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Nanosize Surface Electromodification of Carbon Fibers by Conductive Polymers  and Their Characterizations

Nanosize Surface Electromodification of Carbon Fibers by Conductive Polymers  and Their Characterizations. Prof.Dr.A. Sezai.S ARAÇ Istanbul Technical University Department of Chemistry & Polymer Science and Technology Maslak 80626 Istanbul,Turkey. 5-7 μ. C arbon fiber reinforcement

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Nanosize Surface Electromodification of Carbon Fibers by Conductive Polymers  and Their Characterizations

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  1. Nanosize Surface Electromodification of Carbon Fibers by ConductivePolymers  and Their Characterizations Prof.Dr.A.Sezai.SARAÇ Istanbul Technical University Department of Chemistry & Polymer Science and Technology Maslak 80626 Istanbul,Turkey

  2. 5-7μ Carbon fiber reinforcement of polymeric composites • Carbon fibers(CF) are used in composites(i.e.,PAN based CF) in order to produce materials of lower density and greater strength. advanced structural materials:aircraft, spacecraft, and suspension bridges – • The most widely used composite material in tactical aircraft is a carbon fibre/epoxy • A polymeric ‘interface’ acting as a coupling agent, improve the interfacial properties between reinforcing (carbon) fibers and the polymeric matrix . A.S. Sarac, A. Bismarck, E. Kumru, J. Springer,Synth. Met. 123 (2001) 411-423 E.Kumru,J.Springer,A.S.Sarac,A.Bismarck.,  Synth. Met.  123(2001)391-402

  3. Biosensor Appl. • Electromodified carbon fibers also have potential for biosensor applications as microelectrodes -working in small volumes of solutions- • HomogeneousConductive Polymer coated -surface functionalitiesis suitable for the miniaturization of electrode system for a particular analyte. • Several copolymer and polymer coated electrodes(Cz based) were shown to be an effective disposable microelectrode system for the determination of p-aminophenolat low detection limits M. Jamal, E. Magner, A.S.Sarac, Sensors and Actuators 97 (2004)59-66

  4. Carbon Fiber Reinforcementapplying force to a composite material, the brittle matrix cracks at low stress levels > fibres take over Woven fiber Epoxy resin –polymer matrix

  5. The structure & comp. of copolymeric films, plays an important role on the final properties of modified carbon surfaceThe coating parameters & characterization of these functionalised thin filmsareimportant.Improving the interfacial adhesionAdvanced Composites- Interfacial adhesioncontrol the level of fiber/matrix adhesion • A.S.Sarac,M.Serantoni,,A.M.T.Syed,V.J.Cunnane ,Appl.Surface Sci.,(2004) 229,13-18 • A.S.Sarac,A.M.T.Syed,M.Serantoni,,V.J.Cunnane J.Mater.Sci.Lett.(2004) 39,2945-2950

  6. Surface Analysis (the characterizations ofelectrografted thin polymeric film ~10-50nm film characterizations-Fast and simple for org. thin film coating & charac. -Nanosize Change of functionality of surface) • Spectroscopic Functionalities • FTIR-ATR • Raman Composition - XPS,EDX,FIBSIMS Electrochemical Impedance Spectroscopic studies • Morphological • SEM • AFM

  7. AFM of Electrogrowth of P[Cz-co-AAm] onto HOPG Graphite Higher scan rates (100 mV/s) : thin (hf 22 nm) coatings .Lower scan rates (≤ 50 mV/s) ~50 nm A.Bismarck,A.Menner,J.Barner,A.F.Lee,K.Wilson, J.Springer,J.P.Rabe,A.S.Sarac, Surface Coat .Tech. 145(2001)164-175

  8. Current density vs cycle number (▪): 1.53V (●): 1.04 Vand the coating thickness (▫) from the ellipsometric angles

  9. Galvanostatic vs.Cyclic voltammetry polymerization ratevs.film growth. • CV : • Galvanostatic process thin coating (hf15nm) & smoother (RMS=13nm),

  10. AFM of Untreated Carbon fiber(r~5.6 μ) polyethylenedioxythiophene(PEDOT)

  11. Polyterthiophene/CF

  12. Electrocoating of polytetrathiophene onto carbon fiber by cyclic voltammetry10mM TEABF4/MeCN. 10 cycles at 100mVs-1 2 mM Polytetrathiophene in 10 mM TEABF4 / PC , 20 mV/s ,RMS 50 nm (1mm2)5 scan SARAC,A.S.,EVANS,U.,SERANTONI,M.,CUNNANE,V.J.,Carbon 41,14 (2003) 2725-2730

