ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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Hard Coatings and Vapor Deposition Technology Room: Royal Palm 4-6 - Session B3-1 Ion-Surface Interactions in Film Growth and Post- Growth Processes Moderator: S. Fairchild, Air Force Research Laboratory, US, K. Sarakinos, Linköping University, Sweden 8:00am B3-1-1 Tantalum Based Coatings Deposited by Pulsed DC Magnetron Sputtering and Highly Ionized Pulse Plasma Processes, J. Barriga (jbarriga@tekniker.es), L. Mendizabal, U. Ruiz de Gopegui, R. Bayon, Tekniker, Spain Transition metals and their nitrides are widely used in the industry as protective coatings because of their excellent tribological properties. Among them, tantalum (Ta) demonstrated to provide high wear protection [1] as well good corrosion resistance and biocompatibility [2]. However, there are only a few studies up to date about tribological analysis of coatings based on this metal. This could be due to the difficulty in evaporating Ta in Physical Vapor Deposition systems because its relatively low thermal and electrical conductivity and high fusion temperature. In this work three different evaporation techniques are used and compared. All of them are varieties of Magnetron Sputtering: pulsed DC, HiPIMS (High Power Impulse MS) and MPP (Modulated Power Pulse). With these last two techniques there is a potential improvement on coating quality because during the evaporation process we have peaks of high power density increasing the ionization, density of the coating, adhesion and wear resistance [3]. We have seen that h igh power techniques (HiPIMS and MPP) enhance the hardness of TaN coatings compared to conventional Pulsed DC MS. The interface TaN with stainless steel is denser with MPP technique and better adhesion of the coating is achieved. In corrosion tests all samples show passive behavior and low corrosion currents in the anodic branch. TaN by HiPIMS showed the highest corrosion resistance which increased when increasing the immersion time due to its denser microstructure and the stable electrochemical behavior of its passive film formed in PBS solution. [1] J. Esteve, E. Martínez, A. Lousa, F. Montalà, L.L. Carreras, “Microtribological characterization of group V and VI metal-carbide wearresistant coatings effective in the metal casting industry”, Surf. Coat. Technol. 133–134 (2000) 314–318. [2] J. Black, "Biological performance of tantalum". Clin. Mater. 16 (3): 167–173. (1994). doi:10.1016/0267-6605(94)90113-9. [3] A.P. Ehiasarian, book chapter: “Fundamentals and Applications of High Power Impulse Magnetron Sputtering”, Plasma Surface Engineering Research and its Practical Applications, p. 35 – 86 (2007), ISBN 978-81- 308-0257-2. 8:20am B3-1-2 Studies on plasma immersion ion implantation of nitrogen on titanium, K. R. M. Rao (rammohanrao.k@gmail.com), Department of Engineering Chemistry, GITAM Institute of Technolocgy, GITAM University, India, E. Richter, Institute of Ion Beam Physics for Materials Research, Helmholtz-Zentrum Dresden-Rossendorf, Germany, S. Mukherjee, FCIPT,Institute of Plasma Research, India, I. Manna, Central Glass and Ceramic Research Institute, India Abstract Formation of titanium nitride layer by following plasma immersion ion implantation (PIII) has been investigated at variable energies. For PIII experiments, square shaped commercially pure Ti samples of 1 mm thickness and 100 mm 2 area were mirror polished by standard metallographic techniques using 10-0.1 μm sized diamond paste. PIII was performed at variable negative bias without auxiliary heating. PIII chamber was first evacuated to 2 x 10 -3 Pa, then back filled with dehumidified N2 gas to 0.4 Pa pressure. Nitrogen plasma was created by a radio frequency (13.56 MHz) coupled generator operated at 400 W. N2 + ion implantation from this RF coupled N2 + with 10 21 ions/m 2 was carried out at variable energy. Post implanted specimens were examined by X-ray diffraction (XRD) and Scanning Electron Microscope (SEM) for phase analysis and surface topography respectively. X-ray diffraction (GAXRD) using Cu-ka radiation (0.154 nm). All of them reflected the signature of the usual peaks of Ti along with TiN111. The volume fraction of TiN seems to be directly related to the implantation voltage. Moreover, the surface modified samples were exposed to Hank’s solution as the corrosive medium for the assessment of corrosion resistance properties. Friday Morning, April 27, 2012 Friday Morning, April 27, 2012 128 These samples were subjected to potentiodynamic polarization tests at 1 mV/sec scan rate and compared with respect to their polarization characteristics. Since TiN phase has been found in almost all the treatment conditions the enhancement in corrosion resistance may be attributed to the presence of titanium nitride covered on the surface layer. It has also been found that the corrosion resistance was higher at higher implantation voltage. The best condition of PIII for the corrosion resistance in Hank’s solution was found to be at a dose 2.4 x 10 21 ions/m 2 . 