly studying thefeasibility of deposing inside the vacuum pipe a substratetype “getter” which acts as a distributed pumping systemall along the inner surface of the pipe. Contact with theSAS getter company, the world experts of this technique,are under way. We are confid<strong>en</strong>t to reach a vacuum betterthan 10 −11 mbar which is <strong>en</strong>ough for our experim<strong>en</strong>t.Mirror intrinsic birefring<strong>en</strong>ce : static birefring<strong>en</strong>ce interfer<strong>en</strong>tialmirrors used in Fabry-Perot cavities is a limitingfactor of the signal to noise ratio. In refer<strong>en</strong>ce [Bielsa etal., Applied Physics B 97, 457, (2009)], we reported newmeasurem<strong>en</strong>ts that confirm that mirror phase retardation inducedby mirror birefring<strong>en</strong>ce decreases wh<strong>en</strong> mirror reflectivityincreases. Our study indicates that the origin ofthe intrinsic birefring<strong>en</strong>ce can be ascribed to the reflectinglayers close to the substrate. We believe that this is animportant step forward the realization of birefring<strong>en</strong>ce-freemirrors.Perot cavity (l<strong>en</strong>gth 2.2 m) of finesse 198000 (figure 177).The linewidth of the cavity resonance (FWHM) is around350 Hz which is one of the smallest ever realized. TheLMA in Lyon is curr<strong>en</strong>tly analysing the other mirrors toimprove their performances, which will allow us to furtherimprove our cavity finesse.Figure 177: The finesse of a Fabry Perot cavity is evaluatedthanks to the lifetime of the photon in the cavity. Here, the lifetimeτ is 463 µs. The corresponding finesse is F = πcτŁ = 198000.New coil : we have built a new coil in order to reach theproject goal of 25 T. It is based on our ”X” geometry, andwe have named it the XXLCoil. Its l<strong>en</strong>gth is of about50 cm. We have tested it at the LNCMI in Toulouse andat the DHMFL in Dresd<strong>en</strong> where we have reached 31 T(figure 178) (B 2 L ≥ 300 T 2 m). This result is a big stepforward the measurem<strong>en</strong>t of the vacuum magnetic birefring<strong>en</strong>ce,since we have fulfill the project requirem<strong>en</strong>ts. In thefinal experim<strong>en</strong>t, we will use three coils like this one.Dynamical response of the Fabry Perot cavity : our Fabry-Perot cavity stores photons for an average time which isbigger than 300 µ s. The magnetic pulse duration is a fewmilliseconds. Wh<strong>en</strong> the storage time of photons approachesthe pulse duration, the effect of the cavity low-pass filtercannot anymore be neglected and the ellipticity signal is nolonger exactly proportional to the square of the magneticfield amplitude. We have observed such a behaviour, andwe have implem<strong>en</strong>ted the appropriate correction in the dataanalysis program.Very low loss cavity mirrors : we have tested four new mirrorsmade by LMA in Lyon. The mirrors curr<strong>en</strong>tly used inour cavity have losses of the order of 20 ppm. LMA mirrorlosses are expected to have losses as low as a few ppm. Ourmeasurem<strong>en</strong>ts confirm such expectations. We have measuredfor the best LMA mirror losses of about 5 ppm. As aconsequ<strong>en</strong>ce, using such a mirror, we have realized a FabryFigure 178: Magnetic field obtained with a transverse coil(XXLCoil). The relevant parameter for the magnetic vacuum birefring<strong>en</strong>cemeasurem<strong>en</strong>t is B 2 L=250 T 2 m. This factor has be<strong>en</strong>improved by a factor t<strong>en</strong> in this new configuration.P. Berceau, F. Bielsa, J. Mauchain, R. BattestiA. Dupays, M. Fouché and C. Rizzo (<strong>Laboratoire</strong> Collisions Agrégats Réactivité, Toulouse, France)125


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009Special purpose NMR probe for spectroscopy of quadrupolar nuclei at 30 TAlthough Nuclear Magnetic Resonance (NMR) is a wellestablished technique, there is a continuous demand for improveds<strong>en</strong>sitivity and spectral resolution. This is the basisfor the implem<strong>en</strong>tation of NMR techniques in high magneticfields. State of the art NMR spectroscopy is based onsuperconducting magnets with field str<strong>en</strong>gths up to 23.5 T.Higher dc magnetic fields may become possible with furtherdevelopm<strong>en</strong>t of superconducting technology, but theprogress is predicted to be increm<strong>en</strong>tal and exp<strong>en</strong>sive. Asan alternative, dc fields up to 34 T produced by resistivemagnets are already available, and there is considerable interestwithin the NMR community to implem<strong>en</strong>t g<strong>en</strong>eralpurpose and in particular high resolution NMR in thesemagnets. However, until rec<strong>en</strong>tly, NMR in resistive magnetswas limited to low resolution spectroscopy due to thestrong field inhomog<strong>en</strong>eity and the limited stability of thehigh power installations. In order to overcome these intrinsicdrawbacks, the developm<strong>en</strong>t of tailored and s<strong>en</strong>sitivityoptimized NMR instrum<strong>en</strong>tation is required.In this contribution we report on the commissioning of adedicated probe for NMR spectroscopy of quadrupolar nuclei(nuclear spin I > 1/2) at 30 T. In this case high magneticfield can overcome the problem of s<strong>en</strong>sitivity andline broad<strong>en</strong>ing in NMR spectra of low-s<strong>en</strong>sitivity nucleiwith strong quadrupole interactions [O. Pauvert et al., Inorg.Chem. 48, 8709 (2009)]. In order to fully b<strong>en</strong>efit fromthe advantages of higher magnetic fields, the <strong>des</strong>ign of theNMR probe has to be optimized for this particular application.A basic origin of low s<strong>en</strong>sitivity is a low gyromagneticratio γ of the examined nucleus (like 91 Zr or 25 Mg),that cannot be comp<strong>en</strong>sated as in the case of low naturalabundance, where isotope <strong>en</strong>richm<strong>en</strong>t increases s<strong>en</strong>sitivity.For a pulsed NMR experim<strong>en</strong>t consisting of an excitation ofthe nuclear transition by a radio frequ<strong>en</strong>cy (RF) field withstr<strong>en</strong>gth B 1 , followed by a detection period, a low value ofγ induces both a low signal (∝ γ 3 ) and a small spectral excitationwidth (∝ γB 1 ). H<strong>en</strong>ce, the effici<strong>en</strong>cy of an NMRexperim<strong>en</strong>t involving low-γ nuclei is strongly reduced. Inresponse to these limiting constraints the <strong>des</strong>ign of the RFcircuit of the NMR probe has to <strong>en</strong>sure that strong RF fieldsB 1 can be applied and that electric losses are minimized.In figure 179 we pres<strong>en</strong>t our realization of a room temperatureNMR probe meeting these constraints: Its bottomtuned RF circuit consists of the sol<strong>en</strong>oid NMR RF excitationand detection coil of a giv<strong>en</strong> inductance L C that isconnected in series with a variable tuning capacitance C T .L C and C T form a tunable series resonance circuit matchedto the source impedance (50 Ω) by a variable matching inductanceL M that is connected in parallel. Since the probeis based on the concept of creating strong B 1 fields by theapplication of high RF power, the probe has to withstandhigh voltages of the order of several kV without electricbreakdown. Therefore the tuning capacitance is realized bya copper cylinder capacitor, that can be continuously filledwith an alumina tube. In addition all conducting parts arerounded to avoid sources of arcing. Low electric loss is <strong>en</strong>suredby the usage of high conducting materials (copper,brass). The available tuning range of the probe (30 to 500MHz) covers most quadrupolar nuclei up to 30 T. The outerdiameter of the probe (28 mm) leaves space for future ext<strong>en</strong>sionslike passive shimming ev<strong>en</strong> in the 34 mm narrowbore M9 magnet of LNCMI-G.In addition, the probe is equipped with a second NMR circuitthat is used to stabilize the 24 MW magnet power supplyduring the experim<strong>en</strong>t by an active, NMR based fieldstabilization (NMR spin-lock). For this purpose the 63 CuNMR signal of a CuCl refer<strong>en</strong>ce sample is continuouslyrecorded and used for the g<strong>en</strong>eration of a control signal. Inorder to avoid crosstalks betwe<strong>en</strong> the two RF circuits thespin-lock circuit is fully shielded by a metallic cap. Theactive field stabilization <strong>en</strong>ables long time averaging of theNMR signal with refer<strong>en</strong>ce drifts of less than 1 ppm.After adjustm<strong>en</strong>t and optimization the probe was proved tobe fully operational. It withstands pulsed RF power of morethan 1 kW with a B 1 effici<strong>en</strong>cy of 18 G/ √ W for a sol<strong>en</strong>oidNMR coil of 3 mm inner diameter and 5 mm l<strong>en</strong>gth. At1 kW this corresponds to B 1 field str<strong>en</strong>gths of 570 G. Subsequ<strong>en</strong>tlythe probe with the spin-lock option was usedto conduct 91 Zr NMR studies on a series of inorganic Zrcompounds at 30 T. The obtained results provide a systematicand quantitative determination of the relation betwe<strong>en</strong>structural parameters (bond l<strong>en</strong>gths, bond angles, coordinationgeometry) and NMR parameters (chemical shift andquadrupole t<strong>en</strong>sors) of Zr compounds.Figure 179: Schematic view of the RF part of NMR probe consistingof the main RF circuit (upper right) and the shielded NMRspin-lock part (lower left, shielding cut for clarity).S. Krämer, C. de Vallée, H. Stork, J. Spitznagel, M. Horvatić, C. BerthierF. Fayon, A. Rakhmatullin, O. Pauvert, C. Bessada, D. Massiot (CEMHTI-CNRS, Orléans, France)126


2009 MAGNET DEVELOPMENT AND INSTRUMENTATIONNew rotating sample holder for broad-band quasi-optical HF-EPRspectroscopyDuring the last year, we have developed and used a newrotating sample holder for single crystal ori<strong>en</strong>tation studies.The system was constructed for our broad-band quasiopticalhigh field electron paramagnetic resonance (HF-EPR) spectrometer. For the <strong>des</strong>ign, a construction similarto the one of the Fabry-Pérot resonator was used, with themain structure made of Torlon. A simplified scheme of therotating holder attached to a corrugated waveguide is depictedin figure 180 and a photograph of a part of the holderwith a sample is shown in figure 181.The rotating holder relies on a rotating piezoelectricnanopositioner ANRv50 (Attocube systems AG) with a resistive<strong>en</strong>coder allowing for an absolute measurem<strong>en</strong>t of theangle. The calibrated <strong>en</strong>coder <strong>en</strong>ables the direct measurem<strong>en</strong>tof the position in the range 0 ◦ −337 ◦ . Due to the lackof space in the cryostat, it is not possible to use directly thepiezoelectric elem<strong>en</strong>t to rotate the sample holder. Thus, agear mechanism had to be introduced, with one gear driv<strong>en</strong>by the rotating piezoelectric device. The driv<strong>en</strong> gear in turndrives the Teflon holder for the sample. The mechanicalgear is responsible for the main uncertainty in the rotationposition, which is however less than 1 ◦ . A direct use ofthe rotating piezoelectric nanopositioner should decreasethis uncertainty by one order of magnitude (this configurationwill be soon possible with the installation of a newmagnet with a 50 mm bore in the VTI ). A flat gold platedmirror is placed below the sample for the reflection of theMW. A smooth guide having 6 mm inner diameter is usedto propagate the MW from the corrugated taper to the top ofthe gear mechanism, a few millimetres apart from the sample(Fig. 180). A necessary modulation coil for continuouswave EPR is wound directly onto the Torlon housing of therotating sample holder. It has a maximum field amplitudeof 25 G at the sample (with the actual power supply).Figure 180: Scheme of the rotating holder attached to the corrugatedwaveguide. The sample (black point) is placed on a Teflonholder. The gears are driv<strong>en</strong> by the rotating piezoelectric nanopositionerANRv50 (Attocube systems AG) with a resistive <strong>en</strong>coderallowing an absolute measurem<strong>en</strong>t of the angle. The modulationcoils are repres<strong>en</strong>ted by the crossed area. One part of the holder(dark-gray) is fixed to the corrugated waveguide; the other part(light-gray) with the sample can be dismounted. A photograph ofthis part of the holder is in Fig. 181.Manipulation and loading of the sample are very easy andcomfortable. The holder has two parts. Whereas one partwith the modulation coil is fixed to the corrugated waveguide,the second part with the sample can be easily removedfrom the previous one (Fig. 181). The sample located onthe Teflon holder is accessible as well from the top thanfrom the si<strong>des</strong>. This construction allows safe manipulationwith the sample under the microscope and eliminates errorswhich can be introduced during the manipulation with thesample.Detailed information for the rotating holder as well asFabry-Pérot resonator can be found in [Neugebauer andBarra, Appl. Magn. Reson. 37, 833 (2009)].Figure 181: Photograph of a part of the rotating holder used forori<strong>en</strong>tation studies of single crystals.P. Neugebauer, J. Flor<strong>en</strong>tin and A.-L. Barra127


