P <strong>in</strong>dicat<strong>in</strong>gP forforPP curvesP exist<strong>in</strong>gP atP andPPoster Session, Thursday, June 17Theme F686 - N11231Polyol Synthesis of PVP–MnR3ROR4R Nanocomposite1123Z. DurmusP P, UA. BaykalUP P*, H. Kavas,P P, M.S. ToprakP2PDepartment of Chemistry,P PDepartment of Physics, Fatih University, B.Çekmece, 34500 Istanbul, TurkeyP3PFunctional Materials Division, Royal Institute of Technology - KTH, SE-16440 Stockholm, SwedenAbsract- We report on the synthesis of polyv<strong>in</strong>yl pyrrolidone (PVP)-MnR3ROR4R nanocomposites via a polyol route. The capp<strong>in</strong>g of PVP aroundMnR3ROR4R nanoparticles was confirmed by FTIR spectroscopy, the <strong>in</strong>teraction be<strong>in</strong>g via bridg<strong>in</strong>g oxygens of the carbonyl (C=O) and thenanoparticle surface. Tc and TRBR PVP-MnR3ROR4 Rnanocomposite were observed at 42 K and 28.5 K respectively.MnR3ROR4R is known to crystallize <strong>in</strong> the normal sp<strong>in</strong>elstructure with a tetragonal distortion elongated along the c-axis. Manganese ions are placed <strong>in</strong> the tetrahedral A-sites2+3+(MnPP) and octahedral B-sites (MnPP) [1-4]. The FTIRspectra of PVP and PVP-MnR3ROR4R nanocomposite areshown <strong>in</strong> Fig. 1. It is worth not<strong>in</strong>g that the C=O stretch-1band is present at 1660 cmP pure PVP and afterformation of PVP-MnR3ROR4R nanocomposite this stretch<strong>in</strong>g-1red shifts of ~20 cmPa strong <strong>in</strong>teractionbetween MnR3ROR4R nanoparticles and C=O of PVP hostmatrix.Magnetization (emu/g)0,30,20,1FC (100 Oe)ZFC-dM/dT-dM/dTFC0 20 40 60 80ZFC% Transmittance (a.u.)PVPPVP/Mn 3O 4295829234000 3500 3000 2500 2000 1500 1000 500Wavenumber (cm -1 )Figure 1. FTIRnanocomposite.28822855In plane C–H bend<strong>in</strong>gof different –CH 21660spectra of (a) pure PVP (b) PVP-MnR3ROR4RCrystall<strong>in</strong>e phase was identified as MnR3ROR4R and thecrystallite size was obta<strong>in</strong>ed as 6±1 nm from X-ray l<strong>in</strong>eprofile fitt<strong>in</strong>g. As compared to the average particle size of6.1±0.1 nm obta<strong>in</strong>ed from TEM analysis <strong>in</strong> Fig. 2, whichreveal nearly s<strong>in</strong>gle crystall<strong>in</strong>e nature of thesenanoparticles.Relative Frequency3530252015c)1642–C–N stretch<strong>in</strong>g–C–N stretch<strong>in</strong>gD=6,1 nm=0,10,00 20 40 60 800 20 40 60 80Temperature, (K)Figure 3. Zero-field-cooled (ZFC) and field-cooled (FC)magnetization curves PVP-MnR3ROR4R nanocomposite.The sample has hystheresis with small coercivity andremanenet magnetization at 40 K, resembl<strong>in</strong>g thesuperparamagnetic state. a.c. conductivity measurementson PVP-MnR3ROR4 Rnanocomposite revealed a conductivity <strong>in</strong>-7 -1the order of 10PP S·cmP lower frequencies (Fig. 3). Theconductivity changes with respect to frequency can be+2expla<strong>in</strong>ed by electronic exchange occur<strong>in</strong>g between MnP+3’and MnP <strong>in</strong> sublattice of sp<strong>in</strong>el lattice. The P’’of PVP-MnR3ROR4 Ras a function of frequency arefound to be slightly temperature dependent.* Correspond<strong>in</strong>g author: hbaykal@fatih.edu.tr[1] Z. Durmu., A. Baykal, H. Kavas, M. Direkçi, M.S. Toprak,Polyhedron, 28, 2119-2122 (2009).