nanocomposites: synthesis and characterization
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1 National Institute for Research and Development of Isotopic and Molecular Technologies Cluj-Napoca Romania Carbon nanotubes-polypyrrole nanocomposites: synthesis and characterization R. Turcu a, O. Pana a, Al. Darabont b, D. Lupu a, A.R. Biris a, N. Aldea a, N. Jumate c, M.L. Soran a a National Institute R&D for Isotopic and Molecular Technologies, PO Box 700, Cluj-Napoca, Romania b Babes-Bolyai University, Faculty of Physics, Cluj-Napoca, Romania c Technical University of Cluj-Napoca, Materials Science Dept., Cluj-Napoca Romania
2 Outline Synthesis of carbon nanotubes Synthesis of carbon nanotubes-polypyrrole (PPY-CNT) nanocomposites Characterization methods: -SEM and TEM (JSM 5600 LV and 1010 JEOL microscopes) - FTIR spectroscopy (JASCO FTIR 610) - X-ray diffraction (powder diffractometer in Brag-Brentano geometry, Ni filtered CuK α radiation) Results and discussion Conclusion
3 Synthesis of carbon nanotubes Multi-walled and single-walled CNTs were obtained by chemical vapor deposition from hydrocarbons in the presence of a metal catalyst. Two methods were used to introduce the carbon source material into the pyrolysis furnace: either as a vapor in a gas stream (Ar) or by liquid injection using an atomizer (sprayer). A single step synthetic route, which involves the spray-pyrolysis of ferrocene as catalyst dissolved in liquid hydrocarbon (e.g. benzene, xylene) as carbon source, in an Ar atmosphere ; temperatures between o C. The fixed-bed method: the catalyst is put into the reactor at the beginning of the CNTs synthesis. We developed a new technique, by which the heating of the catalyst may be achieved by high frequency induction heating (IH). This method show some advantages compared to the usual outer furnace technique: a faster heat transfer to the catalyst, versatility in the temperature control, higher temperatures available for synthesis and thermal annealing, reduced extent of the heating zone, lower energy consumption, lowering of the overall time for a batch due to the fast heating and cooling rates. D.Lupu et al., Carbon 42 (2004) 503
4 Synthesis of PPY-CNT nanocomposites PPY-CNT nanocomposites were obtained by in situ chemical oxidative polymerization of pyrrole monomer in aqueous solution containing dispersed MWCNTs. MWCNTs treated in acids mixture HNO 3 :H 2 SO 4 (1:1) and untreated MWCNTs were used Oxidant : ammonium persulfate (APS) Dodecylbenzensulfonic acid (DBS) or the Fe 3 O 4 nanofluid having a double layer sterical stabilization with myristic acid were added to the water suspension of MWCNTs untreated in acids mixture Samples notations: a PPY-CNT - b PPY-CNT - c PPY-CNT - prepared using acids treated MWCNTs; prepared using MWCNTs untreated in acids and with the addition of DBS in the polymerization solution (DBS/pyrrole=0.5 molar ratio); prepared using MWCNTs untreated in acids and with the addition of Fe 3 O 4 nanofluid in the polymerization solution.
5 Morphology of MWCNTs prepared by spray-pyrolysis of liquid hydrocarbon-ferrocene solution TEM image of MWCNTs FESEM image of bundles aligned MWCNTs
6 HRTEM image of carbon nanotubes obtained by induction heating from acetylene in nitrogen on Fe:Co:CaCO 3, at 720 o C.
7 Morphology of PPY- CNT TEM image of nanocomposite a PPY-CNT SEM image of nanocomposite a PPY-CNT
8 FTIR spectroscopy Absorbance (a.u.) b PPY-CNT a PPY-CNT Absorbance (a.u.) PPY wavenumber (cm -1 ) wavenumber (cm -1 ) PPY a PPY-CNT b PPY-CNT Band assignments ring deformation C-H bending ring deformation C-H in-plane bend ring breathing C-H in-plane bend ring breathing with contribution from C=C/C-C and C-N C=C/C-C streching
9 Structural characterization by XRD Intensity MWCNTs Intensity theta (degree) Intensity theta (degree) theta (degree) XRD spectrum for the sample c PPY-CNT. Inset: XRD spectrum for MWCNTs Fe 3 O 4 characteristic peaks are observed in the range degrees. (1) - experimental XRD spectrum for c PPY-CNT; (2) background correction; (3) PPY contribution; (4) line attributed to the reflection on the plane with (002) Miller indices from MWCNTs
10 EDX spectrum of the sample c PPY-CNT together with relative quantitative analysis for the main elements and the map distribution of Fe Quantitative results Weight% C O S Fe
11 The analysis of XRD line broadening Generalized Fermi Function (GFF): GFF A ( 2θ ) = a( 2θ c) b( 2θ c) e + e (1) The integral width δ h (a, b) of the experimental function: δ ( a, b) = h ( a a b b ) π a cos 2 a 1 /( a + b ) π + b b (2) The experimental h, the true sample f and instrumental g functions are related by the integral equation: h ( s) = f ( s t) g( t) dt (3) The integral width of the true XRLP sample, δ f : where ρ = (a + b)/2 for f and g functions. δ f π πρ h ( ρ = cos + 1 h, ρ g ) πρ h 2 cos ρ g ρ h 2ρ g (4) The average particle size, (classical Scherrer relation): D D = 0.9λ δ cos θ f (5) N. Aldea et al. Spectrochim. Acta Part B 57 (2002) N. Aldea et al. J. Optoelectron. Adv. Mater. 6(1), (2003) 225.
12 Table1. The parameters of GFF approximation GFF A±δA a±δa b±δb c±δc g ± ± ± ± h MWCNTs ± ± ± ± h c PPY-CNT ± ± ± ± Table2. The integral widths for instrumental, δ g, experimental, δ h and true sample, δ f functions and MWCNTs average crystallite sizes, D Sample δ g (a,b) [2θ] δ h (ρ h,ρ g ) [2θ] δ f (ρ h,ρ g ) [2θ] D [Ǻ] g MWCNTs c PPY-CNT The observed diffraction profile of a standard graphite sample, considerate to be free of structural imperfection was used to represent the instrumental g function.
13 CONCLUSION PPY-CNT nanocomposites have been obtained by using either MWCNTs previously treated with acids or untreated; The polymerization of pyrrole occurs dominantly on the surface of MWCNTs, resulting in the formation of the nanocomposite; The easy polymerization of pyrrole monomer on MWCNTs could be an attractive method to attach different inorganic nanoparticles (e.g. magnetic Fe 3 O 4 ) or functional groups with the polymer layer; PPY-CNT nanocomposites offer great promise for applications in supercapacitors, biosensors, electronic devices.
14 Acknowledgement This work was supported by the Romanian Ministry of Education and Research under the research program CERES, project nr /2004. We acknowledge the participation in the EU NoE Nanofun- Poly.
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