MAGNET DEVELOPMENT AND INSTRUMENTATION 2009A new magnetometer for use in dc magnetic fields in excess of 28 T.Since many years we have developed int<strong>en</strong>se collaborationwith Fr<strong>en</strong>ch and foreign groups in the frame of the studyof the magnetic properties of solids under strong magneticfield and that in the 1.5 − 400 K temperature range. In2009 these exchanges with differ<strong>en</strong>t groups (France, USA,Poland, Turkey, Romania, Canada.) have be<strong>en</strong> th<strong>en</strong> maintained.A new chall<strong>en</strong>ge originates from the capability ofproduction of continuous magnetic field at the 35 T level(M9 magnet). Such a field value leads to an important reductionof the inner bore of the magnet that does not exceed34 mm. The construction of a new home-made magnetometerwas under tak<strong>en</strong> in the second half of the year2008. In March 2009, this new magnetometer has be<strong>en</strong> successfullytested on the M9 magnet with magnetic fields upto 35 T in the 1.5 − 350 K temperature range. It is worthnoting that the two main chall<strong>en</strong>ges were (i) one uniquesample holder which can be used either in a 50 mm boreor in a 34 mm bore in Gr<strong>en</strong>oble or in the Vibrating SampleMagnetometer in the NHMFL (Tallahassee USA). Thischoice allows an accurate comparisons of the magnetization(M) values delivered by the differ<strong>en</strong>t magnetometers underid<strong>en</strong>tical experim<strong>en</strong>tal conditions; (ii) Precise absolute calibrationof the magnetometer was performed using differ<strong>en</strong>tsingle crystals.Finally, the set sup offers the advantage of a good s<strong>en</strong>sitivityin the order of 2 × 10 −3 emu; the relative accuracy isestimated to be 0.1% wh<strong>en</strong> M is of the order of one emu,while the reproducibility on the field and on temperatureare estimated to be 0.01 T and 0.2 K, respectively. Thesample cavity is a cylinder whose axis is parallel to the appliedmagnetic field; its volume is of about 125 mm 3 inthe 4.2 − 400 K temperature range. In the 1.5 − 4.2 K domain(pumped helium bath) the available diameter of thesample increases up to 12 mm. The sample may be eitherpowder or ori<strong>en</strong>ted powder or single crystal. Isothermal orisofield magnetization curves may be obtained in positiveand (or) negative field. The quality of the measurem<strong>en</strong>tsperformed using this new home made magnetometer is illustratedby the figures 182 and 183. From each isothermalM T (H) obtained for the deuteride Y 0.7 Er 0.3 Fe 2 (D) 4.2the temperature variation of the differ<strong>en</strong>tial magnetic susceptibility(dM/dH)T versus the applied field was deduced(figure 182). The critical field of the transition is th<strong>en</strong> definedas the field corresponding to the maximum.In November 2009, in collaboration with the Academy ofSci<strong>en</strong>ces of Prague magnetic measurem<strong>en</strong>ts under pressure(P up to 11 kbar) were performed. Although the new M1magnet failed in relatively low field (100 kOe) the figure183 shows that measurem<strong>en</strong>ts of excell<strong>en</strong>t quality canbe performed. In the following month further experim<strong>en</strong>tsare expected with H up to 330 kOe in the 1.6 − 4.2 K temperaturerange.Figure 182: Differ<strong>en</strong>tial magnetic susceptibility versus appliedfield (up to 35 T) for the Y 0.7 Er 0.3 Fe 2 (D) 4.2 deuteride.Figure 183: Isothermal magnetization curves for the Ce 2 Fe 17alloy at 4.2 K under differ<strong>en</strong>t pressures.M. GuillotA. Zd<strong>en</strong>ek, K. Jiri, S. Yuriy, M. Martin, (Institute of Physics, The Academy of Sci<strong>en</strong>ces of the Czech Republic, Prague)C.V. Colin, O. Isnard (Institut Néel, CNRS and Université Joseph Fourier)128


2009 PROPOSALSProposals for Magnet Time – Projects Carried Out in 2009APPLIED SUPERCONDUCTORSInvestigation of the magnetic flux p<strong>en</strong>etration and conc<strong>en</strong>tration in bulk high-Tc Superconductors shaped with an array ofholes under pulsed magnetization conditionsChaud - CNRS/CRETA, Gr<strong>en</strong>oble, FranceDr. HaanappelTransport critical curr<strong>en</strong>t d<strong>en</strong>sity Jc in carbon-doped multifilam<strong>en</strong>tary PIT-MgB 2 wires in high magnetic fieldSulpice A. - CNRS, Institut Néel, Gr<strong>en</strong>oble, FranceDr. Wang, Dr. MossangTransport properties of MgB 2 superconducting wires with improved behaviour in high magnetic fieldsMalagoli A. - CNR-INFM, LAMIA, G<strong>en</strong>ova, ItalyDr. Fanciulli, Dr. Vignolo, Dr. RomanoCritical curr<strong>en</strong>ts of HTS wires under high magnetic flux d<strong>en</strong>sities and at variable temperatures for high field magnetsTixador P. -CNRS, Institut Néel, Gr<strong>en</strong>oble, FranceJ.P. Domps, Dr. Porcar, Dr.J.M. ReyTransport critical curr<strong>en</strong>t d<strong>en</strong>sity in carbon-doped MgB 2 wiresSulpice A. - CNRS, Institut Néel, Gr<strong>en</strong>oble, FranceDr. Wang, Dr. MossangTransport properties of MgB 2Malagoli A. - CNR-INFM, LAMIA, G<strong>en</strong>ova, ItalyDr. Vignolo, Dr. RomanoMAGNETISMHigh field magnetotransport in GeMn magnetic semiconductorsGerber - Tel Aviv University, IsraelDr. RaquetHigh field magnetization experim<strong>en</strong>ts on single crystalline (5-MAP) 2 CuBr 4Suellow - TU Braunschweig, Institute for Physics of Cond<strong>en</strong>sed Matter, GermanyBallonHigh field anisotropy of hematite and goethiteDekkers - Departm<strong>en</strong>t of Earth Sci<strong>en</strong>ces, Utrecht University, The NetherlandsF. DurantelHigh field magnetisation studies of the low-dim<strong>en</strong>sional zig-zag spin chains in Na 2 Cu 5 Si 4 O 14Klingeler - Insitute for Solid State Research @ IFW Dresd<strong>en</strong>, GermanyDr. Broto129


PROPOSALS 2009High field torque measurem<strong>en</strong>ts on a molecular dysprosium triangleSessoli R. - Universita degli Studi de Fir<strong>en</strong>ze, Dipartim<strong>en</strong>to di Chimica, Fir<strong>en</strong>ze, ItalyDr. LuzonSpin-Jahn-Teller effect in antiferromagnetic molecular whells: A systematic study of the field-ori<strong>en</strong>tation dep<strong>en</strong>d<strong>en</strong>ceWaldmann O. - Physikalisches Institut, Universität Freiburg, GermanyDr. LortzeMagnetic properties of new transition-metal thiospinels: study of the inter-network interactions in Mn 1−x Cd x Cr 2 S 4(0< x


2009 PROPOSALSSpin-Jahn-Teller effect in antiferromagnetic wheels: Its effect on the dielectric constantWaldmann O. - Physikalisches Institut Universität Freiburg, GermanyDr. LotzeQuantum oscillations of the total spin induced by Dzyaloshinski-Moriya interactions in the frustrated Cr 8 Ni AF ringAffronte M. -Instituto Nazionale di Fisica della Material, S3 <strong>National</strong> Research C<strong>en</strong>tre, Mod<strong>en</strong>a, ItalyDr. CarrettaSaturation magnetization of Fe 7 S 8 monoclinic 4C pyrhotite crystalsFillion G. - CNRS, Institut Louis Néel, Gr<strong>en</strong>oble, FranceGaMnAs val<strong>en</strong>ce band spectroscopy: <strong>en</strong>ergy-and mom<strong>en</strong>tum-resolved tunneling anisotropic magneto-resistanceDr. Giraud - CNRS, LPN, Marcoussis, FranceDr. FainiTorque and magnetization studies on the high field phases of the 2D frustrated spin system SrCu 2 (BO 3 ) 2Takigawa M. - University of Tokyo, Institute for Solid State Physics, Kahiwa-shi, Chiba, JapanDr. LevyStructural transitions in liquid crystal with negative and extremely low diamagnetic anisotropy doped with magneticparticlesKopcansky P. - Institute of Experim<strong>en</strong>tal Physics, Slovak Academy of Sci<strong>en</strong>ces, Kosice, SlovakiaDr. Koneracka, Dr. Timko, Dr. Koneracka, Dr. TomasovicovaSpin-Jahn-Teller effect in antiferromagnetic wheels: a systematic study of the field-ori<strong>en</strong>tation dep<strong>en</strong>d<strong>en</strong>ceWaldmann O. - Physikalisches Institut Universität Freiburg, GermanyDr. LotzeNMR investigation of high field phases of Volborthite with a distorted Kagome latticeTakigawa M. - University of Tokyo, Institute for Solid State Physics, Kahiwa-shi, Chiba, JapanDr. YoshidaGiant coercive fields in LuFe 2 O 4 at low temperaturesde Groot J. - Institut für Festkörperforschung, Forschungsz<strong>en</strong>trum Jülich, GermanyDr. AngstMAGNETIC RESONANCEMicrowave absorption in high pulsed magnetic field and crystal field problem in tetragonal compounds Ba 2 Cu 3 O x (x =6.0, 6.3)Kazei - Moscow State University, RussiaDr. GoiranMicrowave absorption peculiarities at the spontaneous and magnetic field induced phase transitions in the Jahn-Tellercompound DyVO 4Kazei - Moscow State University, RussiaDr. GoiranParamagnetic relaxation <strong>en</strong>hancem<strong>en</strong>t in NMR at very high magnetic field131


PROPOSALS 2009Kowalewski J. - Physical Chemistry, Arrh<strong>en</strong>ius Laboratory, Stockholm University, Swed<strong>en</strong>Dr. Fries91 Zr solid-state NMR spectroscopy at very high magnetic fieldFayon F. - CEMHTI-CNRS, Orléans, FranceDr. Rakhmatullin Milan, O. Pauvert, Dr. Bessada, Dr. MassiotNMR investigation of the Bose-Einstein cond<strong>en</strong>sation in the Han purple compound BaCuSi 2 O 6Stern R. - <strong>National</strong> Institute of Chemical Physics, NICPB, Tallinn, EstoniaDr. Kimura, F. AimoHigh field NMR study of the ortho-VIII YBaCuO 6,7Juli<strong>en</strong> M.H. - UJF, <strong>Laboratoire</strong> de Spectrométrie Physique, Saint Martin d’Hères, FranceDr. BonnMETALS AND SUPERCONDUCTORSHigh Field Hall Effect in YBCODoiron-Leyraud - Universite Sherbrooke, CanadaDr. ProustQuantum Oscillations in high purity, underdoped cuprate superconductorsBonn - University of British Columbia, CanadaDr. ProustTDO experim<strong>en</strong>ts on heavy-fermion systems in pulsed magnetic fieldsKnafo - LNCMI-T, FranceF. DurantelPulsed field transport measurem<strong>en</strong>ts on FeSeTe single crystalsBraithwaite - CEA, FranceDr. KnafoFermi surface studies and upper critical field anisotropy in iron chalcog<strong>en</strong>itesColdea - Bristol University, UKDr. ProustPoint contact spectroscopy of high Tc superconductors in pulsed magnetic fieldsRikk<strong>en</strong> - LNCMI Toulouse, FranceDr. GalibertConductivity t<strong>en</strong>sor of Bi 1−x Sb x beyond the quantum limitBehnia - Ecole Supérieure de Physique et de Chimie Industrielles, Paris, FranceDr. ProustQuantum interfer<strong>en</strong>ce and closed orbits in the quasi-two-dim<strong>en</strong>sional organicconductorß”-(BEDT-TTF) 4 H 3 O[Fe(C 2 O 4 ) 3 ] dichlorob<strong>en</strong>z<strong>en</strong>eLaukhin - Institut de Ci<strong>en</strong>cia de Materials de Barcelona (CSIC), Bellaterra, SpainDr. Audouard132