8:40am B3-1-3 On the role of ions during reactive magnetron sputtering, D. Depla (Diederik.Depla@ugent.be), Ghent University, Belgium INVITED Ions play an prominent role during reactive magnetron sputtering. Their influence can be quite explicit as for example when a substrate bias is applied during thin film growth. However, ions can also play a more hidden role. This paper aims to give an overview of the different processes in which ions play a key role. The first, and most obvious during magnetron sputtering, is of course the sputter process as such. Although it seems straightforward to describe this, fundamental issues as the angular emission profile, compound sputter yield hampers a quantitative description of the deposition profile, and therefore the deposition rate at the substrate[1]. A similar question exists about the role of ions during the sustaining mechanism of the magnetron discharges. In recent years, substantial progress has been in the understanding of the behaviour of the electron emission yield when oxidizing the target[2]. As the latter behaviour also influences the emission of negative oxygen ions, a good understanding is needed because high energetic negative oxygen ions affect in an important way thin film growth. A few examples of this behaviour will be given[3]. As the ions bombard the target, they also become implanted. For inert gas atoms, their influence is minor. However, reactive ion implantation is an important pathway in the poisoning mechanism during reactive magnetron sputtering[4]. The paper will discuss the latest trends in the modelling of this process. Finally, ions can be used as a tool to influence the thin film growth. As they are charged species, their energy can easily be influenced by biasing the substrate. Moreover, they can also be guided towards the substrate. This approach becomes even more interesting when most of the metal species are ionized as in HIPIMS plasmas. However, when studying thin film growth, one must realize that not only the ions are important, and other species play also their role. This will be discussed in the context of the characterisation of the different particle fluxes from the plasma towards the substrate [5]. [1] F Boydens, W P Leroy, R Persoons and D Depla, Submitting for publication to Physica status Solidi a [2] D Depla, S Mahieu, R.De Gryse, Thin Solid Films 517 (2009) 2825 [3] S Mahieu, WP Leroy, K Van Aeken, D Depla, JAP 106 (2009) 093302 [4] D. Depla, X. Y. Li, S. Mahieu,K. Van Aeken,W. P. Leroy, J. Haemers, R. De Gryse, A. Bogaerts, JAP 107 (2010) 0113307 [5] S Mahieu, WP Leroy, K Van Aeken, M Wolter, J Colaux, S Lucas, G Abadias, P Matthys, D Depla, Solar Energy 85 (2011) 538 9:20am B3-1-5 In situ characterization of plasma-surface interactions with a quartz crystal microbalance, C. Corbella (carles.corbella@rub.de), O. Kreiter, S. Grosse-Kreul, Ruhr Universität Bochum, Germany, D. Marinov, Ecole Polytechnique, France, T. de los Arcos, A. von Keudell, Ruhr Universität Bochum, Germany Particle beam experiments were conducted in an ultra-high-vacuum (UHV) vessel and monitored in real time by means of a quartz crystal microbalance (QCM). Several atom and ion guns were focused to the QCM and sent controlled fluxes of particle beams constituted by different elements. The UHV was achieved by using a turbomolecular pump in combination with an ion-getter-pump. First, the study of ion-enhanced oxidation of aluminium targets during reactive magnetron sputtering was performed by bombarding an Al-coated QCM with argon ions and oxygen atoms. An effusion cell provided Al vapour to restore the metallicity of the QCM. Second, beams of argon ions, together with oxygen and hydrogen species, were used to investigate the chemical sputtering of diamond-like carbon (DLC) films during plasma etching processes. For this purpose, we deposited DLC thin films on the QCM. Finally, remote plasmas interacted with the QCM to promote the physisorption/chemisorption of nitrogen atoms on SiO2 surfaces. The treated surfaces were studied by X-ray photoelectron spectroscopy (XPS). These experiments shed some light into fundamental plasma-surface processes taking place in industrial plasma applications.