[2] T. Ozkaya, A. Baykal, H. Kavas, Y. Koseoglu, M.S. Toprak,Physica B 403 (2008) 3760–3764.[3] A. Baykal, Y. Koseoglu, M. Senel, Cent. Eur. J. Chem. 5(1)2007 169–176.[4] Z. Durmu, H. Kavas, A. Baykal, M.S. Toprak, Cent. Eur. J.Chem. 7(3) 2009 555-559.10505,0 5,5 6,0 6,5 7,0 7,5Diameter (nm)Figure 2. TEM micrograph of PVP-MnR3ROR4R and calculatedhistogram from several TEM images with a log-normal fitt<strong>in</strong>g.6th Nanoscience and Nanotechnology Conference, zmir, 2010 717
PPPR2R PIN(80)PPgPP OzlemPPoster Session, Thursday, June 17Theme F686 - N1123Synthesis and Characterization of Poly<strong>in</strong>dole/TioR2R Nanocomposites111Bekir SahanP ErolPUH. Ibrahim UnalUP P*1PSmart Materials Research Lab. Department of Chemistry, University of Gazi, Ankara, TurkeyAbstract-Poly<strong>in</strong>dole/TiOR2R nanocomposites are synthesized by <strong>in</strong>-situ polymerization us<strong>in</strong>g FeClR3R as an oxidiz<strong>in</strong>g agent <strong>in</strong> the presence ofsodium dodecybenzenesulfonate (Na-DBS) surfactant at two compositions with high yields. Characterizations of the poly<strong>in</strong>dole (PIN) andpoly<strong>in</strong>dole/TiOR2R nanocomposites were carried out by us<strong>in</strong>g various techniques namely: elemental analysis, FTIR, particle size, conductivity,magnetic susceptibility, density, TGA, XRD, SEM and TEM measurements.Polymer and metal oxides have been studied for manyyears for their <strong>in</strong>dependent electrical, optical, and mechanicalproperties. The comb<strong>in</strong>ation of semiconduct<strong>in</strong>g andmechanical properties of conjugated polymers with theproperties of metals or semiconduct<strong>in</strong>g <strong>in</strong>organic particleshas brought new prospects for wide application areas [1].One of the widely studied metal oxide is TiO R2R because of itsunique optical, electrical, chemical, high photocatalyticactivity, photoelectric conversion efficiency, electrok<strong>in</strong>etic,colloidal and electrorheological properties [2-3]. Among theclasses of <strong>in</strong>herently conductive polymers, PIN is much<strong>in</strong>terested one due to its several advantages such as fairlygood thermal stability, electrochromic properties, high redoxactivity and stability [4]. Therefore, PIN has received asignificant amount of attention <strong>in</strong> the past several years andmay be a good candidate for applications <strong>in</strong> various areas,such as electronics, electrocatalysis, anode materials <strong>in</strong>batteries, anticorrosion coat<strong>in</strong>gs and electrorheology. PINand its derivatives have been synthesized either by anTable 1. Some physical characteristics of the materials.Cod<strong>in</strong>gConductivity-(S cmP1 4)x10PMagneticsusceptibility(XRgR,cm1 7P)x10P-Density-3(g cmP P)PIN 1.03 21.27 0.94 21*PS-PIN 1.40 11.55 0.95 20TiOR2R(10)/PIN(90) 0.12 32.88 0.98 18TiOR2R(20)/PIN(80) 0.11 87.701.03 19*PS-TiOR2R(10)/PIN(90) 7.74 8.39 1.02 19*PS-TiO (20)/ 4.32 9.661.06 18*Where S denotes the presence of surfactant.Positive magnetic susceptibility values were <strong>in</strong>dicatedthat conduct<strong>in</strong>g mechanism <strong>in</strong> the PIN