Characterization of nanoporosity in polymer-derived ceramic fibres by X-ray scattering techniques

作者: Ludo K. Frevel , Robert L. Miller , Jonathan Lipowitz , James A. Rabe

DOI: 10.1007/BF01045776

关键词: Composite materialPorosimetrySurface energyMaterials scienceSmall-angle X-ray scatteringPorosityScatteringMineralogyVolume fractionCeramicX-ray scattering techniques

摘要: Ceramic fibres with Si-C-O and Si-N-C-O compositions, prepared by pyrolysis of polymer precursors, generally have densities lower than those calculated from a volume additivity rule. However, techniques often used to detect porosity such as electron microscopy methods, surface area porosimetry measurements show that little surface-connected is present. X-ray scattering measurements, both wide-angle (WAXS) small-angle (SAXS), considerable in the range 1° < 2θ 10° (CuKα). Treatment data classical Guinier (low angle limit) Porod (high methods indicate closed, globular, nanometre-scale (1 3 nm diameter) present all ceramic examined. power correlates quantitatively fraction porosity, expected if dominant facto affecting scattering. Nano-particles excess carbon ofβ-SiC nanocrystallites, though present, are minor contributors X-rays these fibres. Fibres three-dimensional, not fractal dimension, oriented. As density increases increasing temperature, average pore size decreases. This results thermodynamically favourable reduction free energy apparently occurs viscous flow process.

参考文章(15)
S. Lowell, Joan E. Shields, Powder surface area and porosity ,(1984)
JONATHAN LIPOWTZ, H.A. FREEMAN, R.T. CHEN, E. R. PRACK, Composition and Structure of Ceramic Fibers Prepared from Polymer Precursors Advanced Ceramic Materials. ,vol. 2, pp. 121- 128 ,(1987) , 10.1111/J.1551-2916.1987.TB00066.X
Jonathan Lipowitz, Gary E. Legrow, Thomas F. Lim, Neal Langley, Silicon Carbide Fibers from Methylpolysilane (MPS) Polymers Proceedings of the 12th Annual Conference on Composites and Advanced Ceramic Materials, Part 1 of 2: Ceramic Engineering and Science Proceedings, Volume 9, Issue 7/8. pp. 931- 942 ,(2008) , 10.1002/9780470310496.CH45
Glatter O, Kratky O, Pilz I, Small Angle X-Ray Scattering ,(1982)
S. Yajima, Y. Hasegawa, J. Hayashi, M. Iimura, Synthesis of continuous silicon carbide fibre with high tensile strength and high Young's modulus Journal of Materials Science. ,vol. 13, pp. 2569- 2576 ,(1978) , 10.1007/PL00020149
C.J. Brinker, G.W. Scherer, Sol → gel → glass: I. Gelation and gel structure Journal of Non-crystalline Solids. ,vol. 70, pp. 301- 322 ,(1985) , 10.1016/0022-3093(85)90103-6
F.D Rumscheidt, S.G Mason, Break-up of stationary liquid threads Journal of Colloid Science. ,vol. 17, pp. 260- 269 ,(1962) , 10.1016/0095-8522(62)90041-7
Dale W. Schaefer, Fractal Models and the Structure of Materials Mrs Bulletin. ,vol. 13, pp. 22- 27 ,(1988) , 10.1557/S088376940006632X
George W. Scherer, C.Jeffrey Brinker, E.Peter Roth, Sol → gel → glass: III. Viscous sintering Journal of Non-crystalline Solids. ,vol. 72, pp. 369- 389 ,(1985) , 10.1016/0022-3093(85)90190-5
Leroy Elbert Alexander, X-ray diffraction methods in polymer science ,(1969)