  13. polytetrathiophene formation on the surface

  14. polymethylcarbazole

  15. Poly[MCz] on CFME in 0.1 M NaClO4 in PC at 100 mV/s.

  16. Poly[MPy] on CFME in 0.1 M NaClO4 in PC at 100 mV/s.

  17. Poly[MPy-co-MCz] on CFME in 0.1 M NaClO4 in PC at 100 mV/s, [MPy]& [MCz]=0.001 M

  18. Poly[MPy-co-MCz] in monomer-free solution.a) 10 mV/s, b) 20 mV/s, c) 50 mV/s, d) 100 mV/s, e) 200 mV/s in a 0.1 M NaClO4 / PC solution. All samples were subsequently cycled 8 times

  19. Scan rate dependence of the copolymer film :Plots of anodic and cathodic peak currents vs. the square root of scan rate Inset: : change in anodic and cathodic peak currents with scan ratein monomer free solution of 0.1M NaClO4/PC Randles Selvic ip = (2.69 x 108) n3/2 A C D1/2ν1/2

  20. Effect of feed ratio of monomers on current ,solid state conductivity and yield.

  21. Comparison the peak current densities of electro-growth of the copolymer films obtained by CV and solid state conductivity in differentmonomer ratios

  22. Anodic peak current densities of Poly[MPy-co-MCz] in different electrolytes using multiple (50 cycles) in monomer-free solution at 100 mV/s, [MPy] &[MCz]=0.001 M.

  23. Poly(N-vinylcarbazole-co-Vinylbenzenesulfonic acid) Element Element NVCzVBSA2 NVCzVBSA2 NVCzVBSA3 NVCzVBSA3 C C 76.57 76.57 85.83 85.83 N N 2.843 2.84 3.76 3.76 O O 15.2 15.20 9.033 9.03 S S 2.83 2.825 0.15 0.147 • Ungrafted CF, • P[NVCz-co-VBSA] grafted CF • 100 mA 4 hrs • 200mA 2 hrs

  24. (b) (c) Poly[NVCz-coVBSA] NVCzVBSA3

  25. Reflectance FTIR of thin carbazole copolymer film on CF

  26. Poly[Methylthiophene-co-carbazole]

  27. Reflectance FTIR & EDX of electrografted P[MeTh-co- Cz] thin copolymer film • A.S.Sarac, J.Springer., Surface Coat.Tech.(2002) 160,227-238

  28. Raman Spectra1330 cm-1 C=C , 1567cm-1 C-C ring

  29. XPS C=S C-N C=O P[Cz-co-MeTh] Carbon fiber at different initial comonomer feed ratios • A.S.Sarac, M.Serantoni, T.Syed, J.Henry, V.J.Cunnane, J.B.McMonagle, Appl.Surface Sci.. 243(1-4)( 2005) 183-198 • A.S.Sarac, A.MT.Syed, M.Serantoni, J.Henry, V.J.Cunnane, J.B.McMonagle. • Appl.Surface Sci. Sci.222,1-4(2004) 148-165

  30. Reflectance FTIR of vinyl group in copolymer

  31. Poly[MeTh-co-NVCz]

  32. Electrocoated carbon fibre single fibre pull-out test. a)The fibre was partially pulled-out of the electrodepositedcoating. b) fibre completely pulled-out of the electrodeposited coating. The adhesive strength CF/PMMA matrix resulted in 100% improved in thin and homogeneous PMMA coatings. (the interfacial shear strength not so good in thicker coatings) So, electrocoating of MMA can improve the interfacial performance of a carbon fibre reinforced PMMA model composite.

  33. % concentration (determined from XPS ) versus cps (determined from FIBSIMS measurements ) P[NVCz-co-MeTh] M.Serantoni,A.S.Sarac,D.Sutton,V.J.Cunnane, Surface Coat.Tech..( 2005) (in press)

  34. Nanosize Surface chemistry & Morphology of CP electrografting onto Carbon Foam & CF surface &Electrochemical ImpedanceTheir Applications • Thin conductive polymer films can be covalently electrografted onto the CF • Surface structure and composition can be analysed in nanoscale (> 20 nm)(XPS,Raman ,FTIRATR) • Surface morphology (SEM,AFM) • improve the interfacial shear strength • reinforcement appl. • biosensor applications

  35. Istanbul BosphorousAsia-Europe sarac@itu.edu.tr http://atlas.cc.itu.edu.tr/~sarac/ http://www.kimya.itu.edu.tr/saraca/

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