2009 PROPOSALSQuantum Oscillations in high purity, underdoped cuprate superconductorsBonn - University of British Columbia, Vancouver, CanadaDr. ProustdHvA experim<strong>en</strong>t in high Tc superconductors in extreme conditions of temperature and magnetic fieldVignolles - LNCMP, Toulouse, FranceDr. VignollesQuantum oscillations and anomalous transport in overdoped cupratesHussey - University of Bristol, UKDr. ProustQuantum oscillations and Hall effect measurem<strong>en</strong>ts in the cupratesTaillefer - Université de Sherbrooke, CanadaDr. ProustHigh-field magnetization of the heavy-fermion system Ce 1−x La x Ru 2 Si 2Knafo - LNCMP, Toulouse, FranceDr. KnafoLandau States in the electronic spectrum of MWCNTs under 60 TRaquet - LNCMP, Toulouse, FranceDr. RaquetSuppression of superconducting fluctuations by high magnetic fields in high-Tc cuprates and iron pnicti<strong>des</strong>Rullier-Alb<strong>en</strong>que - SPEC- IRAMIS - CEA, Saclay, FranceDr. ProustFermi surface properties under high magnetic fields in CeRh 2 Si 2 and URu 2 Si 2Aoki - INAC/SPSMS, CEA-Gr<strong>en</strong>oble, FranceDr. KnafoExploring the Fermi Surface on Iron Based Pcnitite and Chalcog<strong>en</strong>ite SuperconductorsColdea - Bristol University, UKDr. ProustDe Haas-van Alph<strong>en</strong> oscillations in (BEDT-TTF) 8 [Hg 4 Cl 1 2(C 6 H 5 Br)] 2Lyubovskii - Institute of Problems of Chemical Physics, RAS, RussiaDr. AudouardTests up to 2 GPa of a pressure cell <strong>des</strong>igned for isothermal transport measurem<strong>en</strong>ts at liquid helium temperatures in 55T pulsed magnetic fields. Application to the organic metal (BEDT-TTF) 8 Hg 4 Cl 1 2(C 6 H 5 Br)Audouard - LNCMI-T, FranceDr. AudouardMagneto-transport measurem<strong>en</strong>t in the heavy Fermion CeCoIn5Dr. Vignolles - LNCMI-T, FranceVignolles133


PROPOSALS 2009High field ultrasound measurem<strong>en</strong>ts on the magnetoelectric compound CuFeO 2Quirion - Dep. of Physics, Memorial University, St. John’s, CanadaDr. ProustStudies of Shapiro step response in the interchain transport in NbSe 3 in high magnetic fieldLatyshev Y. - Russian Academy of Sci<strong>en</strong>ces, Institute of radio<strong>en</strong>gineering and electronics, Moscow, RussiaDr. Monceau, A.P. OrlovStudies of Aharonov-Bohm effect on MW nanotubes and few layers graphite with columnar defectsLatyshev Y. - Russian Academy of Sci<strong>en</strong>ces, Institute of radio<strong>en</strong>gineering and electronics, Moscow, RussiaDr. Monceau, A.P. OrlovInvestigation in the possible Fulde-Ferrell-Larkin-Ovchinnikov state in the magnetic-field-induced organicsuperconductor Lambda-(BETS) 2 FeCl 4 by means of magnetic torque experim<strong>en</strong>tsLortz R. - Physics Dept. Hong Kong University of Sci<strong>en</strong>ce and Technology, Hong KongDr. Kobayashi, Dr. Sheikin, Dr. de MuerAngular-dep<strong>en</strong>d<strong>en</strong>t Nernst effect in bismuth beyond the quantum limitBehnia K. - ESPCI, <strong>Laboratoire</strong> de Physique Quantique, Paris, FranceDr. ZhuMapping the fermi surface of ternary pnicti<strong>des</strong>Bartkowiak M. - HLD, Dresd<strong>en</strong>, GermanyDr. GoodrichAngular-dep<strong>en</strong>d<strong>en</strong>t Nernst effect in bismuthBehnia K. - ESPCI, <strong>Laboratoire</strong> de Physique Quantique, Paris, FranceDr. FauquéNormal state magnetotransport anisotropy of the electron-doped high Tc uperconductor Nd 2−x Ce x CuO 4Kartsovnik M. - Walther-Meissner-Institut, Garching, GermanyDr. HelmHigh field de Haas-van Alph<strong>en</strong> effect measurem<strong>en</strong>ts in non-c<strong>en</strong>trosymmetric CeCoGe 3Sheikin I. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. SettaiInterplay of antiferromagnetism and superconductivity and <strong>en</strong>ormous upper critical field in CeIrSi 3 near itspressure-induced quantum critical pointSettai R. - Osaka University, Graduate School of Sci<strong>en</strong>ce, Osaka, JapanDr. Fittipaldi, Dr. SheikinMulti-band conduction in the newly discovered quaternary oxypnicti<strong>des</strong>Ferdeghini C. - CNR - INFM/LAMIA, Dipartim<strong>en</strong>to di Fisica, G<strong>en</strong>ova, ItalyDr. Fanciulli, Dr. TropeanoQuantum oscillation study of the hidd<strong>en</strong> order state by using high quality single crystal of URu 2 Si 2Aoki D. - INAC/SPSMS, CEA Gr<strong>en</strong>oble, Gr<strong>en</strong>oble, FranceDr. Sheikin134


2009 PROPOSALSThermoelectric t<strong>en</strong>sor of URu 2 Si 2 up to 28 T in a dc fieldMatsuda T. - CEA-Gr<strong>en</strong>oble, Gr<strong>en</strong>oble, FranceDr. SheikinHigh field de Haas-van Alph<strong>en</strong> effect measurem<strong>en</strong>ts in non-c<strong>en</strong>trosymmetric CeIrSi 3Settai R. - Osaka University, Graduate School of Sci<strong>en</strong>ce, Osaka, JapanDr. SheikinEnormous upper critical field in CeCoGe3 near its pressure-induced quantum critical pointSettai R. - Osaka University, Graduate School of Sci<strong>en</strong>ce, Osaka, JapanDr. SheikinHigh field de Haas-van Alph<strong>en</strong> effect measurem<strong>en</strong>ts in non-c<strong>en</strong>trosymmetric CePt 3 SiSettai R. - Osaka University, Graduate School of Sci<strong>en</strong>ce, Osaka, JapanDr. SheikinHigh field resistivity measurem<strong>en</strong>ts on single crystalline UPt 2 Si 2Schulze Grachtrup D. - Institute für Physik der Kond<strong>en</strong>siert<strong>en</strong> Materiel, TU Braunschweig, Braunschweig, GermanyNernst effect in the high-Tc superconductor YBCOTaillefer L. - Université de Sherbrooke, Sherbrooke, QC, CanadaDr. Behnia, Dr. Liangde Haas-van Alph<strong>en</strong> effect measurem<strong>en</strong>ts across the 28 T metamagnetic transition in CeIrIn 5 : in search for field-inducedmodification of the Fermi-surfaceSheikin I. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. AokiInvestigation of the uppper critical field of superconducting carbon nanotubes fabricated in the channels of AlPO4-5zeolite crystalsLortz R. - Hong Kong University of Sci<strong>en</strong>ce and Technology, Hong Kong, ChinaDr. WangAnisotropy of the in-plane normal state magneto-resistance of Sr 1−x La x CuO 2 epitaxial thin filmsRaffy H. - Université Paris Sud, <strong>Laboratoire</strong> de Physique <strong>des</strong> Soli<strong>des</strong>, Orsay, FranceDr. JovanovicTransport measurem<strong>en</strong>ts of Hc 2 and its anisotropy in FeSe 1−x Te x single crystals in static magnetic fieldBraithwaite D. - INAC/SPSMS/IMAPEC, CEA Gr<strong>en</strong>oble, FranceMagnetotransport in thin single crystals of graphite and graph<strong>en</strong>e containing nanoholesLatyshev Y. - Russian Academy of Sci<strong>en</strong>ces, Institute of radio<strong>en</strong>gineering and electronics, Moscow, RussiaDr. Monceau, A.P. OrlovMagnetostriction measurem<strong>en</strong>ts across the 26 T metamagnetic transition in CeRhSi 2Sheikin I. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. de Muer, Dr. Rodiere, Dr. Ha<strong>en</strong>, Dr. Lejay135


PROPOSALS 2009Angle resolved high field magnetic torque measurem<strong>en</strong>ts on Sr 4 Ru 3 O 1 0 single crystals and Sr 4 Ru 3 O 1 0/Sr 3 Ru 2 O 7 eutecticcrystalsZola D., Departm<strong>en</strong>t of Physics, University of Salerno, ItalyDr. Te<strong>des</strong>co, Dr. Polichetti, Dr. FittipaldiSEMICONDUCTORSMagnetotransport in silicon (110) MOSFETGold - CEMES-CNRS, FranceDr. GoiranPhotoluminesc<strong>en</strong>ce effici<strong>en</strong>cy and <strong>en</strong>ergy in the high mobility 2DEG. in the extreme quantum limit.Bellani - Dep. of Physics, ItalyEscoffierElectronic properties of graph<strong>en</strong>e nano-ribbons in high magnetic fieldEscoffier - LNCMP, Toulouse, FranceDr. EscoffierMono and bilayer graph<strong>en</strong>e in very high magnetic fieldsShukla - Institut de Minéralogie et de Physique <strong>des</strong> Milieux cond<strong>en</strong>sés (IMPMC), Paris, FranceDr. EscoffierAnomalous Quantum Hall effect in graph<strong>en</strong>e and bi-layer graph<strong>en</strong>eEscoffier - LNCMP, Toulouse, FranceDr. EscoffierHigh field spectroscopy of epitaxial graph<strong>en</strong>e layersPlochocka - Gr<strong>en</strong>oble High Magnetic Field Laboratory, FranceN. UbrigInvestigation of the dynamic alignem<strong>en</strong>t of DNA-wrapped single walled carbon nanotubes in liquid Susp<strong>en</strong>sionKono - Departm<strong>en</strong>t of Electrical and Computer Engineering, Rice University, Houston, USAN. UbrigLandau Level spectroscopy of graph<strong>en</strong>e monolayerUbrig - LNCMP, Toulouse, FranceN. UbrigElectron effective mass in InN under pressureLeotin - LNCMP, Toulouse, FranceDr. BrotoHigh magnetic field magnetoabsorption under high pressure in InSeSegura - Departam<strong>en</strong>to de Física Aplicada Ed. Investigación, Val<strong>en</strong>cia, SpainDr. BrotoMagneto-transport studies of magnetic impurities doped graphiteKumar - Neel Institute, CNRS/UJF, Gr<strong>en</strong>oble, France136


2009 PROPOSALSDr. EscoffierCyclotron resonance experim<strong>en</strong>ts in novel semiconductor dilute nitride alloysPatane - University of Nottingham, UKDr. GoiranTwo-dim<strong>en</strong>sional electron gas mobility and d<strong>en</strong>sity in AlInN/AIN/GaN heterostructuresGrandjean - EPFL, Lausanne, SwitzerlandDr. GoiranHigh field magneto-transport in FeSi thin filmsMarrows C.H. - School of Physics and Astronomy, University of Leeds, Leeds, U.K.Dr. PorterPolarized magneto-Raman scattering of optical phonon in epitaxial graph<strong>en</strong>eFaugeras C. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. Potemski, Dr. P. KossackiMagneto-optical investigation of the main absorption line of epitaxial graph<strong>en</strong>e in the extreme quantum limitMartinez G. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. De Heer, Dr. Orlita, Dr. Potemski, Dr. BergerPolaronic effects in single doped GaAs based quantum wellMartinez G. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. Friedland, Dr. Orlita, Dr. FaugerasTemperature dep<strong>en</strong>d<strong>en</strong>ce of a quantum Hall effect in Graph<strong>en</strong>eDiez E. - Universidad de Salamanca, Facultad de Ci<strong>en</strong>cias Fisicas, Salamanca, SpainDr. AmadoCurie temperature of diluted ferromagnetic semiconductorsVasek P. - Institute of Physics, Academy of Sci<strong>en</strong>ces of the Czech Republic, Prague, Czech RepublicDr. Smrcka, Dr. SvobodaPolarized magneto-optical investigation of the main absorption line of epitaxial graph<strong>en</strong>e in the extreme quantum limitMartinez G. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. Potemski, Dr. OrlitaMagneto-optical studies of combined exciton- cyclotron resonance in two dim<strong>en</strong>sional hole gasBryja L. - Institute of Physics, Wroclaw Technical University, Wroclaw, PolandDr. JadczakEffects of magnetic fields on excitonic features in optical spectra of CuInSe 2 single crystalsYakushev M. - University of Strathclyde, Departm<strong>en</strong>t of Physics, Glasgow, U.K.Dr. MartinFractional quantum Hall effect in CdTe/CdMgTe quantum wellsKunc J. - Charles University, The Institute of Physics, Prague, Czech Republic137