9:40am B3-1-6 Compressive stress generation and atom incorporation during growth of low-mobility materials, G. Abadias (gregory.abadias@univ-poitiers.fr), A. Fillon, A. Michel, C. Jaouen, Institut P' - Universite de Poitiers, France The incorporation of growth-induced defects from energetic deposited particles during sputter-deposition, known as the “atomic peening” effect, is revisited in low-mobility material thin films by combining in situ and realtime wafer curvature and ex situ X-ray diffraction techniques. A series of metastable Mo1-xSix solid solution films were deposited by magnetron sputtering at low pressure (0.12 Pa) in Ar plasma discharge onto crystalline (110) Mo template layers. Unbalanced magnetron configuration and substrate bias voltages up to -120V were used to increase the contribution of energetic ions to the total deposited energy. The stress evolution was monitored in real-time using a multiple-beam optical stress sensor (MOSS) designed by kSA and implemented in the deposition chamber. The stress-field was determined from XRD using the sin 2 ψ technique adapted for the case of textured/epitaxial layers. Post-growth ion irradiation using 310 keV Ar + ions at low dose(< 0.2 dpa) were carried out to identify the nature of point-defects and associated stress field. Compressive stress evolution due to atomic peening is observable only above a first critical energy threshold. The stress-field appears in that case fully biaxial. Grain-size dependence of stress confirms that defect creation is confined to the grain boundaries. Further increase of the deposited energy, above a second threshold, results in the creation of additional volume defects inside the grains, i.e. expansion of the unit cell. Examination of sin 2 ψ plots evolution on irradiated films shows that defects incorporated in the grain boundaries are stable, while those created inside the grain are highly unstable. In a deposited-energy/composition space diagram, these thresholds depict the existence of biaxial or hydrostatic stress domains related to these two distinct defect creation mechanisms. The strong variation of the critical energy thresholds with the Si content points out the sensitivity of defects creation to the intrinsic properties of the material. 10:00am B3-1-7 Variation of substrate biasing and temperature and their influence on the crystal orientation of γ-Al2O3 films, M. Prenzel (marina.prenzel@rub.de), A. Kortmann, A. von Keudell, Ruhr Universität Bochum, Germany Temperature and substrate bias play a key role in the structural evolution of aluminium oxide (Al2O3) during the deposition process. On the one hand, crystallinity depends on the mobility of the particles in the growing film, which is influenced by the substrate temperature. On the other hand, correct tailoring of the substrate bias allows to selectively control the energy distribution function of the ions impinging on the substrate (IEDF). Thus, film characteristics such as hardness, adhesion, crystallinity, or wear resistance can be controlled. In this work, manipulation of the substrate bias is performed by variation of the frequency, amplitude and shape of the applied bias signal. We will show how different bias functions affect the shape of the IEDF while keeping the mean energy constant at 55 eV, and how this in turn has a clear influence on the crystallinity of the film. The films are deposited in a RF magnetron discharge, driven by 13.56 MHz and 71 MHz. The target is mounted on the powered electrode and a silicon substrate is placed on a biased electrode at the opposite side. Our previous experiments have already shown a preferred orientation in the film when using a rectangular pulsed bias with 1 MHz frequency and an ontime of 5 µs. Here, we will present a thorough investigation of how variations in frequency and duty cycle in the bias signal affect the IEDF and film properties for constant mean energy and an on-time of 5 µs. Additionally, the influence of growth temperature (500 °C, 550 °C and 600 °C) will be shown. Film characterization is performed using FTIR and XRD to determine the orientation/crystallinity of the films. The measurements are correlated with the measured and simulated IEDFs in each case. We will show how the tailoring of the IEDF through bias shape manipulation is excellent tool for controlling film structure. The work is funded by DFG within SFB-TR 87. 10:20am B3-1-8 High-Voltage Positive Nanopulse Assisted Hot- Filament CVD Diamond Growth, M. Takashima, N. Ohtake (ohtaken@mech.titech.ac.jp), Tokyo Institute of Technology, Japan In this study, extremely short pulse, whose pulse width was about 50 ns and called "nanopulse", assisted hot-filament chemical vapor deposition method was used for the diamond synthesis, and depositions at low substrate temperature below 500 °C were attempted decreasing filament temperature and using high-voltage nanopulse assist. In addition, characteristics of nanopulse plasma were investigated through optical emission spectroscopy (OES) analysis as well as time resolved optical emission spectroscopy (TROES) analysis. Spectrometer used was special and the time resolution of 10 ns was enough to trace nanopulse plasma and investigate the effects of nanopluse on diamond growth. As a result, we had succeed in depositing diamond at the substrate temperature of 400 °C using 1500 °C filament and high-voltage nanopulse assist. Moreover, according to OES and TROES measurements of nanopulse plasma, the relations between diamond properties and deposition conditions were found. Atomic hydrogen played an important role on diamond growth and the diamond was able to be deposited with sufficient concentration of CH radicals at the afterglow of nanopulse plasma. Coatings for Biomedical and Healthcare Applications Room: Sunset - Session D2-1 Coatings for Biomedical Implants Moderator: R. Hauert, Empa, Switzerland, J. Piascik, RTI International, US 8:00am D2-1-1 Functional plasma polymer films engineered at the nanoscale for biomaterial applications, K. Vasilev (krasimir.vasilev@unisa.edu.au), University of South Australia, Australia INVITED Functional coatings presenting a variety of functional chemical groups can be readily prepared by plasma polymerisation in an easy one-step process. Applications of such films span over a range of fields from modification of biomaterials to protective coatings. In my talk, I will present recent developments from our group on various biomaterial coatings prepared by plasma polymerisation which include chemical and biomolecular gradients, and antibacterial coatings based on silver nanoparticles and conventional antibiotics. Surface gradients have become important tools for studying and guiding cellular responses such as migration, adhesion, differentiation, etc. We generate gradients of various surface chemistries via plasma copolymerisation over a moving mask. We used these chemical gradients to direct differentiation of kidney (KSC) and embryonic stem cells. We found that KSC express proximal tubule markers at medium amine group surface concentration and adapt a podocyte-like morphology at high.We extended these surface chemical gradients to density gradients of bound ligands, proteins and nanoparticles. We developed gradients of two proteins because gradients of single protein (employed in cell studies up to now) are probably too simplistic to mimic natural biological processes. We also developed density gradients of nanoparticles to use as a tool to study the effect of nanoscale surface features on cell behaviour. Antibacterial coatings are important for many biomedical applications. We developed unique coatings based on silver nanoparticles which allow control over the rate of release of silver ions. As we show, the rate of silver release can be tuned such that it allows normal adhesion and spreading of mammalian cell and preserves the antibacterial properties of the coatings. We also developed two platforms for release of conventional antibiotics such as vancomycin and levofloxacin. Delicate control over the rate of release was achieved by a plasma polymer overlayer of a controlled thickness. References: K. Vasilev et al “Tunable antibacterial coatings that support mammalian cell growth” Nano Lett 10 (1), 202–207 (2010) K. Vasilev et al “A PEG-density gradient to control protein binding: creating gradients of two proteins”, Biomaterials 31, 392–397 (2010) S. Simovic, D. Losic and K Vasilev “Controlled drug release from mesoporous materials by plasma polymer deposition” Chem Commun 46, 1317 - 1319 (2010) R.V. Goreham, R. D. Short and K. Vasilev “A Novel Method for the Generation of Surface-Bound Nanoparticle Density Gradients” J Phys Chem C 115 (8), 3429-3433 (2011) 8:40am D2-1-3 Effect of the surface atom ordering on the protein adsorption, P. Silva-Bermudez (suriel21@yahoo.com), L. Huerta, S.E. Rodil, Instituto de Investigaciones en Materiales, Universidad Nacional Autónoma de Mexico, México The study of the protein adsorption is relevant to understand the interactions biological media–foreign material since the adsorbed protein layer on the material surface mediates the interactions cell-material, greatly determining the biological response. The protein adsorption on solid surfaces is mainly driven by the surface properties; different studies have shown that properties such as hydrophobicity or roughness influence protein adsorption. Also, certain crystalline phases of a material have been 129 Friday Morning, April 27, 2012
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I C M C T F 2 0 1 2 INTERNATIONAL C
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TABLE OF CONTENTS Welcoming Remarks
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2012 ICMCTF SCHEDULE OF EVENTS DAY
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SYMPOSIUM A Coatings for Use at Hig
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Marco Cremona Pontificia Universida
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Exhibitor Keynote Lecture Tuesday,
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2011/12, discuss ideas and prioriti
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At the focus topic, from the experi
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2012 R.F. Bunshah Annual Award & IC
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ICMCTF 2012 Graduate Student Awards
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ICMCTF 2012 thanks Plansee for thei
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ICMCTF 2012 thanks AJA Internationa
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ICMCTF 2012 thanks CemeCon for thei
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ICMCTF 2012 Short Courses April 22
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ICMCTF 2012 Planning Grid We provid
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Key to Session/Paper Numbers A Coat
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Monday Morning, April 23, 2012 Fund
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New Horizons in Coatings and Thin F
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Fundamentals and Technology of Mult
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Advanced Characterization of Coatin
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Hard Coatings and Vapor Deposition
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Tribology & Mechanical Behavior of
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Coatings for Use at High Temperatur
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Applications, Manufacturing, and Eq
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Wednesday Afternoon, April 25, 2012
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Thursday Afternoon Poster Sessions