and PIN/TiOR2Rnanocomposites were polaron <strong>in</strong> nature. The presence ofNa-DBS surfactant and <strong>in</strong>creased percentage of TiOR2R wereobserved to slightly enhance the density of the materialssynthesized. It was observed that, the thermal stabilities ofthe PIN/TiOR2R nanocomposites were higher than PIN asexpected, which is an important parameter for <strong>in</strong>dustrialapplications such as vibration damp<strong>in</strong>g <strong>in</strong>electrorheological fluids. Expected dist<strong>in</strong>ctive XRDpatterns of PIN/TiOR2R nanocomposites were identical tothose of TiOR2R nanoparticles reported <strong>in</strong> the literature, withan implication of deposited PIN on the surface of TiOR2Rparticles and had no effect on the degree of thecrystall<strong>in</strong>ity of TiOR2R. SEM and TEM results revealed themorphologies of the materials and <strong>in</strong>dicated thehomogeneous distribution of the components <strong>in</strong> the PINand PIN/TiOR2R nanocomposites. In conclusion, PIN/TiOR2Rnanocomposites were successfully synthesized, suitable forfurther zeta-potential measurements, electrorheologicalParticlesizes(μm)electrochemical, a chemical oxidative, emulsion, or<strong>in</strong>terfacial polymerization [5-6].In this study PIN/TiOR2R nanocomposites were synthesizedespecially to <strong>in</strong>vestigate their colloidal properties andelectrorheological activities <strong>in</strong> order to use as vibrationdamp<strong>in</strong>g material <strong>in</strong> shock absorbers <strong>in</strong> future studies. Forthis purpose, first PIN, then four types of PIN/TiOR2Rnanocomposites were synthesized without and with thepresence of 7%Na-DBS, and all the cod<strong>in</strong>gs are given <strong>in</strong>Table 1. Elemental analysis results <strong>in</strong>dicated that thenanocomposites were successfully prepared with desiredamounts of surfactant and composition. FTIR results showedthe expected dist<strong>in</strong>ctive absorptions belong<strong>in</strong>g to both PIN,TiOR2R proofed the formation of both homopolymer andPIN/TiOR2R nanocomposites. Conductivities of the materialswere observed to <strong>in</strong>crease with the <strong>in</strong>clusion of surfactantonto the PIN and PIN/TiOR2R nanocomposite surfaces(Table 1).(solidification of dispersions under the <strong>in</strong>fluence ofexternal electric field <strong>in</strong> milliseconds, repeatedly andreversibly) studies, creep-recovery tests and vibrationdamp<strong>in</strong>g experiments, which will be the second part of thisstudy.* HTCorrespond<strong>in</strong>gTH author: hiunal@gazi.edu.tr[1] Q.-T. Vu, M. Pavlik, N. Hebestreit, J. Pfleger, U. Rammelt,W. Plieth, Electrochim. Acta 51, 1117 (2005).[2] Q.-T. Vu, M. Pavlik, N. Hebestreit, U. Rammelt, React.Funct. Polym. 65, 69 (2005).[3] J.J.M. Halls, K. Pichler, R.H. Friend, S.C. Moratti, A.B.Holmes, Appl. Phys. Lett. 68, 3120 (1996).[4] G. Nie, X. Han, J. Hou, and S. Zhang, J. Electroanal. Chem.604, 125 (2007).[5] Z. Cai, M. Geng, and Z. Tang, J. Mater. Sci. 39, 4001 (2004).[6] H. Talbi, B. Humbert, and D. Billaud, Synth. Met. 84, 875(1997).6th Nanoscience and Nanotechnology Conference, zmir, 2010 718
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