PROPOSALS 2009Dr. Potemski, Dr. PiotHigh field carrier transport studies in Mn doped II-IV-V2 semiconductorsKilanski L. - Institute of Physics, PAS, Warsaw, PolandDr.DobrowolskiMagneto-optical properties of semiconductor quantum wells subject to in-plane electric fieldTuçek J. - Institute of Physics, Faculty of Mathematics and Physics, Charles University, Prague, Czech RepublicDr. Kunc, Dr. OrlitaSystematic study of the temperature dep<strong>en</strong>d<strong>en</strong>ce of the quantum Hall effect in graph<strong>en</strong>e at high magnetic fieldDiez Fernandez E. - Universidad de Salamanca, Facultad de Ci<strong>en</strong>cias Fisicas, Salamanca, SpainDr. Rossella, Dr. Amado MonteroNIR magneto-spectroscopy of exfoliated graph<strong>en</strong>e membraneFaugeras C. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. PotemskiResonant magneto-polaron effect of a free 2D electron gas in CdTe QW with an in plane magnetic fieldFaugeras C. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. PotemskiInfrared spectroscopy of graph<strong>en</strong>e membranesOrlita M. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. Potemski, Dr. FaugerasSearch for free holes in InN:MgDmowski L.H. - Institute of High Pressure, Polish Academy of Sci<strong>en</strong>ces, Warsaw, PolandDr. Baj, Dr. KonczewiczElectricaly detected spin resonance in silicon MOSFETS and magnetically modulated Si MOSFETSSaraiva P. - Departm<strong>en</strong>t of Physics, University of Bath, U.K.Dr. NogaretFractional quantum Hall effect in trilayer system in a tilted fieldGusev G. - Instituto de Fisica, Universidade de Sao Paulo, BrasilStudy of coupling in a self-assembled QD systemKazimierczuk T. - Institute of Experim<strong>en</strong>tal Physics, University of Warsaw, PolandDr. Potemski, Dr. Goryca, Dr. Kossacki, Dr. PlochockaAbsorption of the graphite in the magnetic fieldPlochocka P. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. Potemski, Dr. Orlita, Dr. KossackiStudy of high excitonic states in quantum dots with single magnetic atomsGoryca M. - Institute of Experim<strong>en</strong>tal Physics, University of Warsaw, PolandDr. Potemski, Dr. Plochocka, Dr. Kossacki, Dr. Kazimierczuk138


2009 PROPOSALSHigh field magnetotransport in ferromagnetic semiconductor CdMnGeAs 2Kilanski L. - Institute of Physics, Polish academy of Sci<strong>en</strong>ce, Warsaw, PolandInvestigation of the <strong>en</strong>ergy fine structure of localized emission from GaN(In)As layers in high magnetic fieldKudrawiec R. - Institute of Physics, Wroclaw Institute of Technology, PolandDr. PotemskiMagnetotransport in graphiteVasek P. - Institute of Physics, ASCR, Prague, Czech RepublicDr. Smrcka, Dr. SvobodaAbsorption of the 2DEG system in integer Quantum Hall regimePlochocka P. - CNRS, LNCMI, Gr<strong>en</strong>oble, FranceDr. Potemski, Dr. MaudeSOFT MATTER AND OTHERSInterplay betwe<strong>en</strong> photoluminesc<strong>en</strong>ce and magnetism in MnF 2 , KMnF 3 and RbMnF 3 at high pressure and high magneticfieldRodriguez - Dpt. Ci<strong>en</strong>cias de la Tierra y Fisica de la Materia Cond<strong>en</strong>sada, Facultad de Ci<strong>en</strong>cias, Universidad deCantabria, SpainDr. BrotoSpectroscopic study of Yb 3+ -doped oxi<strong>des</strong> under hydrostatic pressure in magnetic fieldVali<strong>en</strong>te - Universidad de Cantabria, Santander, SpainDr. BrotoMHD effect on electrodeposition of nickel alloys: catalysts for hydrog<strong>en</strong> evolutionZabinski P. - AGH University of Sci<strong>en</strong>ces and Technology, Krakow, PolandDr. AnnaMagneto electro chemistry: Influ<strong>en</strong>ce of the magnetic forces on the mass transferBaaziz D. - GAMAS GDRE, EPM/SIMAP, CNRS, D.U., Saint Martin d’Hères, FranceDr. AlemanyMagnetic dep<strong>en</strong>d<strong>en</strong>ce of the ferroelectric soft mode frequ<strong>en</strong>cy in the t<strong>en</strong>sile strained EuTiO 3 thin filmKamba S. - ASCR, Institute of Physics, Prague, Czech RepublicDr. GoianCalcium hydroxyapatite electrodepositionChopart J.P. - <strong>Laboratoire</strong> DTI, UFR Sci<strong>en</strong>ces Naturelles, Reims, FranceDr. Daltin, Dr. BaudartAlfv<strong>en</strong> waves in liquid sodium: non-linear interactions and turbul<strong>en</strong>ceAlboussiere T. - CNRS, <strong>Laboratoire</strong> LGIT, St Martin d’Hères, FranceD. Schmitt, P. Cardin, F. Plunian, H.C. Nataf, J.P. Masson, P. La RizzaEffect of a magnetic field on the d<strong>en</strong>drite morphology during crystal growth of aluminium and Zinc-based alloys.Analysis of the various effects such as thermo-effects, diffusion, modification of the structures139


PROPOSALS 2009Fautrelle Y. - INPG/EPM, ENSHMG, St Martin d’Hères, FranceDr. Saadi, Dr. Li140


2009 THESESPhD Theses 20091. Nanot Sébasti<strong>en</strong>Structure de ban<strong>des</strong> et transport électronique dans les nanotubes de carbone sous champ magnétique int<strong>en</strong>se.Doctorat de l’Université de Toulouse, délivré par l’Université de Toulouse III Paul Sabatier Thèse sout<strong>en</strong>ue le v<strong>en</strong>dredi30 octobre 20092. Millot MariusSpectroscopies sous haute pression et champ magnétique int<strong>en</strong>se.Doctorat de l’Université de Toulouse, délivré par l’Université de Toulouse III Paul Sabatier Thèse sout<strong>en</strong>ue le 13Novembre 20093. Jaudet CyrilEffet de Haas-van Alph<strong>en</strong> dans les supraconducteurs haute température critique.Doctorat de l’Université de Toulouse, délivré par l’Université de Toulouse III Paul Sabatier Thèse sout<strong>en</strong>ue le 17Novembre 2009141


PUBLICATIONS 2009List of Publications 2009[1] F. Aimo, S. Kraemer, M. Klanjsek, M. Horvatic, C. Berthier and H. Kikuchi. Spin configuration in the 1/3 magnetization plateauof azurite determined by NMR. Physical Review Letters 102, 127205 (2009).[2] L. E. G. Armas, G. M. Gusev, T. E. Lamas, A. K. Bakarov and J. C. Portal. Quantum Hall ferromagnet in a double well withvanishing g-factor. International Journal of Modern Physics B 23, 2933 (2009). 18th International Confer<strong>en</strong>ce on High MagneticFields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[3] A. Audouard, C. Jaudet, D. Vignolles, R. X. Liang, D. A. Bonn, W. N. Hardy, L. Taillefer and C. Proust. Multiple quantumoscillations in the de Haas-van Alph<strong>en</strong> spectra of the underdoped high-temperature superconductor YBa 2 Cu 3 O 6.5 . PhysicalReview Letters 103, 157003 (2009).[4] S. Awirothananon, S. Raymond, S. Stud<strong>en</strong>ikin, M. Vachon, W. R<strong>en</strong>der, A. Sachrajda, X. Wu, A. Babinski, M. Potemski, S. Fafard,S. J. Ch<strong>en</strong>g, M. Korkusinski and P. Hawrylak. Single-exciton <strong>en</strong>ergy shell structure in InAs/GaAs quantum dots. Physical ReviewB 78, 235313 (2008).[5] A. Babinski, A. Golnik, J. Borysiuk, S. Kret, P. Kossacki, J. A. Gaj, S. Raymond, M. Potemski and Z. R. Wasilewski. Threedim<strong>en</strong>sionallocalization of excitons in the InAs/GaAs wetting layer - magnetospectroscopic study. Physica Status Solidi B-BasicSolid State Physics 246, 850 (2009). 5th International Confer<strong>en</strong>ce on Semiconductor Quantum Dots, Gyeongju, SOUTH KOREA,MAY 11-16, 2008.[6] M. G. Banks, R. K. Kremer, C. Hoch, A. Simon, B. Ouladdiaf, J. M. Broto, H. Rakoto, C. Lee and M. H. Whangbo. Magneticordering in the frustrated heis<strong>en</strong>berg chain system cupric chloride CuCl 2 . Physical Review B 80, 024404 (2009).[7] F. Bert, A. Olariu, A. Zorko, P. M<strong>en</strong>dels, J. C. Trombe, F. Duc, M. A. de Vries, A. Harrison, A. D. Hillier, J. Lord, A. Amatoand C. Baines. Frustrated magnetism in the quantum Kagome Herbertsmithite ZnCu 3 (OH) 6 Cl 2 antiferromagnet. Journal ofPhysics: Confer<strong>en</strong>ce Series 145, 012004 (2009).[8] F. Bielsa, A. Dupays, M. Fouche, R. Battesti, C. Robilliard and C. Rizzo. Birefring<strong>en</strong>ce of interfer<strong>en</strong>tial mirrors at normalincid<strong>en</strong>ce. Applied Physics B-Lasers and Optics 97, 457 (2009).[9] L. Bogani, C. Danieli, E. Biavardi, N. B<strong>en</strong>diab, A.-L. Barra, E. Dalcanale, W. Wernsdorfer and A. Cornia. Single-molecule-magnetcarbon-nanotube hybrids. Angewandte Chemie-International Edition 48, 746 (2009).[10] N. Bréfuel, H. Watanabe, L. Toupet, J. Come, N. Matsumoto, E. Collet, K. Tanaka and J.-P. Tuchagues. Concerted spin crossoverand symmetry breaking yield three thermally and one light-induced crystallographic phases of a molecular material. AngewandteChemie International Edition 48,49, 9304 (2009).[11] L. Bryja, A. Wojs, J. Misiewicz, P. Plochocka, M. Potemski, D. Reuter and A. Wieck. Photoluminesc<strong>en</strong>ce studies of positivelycharged excitons in asymmetric GaAs/Ga 1−x Al x As quantum wells with a two-dim<strong>en</strong>sional hole gas. International Journal ofModern Physics B 23, 2718 (2009). 18th International Confer<strong>en</strong>ce on High Magnetic Fields in Semiconductor Physics andNanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[12] M. V. Budantsev, A. G. Pogosov, A. K. Bakarov, A. I. Toropov and J. C. Portal. Effect of an in-plane magnetic field on magnetoresistancehysteresis of the two-dim<strong>en</strong>sional electron gas in the integer quantum Hall effect regime. JETP Letters 89, 92(2009).[13] M. Casse, F. Rochette, L. Thev<strong>en</strong>od, N. Bhouri, F. Andrieu, G. Reimbold, F. Boulanger, M. Mouis, G. Ghibaudo and D. K. Maude.A compreh<strong>en</strong>sive study of magnetoresistance mobility in short channel transistors: Application to strained and unstrained siliconon-insulatorfield-effect transistors. Journal of Applied Physics 105, 084503 (2009).[14] X. Chaud, J. Noudem, T. Prikhna, Y. Savchuk, E. Haanappel, P. Diko and C. P. Zhang. Flux mapping at 77 k and localmeasurem<strong>en</strong>t at lower temperature of thin-wall YBaCuO single-domain samples oxyg<strong>en</strong>ated under high pressure. Physica C-Superconductivity And Its Applications 469, 1200 (2009).[15] R. A. Cooper, Y. Wang, B. Vignolle, O. J. Lipscombe, S. M. Hayd<strong>en</strong>, Y. Tanabe, T. Adachi, Y. Koike, M. Nohara, H. Takagi,C. Proust and N. E. Hussey. Anomalous criticality in the electrical resistivity of La 2−x Sr x CuO 4 . Sci<strong>en</strong>ce 323, 603 (2009).[16] C. Danieli, A. Cornia, C. Cecchelli, R. Sessoli, A.-L. Barra, G. Ponterini and B. Zanfrognini. A novel class of tetrairon(III) singlemoleculemagnets with graph<strong>en</strong>e-binding groups. Polyhedron 28, 2029 (2009). 11th International Confer<strong>en</strong>ce on Molecule-BasedMagnets (ICMM 2008), Flor<strong>en</strong>ce, ITALY, SEP 21-24, 2008.[17] C. R. Dean, B. A. Piot, G. Gervais, L. N. Pfeiffer and K. W. West. Curr<strong>en</strong>t-induced nuclear-spin activation in a two-dim<strong>en</strong>sionalelectron gas. Physical Review B 80, 153301 (2009).[18] E. del Corro, J. Gonzalez, M. Taravillo, W. Escoffier and V. G. Baonza. Graphite under non-hydrostatic conditions. High PressureResearch 28, 583 (2008).[19] W. Desrat, S. Kamara, F. Terki, S. Charar, J. Sadowski and D. K. Maude. Antisymmetric magnetoresistance anomalies andmagnetic domain structure in GaMnAs/InGaAs layers. Semiconductor Sci<strong>en</strong>ce and Technology 24, 065011 (2009).[20] C. v. Dewitz, F. Hatami, M. Millot, J. M. Broto, J. Leotin and W. T. Masselink. Evid<strong>en</strong>ce of type-I direct recombination in InP/GaPquantum dots via magnetoluminesc<strong>en</strong>ce. Applied Physics Letters 95, 151105 (2009).142