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Free Caricatures & Massages!! E-1 V
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ICMCTF 2012 EXHIBIT HALL Internatio
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I C M C T F 2012 S P O N S O R S Bo
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All in Good Measure A 24 µm scan o
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Call For Abstracts Deadline: MAY 2,
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CC800 ® /9 HIPIMS true integration
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Exhibit Hall Reception - Atlas Ball
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Kaufman & Robinson announces their
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Miba Coating Group is the specialis
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PLANSEE SE, 6600 Reutte, Austria, T
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� ��
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Plenary Talk Room: Golden Ballroom
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content. Analyses of the oxidised c
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- The control on the gradient in re
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μ = 0.4 to μ = 0.9). On the other
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application tests the ta-C coated d
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4:10pm C2-2/F4-2-10 Investigation o
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process with surfactant on WO3/ITO
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is already reported. To further com
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conditions. The details of the comp
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esidual stress and to the Poisson
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eactive gases with the target mater
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emerging fields. State-of-the-art t
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transparent conducting layers. Howe
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methods provide similar carrier den
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of AISI 52100 steels by developing
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deposition based on high power puls
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coatings removed from the aluminum
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spectroscopy varies from 25 at% to
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This article describes how to use s
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een demonstrated both theoretically
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Furthermore, the silane coupling ag
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10:40am A1-1-9 High temperature oxi
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10:40am B4-2-10 Understanding the d
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11:00am B5-1-10 Hard nanocrystallin
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* Sandia National Laboratories is a
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fluidized bed of tin, zinc and alum
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mechanical and chemical properties.
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duration for super-low friction see
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stainless steel DIN X42Cr13 surface
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2:30pm TS1-1-3 Surface engineering
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X-ray diffraction patterns of the Z
Page 177 and 178: 11:20am B6-1-11 Direct current magn
Page 179 and 180: loading situations could help to ob
Page 181 and 182: Energetic Materials and Micro-Struc
Page 183 and 184: The present work was supported by t
Page 185 and 186: silica-based hydrophilic coatings i
Page 187 and 188: extent depending on the actual grow
Page 189 and 190: [1] F. Tasnádi, B. Alling, C. Hög
Page 191 and 192: eproducibility of the preparation o
Page 193 and 194: showed by the uncoated 4140 steel s
Page 195 and 196: polarization resistance and corrosi
Page 197 and 198: thin films in which a multiscale mo
Page 199 and 200: centers, ascribed to conduction ele
Page 201 and 202: BP-26 Characterization of laser abl
Page 203 and 204: BP-38 Stress signature of an amorph
Page 205 and 206: simultaneously optimize materials p
Page 207 and 208: CP-17 Effects of UV Light Treatment
Page 209 and 210: amorphous structure with a smooth s
Page 211 and 212: addition, it was observed that the
Page 213 and 214: EP-5 The effective Indenter concept
Page 215 and 216: the substrates directly or after ra
Page 217 and 218: as-grown films using textured Si as
Page 219 and 220: proposed memory device exhibits exc
Page 221 and 222: FP-24 Effect of hydrogen addition o
Page 223 and 224: oxide obtained was correlated to th
Page 225 and 226: Post Deadline Discoveries and Innov
Page 227: chemical bonds have also been achie
Page 231 and 232: 10:20am D2-1-8 Corrosion Resistance
Page 233 and 234: property combination is attractive
Page 235 and 236: PVD is a challenging task. The pres
Page 237 and 238: Chang, G.W.: C2-3/F4-3-3, 29; GP-3,
Page 239 and 240: Huang, K.H.: BP-33, 102 Huang, P.H.
Page 241 and 242: Moody, N.R.: F6-1-1, 7 Moon, S.: D1
Page 243 and 244: Szeremley, D.: G3-1-7, 68 Szesz, E.
Page 245 and 246: NOTES 145
Page 247 and 248: Description of Research Highlights:
Page 249 and 250: their presentations in order to eva
Page 251 and 252: NOTES 151
Page 253 and 254: 153
Page 255 and 256: MARK YOUR CALENDAR FOR ICMCTF 2013!
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ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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