2009 PUBLICATIONS[21] O. Drach<strong>en</strong>ko, D. V. Kozlov, V. Y. Aleshkin, V. I. Gavril<strong>en</strong>ko, K. V. Maremyanin, A. V. Ikonnikov, B. N. Zvonkov, M. Goiran,J. Leotin, G. Fasching, S. Winnerl, H. Schneider, J. Wosnitza and M. Helm. High-field splitting of the cyclotron resonanceabsorption in strained p-InGaAs/GaAs quantum wells. Physical Review B 79, 073301 (2009).[22] C. A. Duarte, G. M. Gusev, T. E. Lamas, A. K. Bakarov and J. C. Portal. Valley splitting and g-factor in AlAs quantum wells. InternationalJournal of Modern Physics B 23, 2948 (2009). 18th International Confer<strong>en</strong>ce on High Magnetic Fields in SemiconductorPhysics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[23] C. Duboc and M.-N. Collomb. Détermination <strong>des</strong> proprités électroniques de complexes du manganèse. spectroscopie derésonance paramagnétique électronique à haut champ (RPE-HF) et calculs théoriques : une combinaison gagnante. ActualitéChimique 326, 19 (2009).[24] C. Duboc and M.-N. Collomb. Multifrequ<strong>en</strong>cy high field EPR investigation of a mononuclear manganese(IV) complex. Chem.Comm. 2717 (2009).[25] C. Faugeras, M. Amado, P. Kossacki, M. Orlita, M. Sprinkle, C. Berger, W. A. de Heer and M. Potemski. Tuning the electronphononcoupling in multilayer graph<strong>en</strong>e with magnetic fields. Physical Review Letters 103, 186803 (2009).[26] C. Faugeras, M. Orlita, S. Deutchlander, G. Martinez, P. Y. Yu, A. Riedel, R. Hey and K. J. Friedland. Measurem<strong>en</strong>t of the infraredtransmission through a single doped GaAs quantum well in an external magnetic field: Evid<strong>en</strong>ce for polaron effects. PhysicalReview B 80, 073303 (2009).[27] B. Fauqué, B. Vignolle, C. Proust, J. Issi and K. Behnia. Electronic instability in bismuth far beyond the quantum limit. NewJournal of Physics 11, 113012 (2009).[28] B. Fauqué, H. Yang, I. Sheikin, L. Balicas, J.-P. Issi and K. Behnia. Hall plateaus at magic angles in bismuth beyond the quantumlimit. Physical Review B 79, 245124 (2009).[29] O. M. Fedorych, S. A. Stud<strong>en</strong>ikin, S. Moreau, M. Potemski, T. Saku and Y. Hirayama. Microwave magnetoplasmon absorptionby a 2DEG stripe. International Journal of Modern Physics B 23, 2698 (2009). 18th International Confer<strong>en</strong>ce on High MagneticFields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[30] D. Fishman, C. Faugeras, M. Potemski, A. Revcolevschi and P. H. M. van Loosdrecht. Magneto-optical readout of dark excitondistribution in cuprous oxide. Physical Review B 80, 045208 (2009).[31] M. Fittipaldi, L. Sorace, A.-L. Barra, C. Sangregorio, R. Sessoli and D. Gatteschi. Molecular nanomagnets and magnetic nanoparticles:the EMR contribution to a common approach. Physical Chemistry Chemical Physics 11, 6555 (2009).[32] S. Frantz, M. Sieger, I. Hart<strong>en</strong>bach, F. Lissner, T. Schleid, J. Fiedler, C. Duboc and W. Kaim. Structure, electrochemistry, spectroscopy,and magnetic resonance, including high-field EPR, of ((µ-abpy)[Re(CO) 3 X] 2 ) 0 , - where abpy = 2,2 ′ -azobispyridineand X = F, Cl, Br, I. J. Organomet. Chem. 694, 1122 (2009).[33] K. J. Friedland, A. Siddiki, R. Hey, H. Kostial, A. Riedel and D. K. Maude. Quantum hall effect in a high-mobility two-dim<strong>en</strong>sionalelectron gas on the surface of a cylinder. Physical Review B 79, 125320 (2009).[34] A. Goiran, J. M. Poumirol, M. P. Semtsiv, W. T. Masselink, D. Smirnov, V. V. Rylkov and J. Leotin. Magnetospectroscopy of AIPquantum wells. Transport and Optical Properties of Nanomaterials 1147, 3 (2009).[35] M. Goiran, M. P. Semtsiv, W. T. Masselink and J. Leotin. AlP/GaP quantum wells for implem<strong>en</strong>ting intersubband devices in the30-60 µm wavel<strong>en</strong>gth region. 2008 33rd International Confer<strong>en</strong>ce On Infrared, Millimeter And Terahertz Waves, Vols 1 And 2350 (2008).[36] J. Gonzalez, C. Power, E. Belandria, J. Jorge, F. Gonzalez-Jim<strong>en</strong>ez, M. Millot, S. Nanot, J. M. Broto and E. Flahaut. Pressuredep<strong>en</strong>d<strong>en</strong>ce of Raman mo<strong>des</strong> in double wall carbon nanotubes filled with -Fe. High Pressure Research 28, 577 (2008).[37] L. Gregoli, C. Danieli, A.-L. Barra, P. Neugebauer, G. Pellegrino, G. Poneti, R. Sessoli and A. Cornia. Magnetostructural correlationsin tetrairon(III) single-molecule magnets. Chemistry-A European Journal 15, 6456 (2009).[38] G. M. Gusev, S. Wiedmann, O. E. Raichev, A. K. Bakarov and J. C. Portal. Emerg<strong>en</strong>t and re<strong>en</strong>trant fractional quantum hall effectin trilayer systems in a tilted magnetic field. Physical Review B (Cond<strong>en</strong>sed Matter and Materials Physics) 80, 161302 (2009).[39] K. Haas, T. Kazimierczuk, P. Wojnar, A. Golnik, J. Gaj and P. Kossacki. Control of local electric fields influ<strong>en</strong>cing the photoluminesc<strong>en</strong>ceof an individual CdTe/ZnTe quantum dot. Acta Physica Polonica A 116, 896 (2009).[40] J. Jadczak, L. Bryja, P. Plochocka, A. Wojs, J. Misiewicz, D. Maude and M. Potemski. Combined exciton-cyclotron resonance inphotoluminesc<strong>en</strong>ce of a two-dim<strong>en</strong>sional hole gas. Acta Physica Polonica A 116, 852 (2009).[41] S. Jandl, A. A. Mukhin, V. Y. Ivanov, A. Balbashov and M. Orlita. Nd 3+ crystal-field study of weakly doped Nd 1−x Ca x MnO 3 .Journal of Magnetism and Magnetic Materials 321, 3607 (2009).[42] C. Jaudet, J. Levallois, A. Audouard, D. Vignolles, B. Vignolle, R. Liang, D. A. Bonn, W. N. Hardy, N. E. Hussey, L. Tailleferand C. Proust. Quantum oscillations in underdoped YBa 2 Cu 3 O 6.5 . Physica B-Cond<strong>en</strong>sed Matter 404, 354 (2009).[43] B. Jouault, M. Gryglas, M. Baj, A. Cavanna, U. G<strong>en</strong>nser, G. Faini and D. K. Maude. Spin filtering through a single impurity in aGaAs/AlAs/GaAs resonant tunneling device. Physical Review B 79, 041307 (2009).[44] M.-H. Juli<strong>en</strong>. Enhanced low-<strong>en</strong>ergy spin dynamics with diffusive character in the iron-based superconductor (La 0.87 Ca 0.13 )FePO:Analogy with high T-c cuprates. Journal of the Physical Society of Japan 77, 125002 (2008).[45] M. H. Juli<strong>en</strong>, H. Mayaffre, M. Horvatic, C. Berthier, X. D. Zhang, W. Wu, G. F. Ch<strong>en</strong>, N. L. Wang and J. L. Luo. Homog<strong>en</strong>eousvs. inhomog<strong>en</strong>eous coexist<strong>en</strong>ce of magnetic order and superconductivity probed by NMR in Co- and K-doped iron pnicti<strong>des</strong>. EuroPhysics Letters 87, 37001 (2009).[46] A. A. Kapustin, A. A. Shashkin, V. T. Dolgopolov, M. Goiran, H. Rakoto and Z. D. Kvon. Spin susceptibility and polarizationfield in a dilute two-dim<strong>en</strong>sional electron system in (111) silicon. Physical Review B 79, 205314 (2009).[47] Z. A. Kazei, V. V. Snegirev, N. P. Danilova, M. Goiran, L. P. Kozeeva and M. Y. Kam<strong>en</strong>eva. Microwave absorption spectra andthe problem of the crystal field in tetragonal compounds HoBa 2 Cu 3 O x (x=6.0, 6.3). JETP Letters 88, 725 (2008).143


PUBLICATIONS 2009[48] T. Kazimierczuk, A. Golnik, M. Goryca, P. Wojnar, J. Gaj and P. Kossacki. Anisotropic exchange interaction betwe<strong>en</strong> p-shellelectron and s-shell hole in CdTe/ZnTe quantum dots. Acta Physica Polonica A 116, 882 (2009).[49] W. Knafo, C. Meingast, A. V. Boris, P. Popovich, N. N. Kovaleva, P. Yordanov, A. Maljuk, R. K. Kremer, H. V. Lohneys<strong>en</strong> andB. Keimer. Ferromagnetism and lattice distortions in the perovskite YTiO 3 . Physical Review B 79, 054431 (2009).[50] W. Knafo, C. Meingast, S. Sakarya, N. H. van Dijk, Y. Huang, H. Rakoto, J. M. Broto and H. V. Lohneys<strong>en</strong>. Critical scalingof the magnetization and magnetostriction in the weak itinerant ferromagnet UIr. Journal of the Physical Society of Japan 78,043707 (2009).[51] W. Knafo, S. Raymond, P. Lejay and J. Flouquet. Antiferromagnetic criticality at a heavy-fermion quantum phase transition.Nature Physics 5, 753 (2009).[52] J. Kobak, M. Goryca, P. Kossacki, A. Golnik, G. Karczewski, T. Wojtowicz and J. Gaj. Magnetization dynamics of a (Cd, Mn)Tequantum well in pulsed magnetic field. Acta Physica Polonica A 116, 907 (2009).[53] Y. Kopelevich, B. Raquet, M. Goiran, W. Escoffier, R. R. da Silva, J. C. M. Pantoja, I. A. Luk’yanchuk, A. Sinch<strong>en</strong>ko andP. Monceau. Searching for the fractional quantum Hall effect in graphite. Physical Review Letters 103, 116802 (2009).[54] M. Koperski, T. Kazimierczuk, M. Goryca, P. Wojnar, A. Golnik, P. Kossacki and J. Gaj. Numerical rate equation approach topicosecond charge state dynamics in CdTe/ZnTe quantum dots. Acta Physica Polonica A 116, 893 (2009).[55] G. Koutroulakis, J. M. D. Stewart, V. F. Mitrovic, M. Horvatic, C. Berthier, G. Lapertot and J. Flouquet. Field evolution ofcoexisting superconducting and magnetic orders in CeCoIn 5 . Phys. Rev. Lett. , in press (arXiv:0912.3548) (2010).[56] Y. I. Latyshev, A. P. Orlov, A. Y. Latyshev, A. M. Smolovich, P. Monceau and D. Vignolles. Rec<strong>en</strong>t experim<strong>en</strong>ts on interlayertunneling spectroscopy and transverse electric field effect in NbSe 3 . Physica B-Cond<strong>en</strong>sed Matter 404, 399 (2009).[57] J. Levallois, K. Behnia, J. Flouquet, P. Lejay and C. Proust. On the <strong>des</strong>truction of the hidd<strong>en</strong> order in URu 2 Si 2 by a strongmagnetic field. Euro Physics Letters 85, 27003 (2009).[58] F. Levy, I. Sheikin, C. Berthier, M. Horvatic and M. Takigawa. Reply to the Comm<strong>en</strong>t by S. E. Sebastian and N. Harrison. EuroPhysics Letters 85, 67008 (2009).[59] F. Levy, I. Sheikin, B. Gr<strong>en</strong>ier, C. Marc<strong>en</strong>at and A. Huxley. Coexist<strong>en</strong>ce and interplay of superconductivity and ferromagnetismin URhGe. Journal of Physics-Cond<strong>en</strong>sed Matter 21, 164211 (2009). 25th International Confer<strong>en</strong>ce on Low Temperature Physics(LT25), Amsterdam, NETHERLANDS, AUG 06-13, 2008.[60] O. Lipscombe, B. Vignolle, T. Perring, C. Frost and S. Hayd<strong>en</strong>. Emerg<strong>en</strong>ce of coher<strong>en</strong>t magnetic excitations in the high temperatureunderdoped La 2 − xSr x CuO 4 superconductor at low temperatures. Physical Review Letters 102, 167002 (2009).[61] G. P. Lousberg, J. Gagnard, E. Haanappel, X. Chaud, M. Ausloos, B. Vanderheyd<strong>en</strong> and P. Vanderbemd<strong>en</strong>. Pulsed field magnetizationof drilled high temperature superconductors: flux front propagation in the volume and on the surface. SuperconductorSci<strong>en</strong>ce and Technology 22, 125026 ((2009)).[62] T. T. A. Lumm<strong>en</strong>, C. Strohm, H. Rakoto, A. A. Nugroho and P. H. M. van Loosdrecht. High-field recovery of the undistortedtriangular lattice in the frustrated metamagnet CuFeO 2 . Physical Review B 80, 012406 (2009).[63] A. Malagoli, V. Braccini, M. Tropeano, M. Vignolo, C. Bernini, C. Fanciulli, G. Romano, M. Putti, C. Ferdeghini, E. Mossang,A. Polyanskii and D. C. Larbalestier. Effect of grain refinem<strong>en</strong>t on <strong>en</strong>hancing critical curr<strong>en</strong>t d<strong>en</strong>sity and upper critical field inundoped MgB 2 ex situ tapes. Journal of Applied Physics 104, 103908 (2008).[64] M. Matsuda, K. Ohoyama, S. Yoshii, H. Nojiri, P. Frings, F. D. andB. Vignolle, G. L. J. A. Rikk<strong>en</strong>, L.-P. Regnault, S.-H. Lee,H. Ueda, and Y. Ueda. Universal magnetic structure of the half-magnetization phase in Cr-based spinels. Physical Review Letters(2009). Accepted for publications.[65] C. Meingast, Q. Zhang, T. Wolf, F. Hardy, K. Grube, W. Knafo, P. Adelmann, P. Schweiss and H. von Lohneys<strong>en</strong>. Resistivity ofMn 1−x Fe x Si Single Crystals: Evid<strong>en</strong>ce for Quantum Critical Behavior. Properties and Applications of Thermoelectric Materials261 (2009).[66] M. Millot, S. George, J. M. Broto, B. Couzinet, J. C. Chervin, A. Polian, C. Power and J. Gonzalez. New diamond anvil cell foroptical and transport measurem<strong>en</strong>ts under high magnetic fields up to 60T. High Pressure Research 28, 627 (2008).[67] M. Millot, S. Gilliland, J. M. Broto, J. Gonzalez, J. Leotin, A. Chevy and A. Segura. High pressure and high magnetic fieldbehaviour of free and donor-bound-exciton photoluminesc<strong>en</strong>ce in InSe. Physica Status Solidi B-Basic Solid State Physics 246,532 (2009).[68] M. Nannini, H. Cloez, S. Girard, C. Roux, J. P. Serries, M. T<strong>en</strong>a, L. Zani and E. Mossang. Characterization of industrial NbTistrands at variable field for JT-60SA toroidal field coils. Fusion Engineering and Design 84, 1404 (2009). 25th Symposium onFusion Technology, Rostock, GERMANY, SEP 15-19, 2008.[69] S. Nanot, R. Avriller, W. Escoffier, J.-M. Broto, S. Roche and B. Raquet. Propagative landau states and fermi level pinning incarbon nanotubes. Physical Review Letters 103, 256801 (2009).[70] S. Nanot, W. Escoffier, B. Lassagne, J. M. Broto and B. Raquet. Exploring the electronic band structure of individual carbonnanotubes under 60 T. Comptes R<strong>en</strong>dus Physique 10, 268 (2009).[71] P. Neugebauer and A. Barra. New cavity <strong>des</strong>ign for broad-band quasi-optical HF-EPR spectroscopy. Appl. Magn. Reson. 37, 833(2009).[72] P. Neugebauer, M. Orlita, C. Faugeras, A. L. Barra and M. Potemski. How perfect can graph<strong>en</strong>e be? Physical Review Letters103, 136403 (2009).[73] A. Nish, R. J. Nicholas, C. Faugeras, Z. Bao and M. Potemski. High-field magnetooptical behavior of polymer-embedded singlewalledcarbon nanotubes. Physical Review B 78, 245413 (2008).[74] A. Nogaret, J.-C. Portal, H. E. Beere, D. A. Ritchie and C. Phillips. Quantum interfer<strong>en</strong>ce of magnetic edge channels activatedby intersubband optical transitions in magnetically confined quantum wires. Journal of Physics-Cond<strong>en</strong>sed Matter 21, 025303(2009).144


2009 PUBLICATIONS[75] S. Nowak, T. Jakubczyk, M. Goryca, P. Ciosmak, A. Golnik, P. Kossacki, P. Wojnar and J. Gaj. Emission of self assembledCdTe/ZnTe quantum dot samples with differ<strong>en</strong>t cap thickness. Acta Physica Polonica A 116, 890 (2009).[76] Y. O<strong>en</strong>er and M. Guillot. Magnetic disorder in Ti doped ErCo 2 : High-magnetic-field study. Journal of Applied Physics 105,07E120 (2009). 53rd Annual Confer<strong>en</strong>ce on Magnetism and Magnetic Materials, Austin, TX, NOV 11-14, 2008.[77] M. Orlita, C. Faugeras, G. Martinez, D. K. Maude, J. M. Schneider, M. Sprinkle, C. Berger, W. A. de Heer and M. Potemski.Magneto-transmission of multi-layer epitaxial graph<strong>en</strong>e and bulk graphite: A comparison. Solid State Communications 149,1128 (2009). Graph<strong>en</strong>e Week 2008 International Confer<strong>en</strong>ce, Trieste, ITALY, 2008.[78] M. Orlita, C. Faugeras, P. Plochocka, P. Neugebauer, G. Martinez, D. K. Maude, A. L. Barra, M. Sprinkle, C. Berger, W. A.de Heer and M. Potemski. Approaching the Dirac Point in High-Mobility Multilayer Epitaxial Graph<strong>en</strong>e. Physical Review Letters101, 267601 (2008).[79] M. Orlita, C. Faugeras, J. M. Schneider, G. Martinez, D. K. Maude and M. Potemski. Graphite from the viewpoint of Landaulevel spectroscopy: An effective graph<strong>en</strong>e bilayer and monolayer. Physical Review Letters 102, 166401 (2009).[80] I. Pallecchi, C. Fanciulli, M. Tropeano, A. Pal<strong>en</strong>zona, M. Ferretti, A. Malagoli, A. Martinelli, I. Sheikin, M. Putti and C. Ferdeghini.Upper critical field and fluctuation conductivity in the critical regime of doped SmFeAsO. Physical Review B 79, 104515(2009).[81] J. Papierska, M. Goryca, P. Wojnar and P. Kossacki. Temperature of a single Mn atom in a CdTe quantum dot. Acta PhysicaPolonica A 116, 899 (2009).[82] A. Patane, W. H. M. Feu, O. Makarovsky, O. Drach<strong>en</strong>ko, L. Eaves, A. Krier, Q. D. Zhuang, M. Helm, M. Goiran and G. Hill.Effect of low nitrog<strong>en</strong> conc<strong>en</strong>trations on the electronic properties of InAs 1−x N x . Physical Review B 80, 115207 (2009).[83] O. Pauvert, F. Fayon, A. Rakhmatullin, S. Kraemer, M. Horvatic, D. Avignant, C. Berthier, M. Deschamps, D. Massiot andC. Bessada. Zr-91 Nuclear Magnetic Resonance Spectroscopy of Solid Zirconium Hali<strong>des</strong> at High Magnetic Field. InorganicChemistry 48, 8709 (2009).[84] M. L. Peres, V. A. Chitta, N. F. Oliveira, Jr., D. K. Maude, P. H. O. Rappl, A. Y. Ueta and E. Abramof. Antilocalization of holecarriers in Pb 1−x Eu x Te alloys in the metallic regime. Physical Review B 79, 085309 (2009).[85] A. P. Petrović, Y. Fasano, R. Lortz, C. S<strong>en</strong>atore, A. Demuer, A. B. Antunes, A. Paré, D. Salloum, P. Gougeon, M. Potel andO. Fischer. Real-space vortex glass imaging and the vortex phase diagram of SnMo 6 S 8 . Physical Review Letters 103, 257001(2009).[86] B. A. Piot, C. R. Dean, G. Gervais, Z. Jiang, L. W. Engel, L. N. Pfeiffer and K. W. West. Distortion of the 2D Wigner crystalinto a ’quasi-3D’ insulator. International Journal of Modern Physics B 23, 2713 (2009). 18th International Confer<strong>en</strong>ce on HighMagnetic Fields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[87] B. A. Piot, D. K. Maude, U. G<strong>en</strong>nser, A. Cavanna and D. Mailly. Interplay among spin, orbital effects, and localization in a GaAstwo-dim<strong>en</strong>sional electron gas in a strong in-plane magnetic field. Physical Review B 80, 115337 (2009).[88] P. Plochocka, P. Kossacki, A. Golnik, T. Kazimierczuk, C. Berger, W. A. de Heer and M. Potemski. Slowing hot-carrier relaxationin graph<strong>en</strong>e using a magnetic field. Physical Review B (Cond<strong>en</strong>sed Matter and Materials Physics) 80, 245415 (2009).[89] P. Plochocka, J. M. Schneider, D. K. Maude, M. Potemski, M. Rappaport, V. Umansky, I. Bar-Joseph, J. G. Groshaus, Y. Gallaisand A. Pinczuk. Optical absorption to probe the quantum Hall ferromagnet at filling factor ν = 1. Physical Review Letters 102,126806 (2009).[90] M. Potemski. Landau level spectroscopy of dirac-like fermions in multilayer graph<strong>en</strong>e. International Journal of Modern PhysicsB 23, 2665 (2009). 18th International Confer<strong>en</strong>ce on High Magnetic Fields in Semiconductor Physics and Nanotechnology, SaoPedro, BRAZIL, AUG 03-08, 2008.[91] V. Preisler, T. Grange, R. Ferreira, L. A. de Vaulchier, Y. Guldner, F. J. Teran, M. Potemski and A. Lemaitre. Investigationof interband optical transitions by near-resonant magneto-photoluminesc<strong>en</strong>ce in InAs/GaAs quantum dots. European PhysicalJournal B 67, 51 (2009).[92] G. Pristas, M. Reiffers, E. Bauer, A. G. M. Jans<strong>en</strong> and D. K. Maude. Suppression of asymmetric differ<strong>en</strong>tial resistance in th<strong>en</strong>on-Fermi-liquid system YbCu 5−x Al x (x=1.3-1.75) in high magnetic fields. Physical Review B 78, 235108 (2008).[93] C. Proust and D. Poilblanc. Des champs magnétiques int<strong>en</strong>ses pour sonder les supraconducteurs. Images de la Physique 87–92(2008).[94] G. Quirion, M. L. Plumer, O. A. Petr<strong>en</strong>ko, G. Balakrishnan and C. Proust. Magnetic phase diagram of magnetoelectric CuFeO 2in high magnetic fields. Physical Review B 80, 064420 (2009).[95] C. Robilliard, B. Pinto Da Souza, F. Bielsa, J. Mauchain, M. Nardone, G. Bailly, M. Fouche, R. Battesti and C. Rizzo. The BMVproject: Search for photon oscillations into massive particles. Canadian Journal of Physics 87, 735 (2009).[96] V. V. Rylkov, B. A. Aronzon, A. S. Lagutin, V. V. Podol’skii, V. P. Lesnikov, M. Goiran, J. Galibert, B. Raquet and J. Leotin.Transport features in laser-plasma-deposited InMnAs layers in strong magnetic fields. Journal of Experim<strong>en</strong>tal and TheoreticalPhysics 108, 149 (2009).[97] J. M. Schneider, M. Orlita, M. Potemski and D. K. Maude. Consist<strong>en</strong>t Interpretation of the Low-Temperature Magnetotransport inGraphite Using the Slonczewski-Weiss-McClure 3D Band-Structure Calculations. Physical Review Letters 102, 166403 (2009).[98] J. Shaver, A. N. G. Parra-Vasquez, S. Hansel, O. Portugall, C. H. Mielke, M. von Ort<strong>en</strong>berg, R. H. Hauge, M. Pasquali andJ. Kono. Alignm<strong>en</strong>t dynamics of single-walled carbon nanotubes in pulsed ultrahigh magnetic fields. Acs Nano 3, 131 (2009).[99] J. Shaver, A. Srivastava, J. Kono, S. A. Crooker, H. Htoon, V. I. Klimov, J. A. Fagan, E. K. Hobbie, N. Ubrig, O. Portugall,V. Perebeinos and P. H. Avouris. High field magneto-optical spectroscopy of highly aligned individual and <strong>en</strong>semble single-walledcarbon nanotubes. International Journal of Modern Physics B 23, 2667 (2009).[100] N. Silva, A. Millán, F. Palacio, E. Kampert, U. Zeitler, H. Rakoto and V. Amaral. Temperature dep<strong>en</strong>d<strong>en</strong>ce of antiferromagneticsusceptibility in ferritin. Physical Review B 79, 104405 (2009).145


PUBLICATIONS 2009[101] R. Stoyanova, A. L. Barra, E. Zhecheva, R. Alcantara, G. Ortiz and J.-L. Tirado. Local Coordination of Fe 3+ in LayeredLiCo 1−y Al y O 2 Oxi<strong>des</strong> Determined by High-Frequ<strong>en</strong>cy Electron Paramagnetic Resonance Spectroscopy. Inorganic Chemistry48, 4798 (2009).[102] P. Strobel, H. Muguerra, S. Hebert, E. Pachoud, C. Colin and M.-H. Juli<strong>en</strong>. Effect of ruth<strong>en</strong>ium substitution in layered sodiumcobaltate Na x CoO 2 : Synthesis, structural and physical properties. Journal of Solid State Chemistry 182, 1872 (2009).[103] L. Thilly, S. Van Petegem, P. O. R<strong>en</strong>ault, F. Lecouturier, V. Vidal, B. Schmitt and H. Van Swyg<strong>en</strong>hov<strong>en</strong>. A new criterion for elastoplastictransition in nanomaterials: Application to size and composite effects on Cu-Nb nanocomposite wires. Acta Materialia57, 3157 (2009).[104] C. A. Thues<strong>en</strong>, A.-L. Barra and J. Glerup. Single crystal electron paramagnetic resonance spectra of CS 2 MnF 6 and K 2 MnF 6diluted in the isomorphous germanium salts. Inorganic Chemistry 48, 3198 (2009).[105] T. D. Tzima, G. Sioros, C. Duboc, D. K. Demertzi, V. S. Melissas and Y. Sanakis. Multifrequ<strong>en</strong>cy electron paramagnetic resonanceand theoretical studies of a mn(II) (S = 5/2) complex. the role of geometrical elem<strong>en</strong>ts on the zero field splitting parameters.Polyhedron 28, 3257 (2009).[106] M. Vachon, S. Raymond, A. Babinski, J. Lapointe, Z. Wasilewski and M. Potemski. Energy shell structure of a single InAs/GaAsquantum dot with a spin-orbit interaction. Physical Review B 79, 165427 (2009).[107] L. Van Khoi, A. Avdonin, R. Szymczak, R. R. Galazka and M. Potemski. Electroluminesc<strong>en</strong>ce and positive magnetoresistanc<strong>en</strong>ear the curie-weiss temperature in the Zn 1−x Mn x Te light emitting devices. Journal of Applied Physics 106, 036102 (2009).[108] L. Van Khoi, A. Avdonin, R. Szymczak, R. R. Galazka and M. Potemski. Magnetoresistance and electroluminsc<strong>en</strong>ce near thecurie-weiss temperature in the Zn 1−x Mn x Te light emitting devices. Acta Physica Polonica A 116, 941 (2009).[109] V. Vidal, L. Thilly, S. Van Petegem, U. Stuhr, F. Lecouturier, P. O. R<strong>en</strong>ault and H. Van Swyg<strong>en</strong>hov<strong>en</strong>. Plasticity of nanostructuredCu-Nb-based wires: Str<strong>en</strong>gth<strong>en</strong>ing mechanisms revealed by in situ deformation under neutrons. Scripta Materialia 60, 171 (2009).[110] D. Vignolles, A. Audouard, V. N. Laukhin, E. Canadell, T. Prokhorova and E. B. Yagubskii. Indications for the coexist<strong>en</strong>ce ofclosed orbit and quantum interferometer with the same cross section in the organic metal β”-(ET) 4 (H 3 O)[Fe(C 2 O 4 ) 3 ]·C 6 H 4 Cl 2 :Persist<strong>en</strong>ce of Shubnikov-de Haas oscillations above 30 K. European Physical Journal B 71, 203 (2009).[111] D. Vignolles, A. Audouard, V. N. Laukhin, M. Nardone, E. Canadell, N. G. Spitsina and E. B. Yagubskii. Magnetic oscillationsamplitude of a dirty quasi two-dim<strong>en</strong>sional organic metal. Synthetic Metals 158, 973 (2008).[112] D. Vignolles, A. Audouard, R. B. Lyubovskii, M. Nardone, E. Canadell, E. I. Zhilyaeva and R. N. Lyubovskaya. ShubnikovdeHaas oscillations spectrum of the strongly correlated quasi-2D organic metal (ET) (8) [Hg 4 Cl 12 (C 6 H 5 Br) (2) ] under pressure.European Physical Journal B 66, 489 (2008).[113] G. Wagnières and G. Rikk<strong>en</strong>. Chirality and magnetism: Free electron on an infinite helix,ncd,mcd,and magnetochiral dichroism.Chem. Phys. Lett. 481, 166 (2009).[114] O. Waldmann, T. C. Stamatatos, G. Christou, H. U. Guedel, I. Sheikin and H. Mutka. Quantum Phase Interfer<strong>en</strong>ce and Neel-Vector Tunneling in Antiferromagnetic Molecular Wheels. Physical Review Letters 102, 157202 (2009).[115] D. Wang, Y. Ma, Z. Gao, X. Zhang, L. Wang, E. Mossang, G. Nishijima, S. Awaji and K. Watanabe. Enhancem<strong>en</strong>t of the High-Field J (c) properties of MgB 2 /Fe Tapes by Acetone Doping. Journal of Superconductivity and Novel Magnetism 22, 671 (2009).[116] D. Wang, X. Zhang, Z. Gao, L. Wang, Y. Ma, S. Awaji, G. Nishijima, K. Watanabe and E. Mossang. Effect of processingtemperature on the superconducting properties of acetone doped MgB 2 tapes. Physica C-Superconductivity and its Applications469, 23 (2009).[117] H. Weihe, S. Piligkos, A. L. Barra, I. Laurs<strong>en</strong> and O. Johns<strong>en</strong>. EPR of Mn 2+ impurities in calcite: a detailed study pertin<strong>en</strong>t tomarble prov<strong>en</strong>ance determination. Archaeometry 51, 43 (2009).[118] S. Wiedmann, G. M. Gusev, O. E. Raichev, A. K. Bakarov and J. C. Portal. High-order fractional microwave-induced resistanceoscillations in two-dim<strong>en</strong>sional systems. Physical Review B 80, 035317 (2009).[119] S. Wiedmann, G. M. Gusev, O. E. Raichev, T. E. Lamas, A. K. Bakarov and J. C. Portal. Magnetoresistance oscillations in doublequantum wells under microwave irradiation. International Journal of Modern Physics B 23, 2943 (2009). 18th InternationalConfer<strong>en</strong>ce on High Magnetic Fields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[120] S. Wiedmann, N. C. Mamani, G. M. Gusev, O. E. Raichev, A. K. Bakarov and J. C. Portal. Magnetoresistance oscillations inmultilayer systems: Triple quantum wells. Physical Review B (Cond<strong>en</strong>sed Matter and Materials Physics) 80, 245306 (2009).[121] A. Wojs, L. Bryja and M. Potemski. Effects of ionized impurities on binding and recombination of positive and negative quasitwo-dim<strong>en</strong>sionalmagneto-trions. International Journal of Modern Physics B 23, 2964 (2009). 18th International Confer<strong>en</strong>ce onHigh Magnetic Fields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[122] A. Wysmolek, M. Kaminska, A. Twardowski, M. Potemski, M. Bockowski and I. Grzegory. Magneto-luminesc<strong>en</strong>ce of gadoliniumdoped gallium nitride. International Journal of Modern Physics B 23, 2994 (2009). 18th International Confer<strong>en</strong>ce on HighMagnetic Fields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[123] A. Wysmolek, R. Stepniewski, K. Wardak, J. Baranowski, M. Potemski, E. Tymicki and K. Grasza. 1.4 eV - luminesc<strong>en</strong>ce bandin 6h-SiC: symmetry of the associated defect. International Journal of Modern Physics B 23, 3019 (2009). 18th InternationalConfer<strong>en</strong>ce on High Magnetic Fields in Semiconductor Physics and Nanotechnology, Sao Pedro, BRAZIL, AUG 03-08, 2008.[124] S. Yoshii, K. Ohoyama, K. Kurosawa, H. Nojiri, M. Matsuda, P. Frings, F. Duc, B. Vignolle, G. L. J. A. Rikk<strong>en</strong>, L. P. Regnault,S. Michimura and F. Iga. Neutron diffraction study on the multiple magnetization plateaus in TbB 4 under pulsed high magneticfield. Physical Review Letters 103, 077203 (2009).[125] X. Zhang, Y. Ma, D. Wang, Z. Gao, L. Wang, Y. Qi, S. Awaji, K. Watanabe and E. Mossang. Phthalocyanine doping to improvecritical curr<strong>en</strong>t d<strong>en</strong>sities in MgB 2 tapes. Superconductor Sci<strong>en</strong>ce and Technology 22, 045019 (2009).[126] A. Zorko, S. Nellutla, J. van Tol, L. C. Brunel, F. Bert, F. Duc, J.-C. Trombe and P. M<strong>en</strong>dels. Electron spin resonance investigationof the spin-1/2 kagomé antiferromagnet ZnCu 3 (OH) 6 Cl 2 . Journal of Physics : Confer<strong>en</strong>ce Series 145, 012014 (2009).146


Contributors of the LNCMI to the Pres<strong>en</strong>t ReportAMANDO M. : 16, 17ANTUNES A.B. : 55, 66, 80, 81, 86, 91, 92, 93, 94AUDOUARD A. : 68, 69, 70AUTERNAUD C. : 115, 117BARRA A.L. : 15, 98, 127BATTESTI R. : 125BÉARD J. : 119BENDICHOU L. : 120BERCEAU P. : 125BERTHIER C. : 60, 62, 82, 83, 126BIELSA F. : 125BILLETTE J. : 119BREFUEL N. : 97BROTO J.M. : 7, 8, 9, 19, 43, 46, 52, 77DAUZHENKA T.A. : 6, 48DEBRAY F. : 104, 107, 108, 109, 110, 111, 115, 116, 117,122, 123DE VALLÉE C. : 126DOMPS J.P.: 104, 123DUBOIS J.B. : 120DUC F. : 70, 84, 85DUFRESNES S. : 104, 123DUMAS J. : 115, 116, 117, 122DURANTEL F. : 121ESCOFFIER W. : 7, 8, 9, 13, 19FAUGERAS C. : 12, 15, 16, 17, 18, 23, 24, 39FERREIRA N. : 120FLORENTIN J. : 127FRINGS P. : 84, 118, 119GALIBERT J. : 6, 48GEORGE S. : 5, 43, 46, 52, 77GIQUEL F. : 119GOIRAN M. : 9, 19, 45GORYCA M. : 51GRIFFE B. : 118GUILLOT M. : 87, 88, 89, 90, 128HORVATIC M. : 60, 62, 82, 83, 126JAUDET C. : 61JOSS W. : 72,73, 124KAMKE M. : 115, 117KLEIN Y. : 61KNAFO W. : 59, 61KOSSACKI P. : 10, 16, 17, 22, 51KOWALIK K. : 29KRÄMER S. : 83, 126KUNC J. : 29, 50KUMAR A. : 13LABBE-LAVIGNE S. : 116LAGARRIGUE J.-M. : 119, 120LECOUTURIER F. : 120LEOTIN J. : 52, 45MALONE L. : 66MARTINEZ G. : 23, 24, 39MATERA J. : 115, 122MAUCHAIN J. : 119, 125MAUDE D.K. : 11, 12, 14, 20, 21, 23, 24, 27, 28, 29, 30,44, 47, 49, 50, 57, 79MILLOT M. : 43, 45, 46, 52, 77MOLLARD C. : 115MOSSANG E. : 101, 102, 103, 104, 123NANOT S. : 7, 8NARDONE M. : 70NEUGEBAUER P. : 15, 98, 127NICOLIN J.-P. : 118ORLITA M. : 15, 17, 18, 20, 21, 22, 23, 24, 39, 50, 78PARDO B. : 115, 117PIOT, B.A. : 12, 28, 30, 57PFISTER R. : 115, 116, 117, 122, 124PLOCHOCKA P. : 10, 22, 27, 29, 51PONTON D. : 115PORTAL J.C. : 31 32, 33, 34, 35, 36, 37, 38, 40PORTUGALL O. : 5, 22, 121POTEMSKI M. : 10, 12, 15, 16, 17, 18, 20, 21, 23, 24,27, 29, 51POUMIROL J.M. : 9, 13, 19, 45PROUST C. : 55, 56, 61, 67, 65PUGNAT P. : 124RAQUET B. : 7, 8, 9, 19RIBEIRO R. : 13RIKKEN G.L.J.A. : 22, 84RONAYETTE L. : 124SCHIAVO T. : 118SCHNEIDER J.M. : 20, 21, 23, 24SHEIKIN I. : 55, 58, 59, 63, 64, 71, 81, 83SOLANE P.Y. : 121SPITZNAGEL J. : 115, 126STORK H. : 126TERAN F.J. : 29TROPHIME C. : 115, 116, 117, 122UBRIG N. : 5, 22VERNEY E. : 115, 117VEYS S. : 115VIDAL N. : 115, 116, 117, 122VIGNOLLE B. : 56, 61, 65, 67, 84VIGNOLLES D. : 61, 65, 69, 70WIEDMANN S. : 31, 32, 33, 34, 35, 36, 37, 38, 40


Collaborating External LaboratoriesAlgeriaFluids Mechanics Laboratory, University of USTHB, Algiers : 108BelarusBelarus State University, Dept Phys. SC & Nanoelectronics, BY-Minsk : 48Belarus State Univ. Research Institute of Physicochemical Problems, BY-Minsk: 48BrazilEPUSP- Escola Politécnica da Universidade de São Paulo, São Paulo : 49Federal University of São Carlos : 50Instituto de Física da Universidade de São Paulo : 31, 32, 33, 34, 35, 36, 37CanadaInstitute of Microstructural Sci<strong>en</strong>ces, NRC, Ottawa : 28, 39University of British Columbia, Vancouver : 55University of Sherbrooke : 55, 78ChileDepartam<strong>en</strong>to de Química, Facultad de Ci<strong>en</strong>cias, Universidad de Chile, Santiago : 92Instituto de Ci<strong>en</strong>cias Básicas, Universidad Católica del Maule, Talca : 92Facultad de Ci<strong>en</strong>cias Químicas, Universidad de Concepción, Concepción : 94ChinaBeijing <strong>National</strong> Laboratory for Cond<strong>en</strong>sed Matter Physics : 60China Northwest Institute for Non-Ferrous Metal Research, Xi’an: 102Institute of Physics, Chinese Academy of Sci<strong>en</strong>ce, Beijing : 60Institute of Electrical Engineering, Chinese Academy of Sci<strong>en</strong>ces, Beijing : 103University of Shanghai, Shanghai : 111Czech RepublicAcademy of Sci<strong>en</strong>ce, Prague : 21, 128FranceAlstom, Belfort : 124CEA-DEN-LTMEX, Saclay : 120CEA, DRFMC-SPSMS-MDN, Gr<strong>en</strong>oble : 84CEA, IRFU, Saclay : 123CEA-IRFU-SACM, Saclay : 120CEA, Saclay : 124CEMHTI-CNRS, Orléans : 126Commissariat à l’Energie Atomique, CEA-Gr<strong>en</strong>oble : 59, 61, 63Commissariat à l’Energie Atomique, INAC, SP2M, Gr<strong>en</strong>oble : 7, 9CMTR, ICMPE, CNRS, Thiais : 90CRETA, CNRS, Gr<strong>en</strong>oble : 107DSM-DAPNIA-SACM, CEA Saclay : 104EPM-SIMAP Laboratory, Gr<strong>en</strong>oble : 108ESPCI, Paris : 55, 66, 67European Synchrotron Radiation Facility, Gr<strong>en</strong>oble : 84, 116GES-UM2, Montpellier : 28, 44IMEP, Gr<strong>en</strong>oble : 49INAC, SPSMS, CEA Gr<strong>en</strong>oble : 62


Institut Jean Lamour, Nancy : 68Institut Laue Langevin, Gr<strong>en</strong>oble : 116Institut Néel, Gr<strong>en</strong>oble : 88, 89, 93, 102, 104, 123, 128INP, Gr<strong>en</strong>oble : 123<strong>Laboratoire</strong> Collisions Agrégats Réactivité, Toulouse : 125<strong>Laboratoire</strong> de Photonique et de Nanostructures, Marcoussis : 30<strong>Laboratoire</strong> de Spectrométrie Physique, Université J. Fourier, Gr<strong>en</strong>oble : 60LEGI CNRS, INP, UJF, Gr<strong>en</strong>oble : 117LGIT/CNRS/OSUG/UJF, Gr<strong>en</strong>oble : 109LPEC, Universit du Maine, Le Mans : 87LPSC, CNRS, Gr<strong>en</strong>oble : 116, 122PHYMAT, Poitiers : 120SERAS, CNRS, Gr<strong>en</strong>oble : 115, 117Sci<strong>en</strong>ces Chimiques de R<strong>en</strong>nes, Université de R<strong>en</strong>nes 1, R<strong>en</strong>nes : 91, 92, 93, 94SIMAP, EPM, CNRS, Gr<strong>en</strong>oble : 111Université Joseph Fourier, Gr<strong>en</strong>oble : 88, 89, 128Université de Nice, Nice : 18University of Paris XII, Thiais: 90University of R<strong>en</strong>nes : 97University of Toulouse : 97GermanyApplied Physics Departm<strong>en</strong>t, University of Erlang<strong>en</strong>-Nürnberg : 11Forschungsz<strong>en</strong>trum Jülich GmbH, Jülich : 86Humboldt-Universitt, Berlin : 52Physikalisches Institut, Universität Karlsruhe : 82TU Braunschweig, Institute for Physics of Cond<strong>en</strong>sed Matter, Braunschweig : 64University of Karlsruhe : 81University of Stuttgart : 81Walther-Meissner-Institut, Garching : 58Hong KongThe Hong Kong University of Sci<strong>en</strong>ce and Technology, Kowloon : 71IsraelThe Institute of Superconductivity, Departm<strong>en</strong>t of Physics, Bar-Ilan University, Ramat-Gan : 72, 73The Racah Institute of Physics, The Hebrew University of Jerusalem, Jerusalem : 72, 73Weizmann Institute, Rehovot : 27ItalyCNR-INFM LAMIA, G<strong>en</strong>ova : 101Columbus Superconductors S.p.A., G<strong>en</strong>ova : 101Universitá degli studi di Pavia : 14University of Flor<strong>en</strong>ce : 81, 98University of Mod<strong>en</strong>a : 98JapanInstitute for Materials Research, Tohoku University, S<strong>en</strong>dai : 84, 103ISSP, University of Tokyo : 83JAEA, Tokai : 84Nihon University, Tokyo : 71University of Kumamoto : 97University of Kyoto : 83, 65, 97University of Osaka, Osaka : 71, 65University of Tokyo, Kashiwa : 55


LithuaniaSC Institute LI-Vilnius : 6PolandAGH University of Sci<strong>en</strong>ce and Technology, Krakow : 110Institute of Experim<strong>en</strong>tal Physics, Warsaw University : 10, 44, 51Institute of High Pressure Physics, Warsaw : 44Institute of Physics Polish Academy of Sci<strong>en</strong>ce, Warsaw : 29, 51, 79, 80RussiaInstitute of G<strong>en</strong>eral and Inorganic Chemistry, Russian Academy of Sci<strong>en</strong>ce, Moscow : 79Institute of Microelectronics Technology of RAS, Chernogolovka, Moscow district : 40Institute of Semiconductor Physics, Novosibirsk : 31, 32, 33, 34, 35, 36, 37, 38IPCP, Chernogolovka, Russian Federation : 69, 70G<strong>en</strong>eral Physics Institute of the Russian Academy of Sci<strong>en</strong>ces, Moscow : 78Moscow Power Engineering Institute, Moscow : 78P.N. Lebedev Physical Institute, Russian Academy of Sci<strong>en</strong>ce, Moscow : 57SpainCT-ISOM, Universidad Politécnica de Madrid : 14DCITIMAC, Santander : 43, 52, 77Electrocerámicas, Instituto de Cerámica y Vidrio, CSIC, Madrid : 91, 93ESI, Bilbao : 77ICMAB, Barcelona : 69, 70ICMUV, Val<strong>en</strong>cia : 46Laboratorio de bajas temperaturas, Universidad de Salamanca : 14SwitzerlandEMPA, Düb<strong>en</strong>dorf : 77EPFL, Lausanne : 83POLDI-Paul Scherrer Institut : 120EPFL, Switzerland : 8The NetherlandsHMFL, Nijmeg<strong>en</strong> : 65MESA+, Enschede : 77UkraineInstitute of Materials Sci<strong>en</strong>ce Problems, Ukrainian Academy of Sci<strong>en</strong>ces, Chernovtsy : 80Institute of Semiconductor Physics, NAS of Ukraine, Kiev : 31, 32, 33, 34, 35, 36, 37United KingdomSchool of Physics and Astronomy, University of Leeds : 47School of Physics and Astronomy, University of Nottingham : 50University of Bristol, Bristol : 56, 65University of Edinburgh, Edinburgh : 85University of Manchester, Manchester : 18USABrown University, Provid<strong>en</strong>ce : 62C<strong>en</strong>ter for Microwave Magnetic Materials and Integrated Circuits, Northeastern University, Boston : 87Columbia University, New York : 27Georgia Tech., Atlanta : 10, 12, 16, 17, 24Garcia c<strong>en</strong>ter Polymers at Engineered Interfaces, Stony Brook Univ. NY : 6


Lawr<strong>en</strong>ce Berkeley <strong>National</strong> Laboratory, Berkeley : 45Physics departm<strong>en</strong>t and Chemistry Laboratory, Stanford : 9Rice University : 5RoseStreet Labs Energy, Pho<strong>en</strong>ix : 45


<strong>Champs</strong> magnétiques continusLNCMI-G, CNRS25 rue <strong>des</strong> Martyrs, B.P. 16638042 GRENOBLE cedex 9 - FranceTél. : +33 (0)4 76 88 10 48Fax : +33 (0)4 76 88 10 01Couriel : lncmi.direction@gr<strong>en</strong>oble.cnrs.fr<strong>Champs</strong> magnétiques pulsésLNCMI-T, CNRS143 av<strong>en</strong>ue de Rangueil31400 TOULOUSE - FranceTel. : +33 (0)5 62 17 28 60Fax:+33(0)562172816Couriel : g<strong>en</strong>eral@lncmp.org

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