Pyrolysis chemistry of an organometallic precursor to silicon carbide

The cross-linking reactions and decomposition of a vinylic polysilane precursor to silicon carbide were systematically investigated in the course of thermolysis to 1,000{degree}C in N{sub 2}. The polymer-to-ceramic conversion chemistry was studied by means of thermogravimetry, infrared spectroscopy,...

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Bibliographic Details
Published in:Chemistry of materials 1991-03, Vol.3 (2), p.257-267
Main Authors: Schmidt, Wayde R, Interrante, Leonard V, Doremus, Robert H, Trout, Todd K, Marchetti, Paul S, Maciel, Gary E
Format: Article
Language:English
Subjects:
400201 - Chemical & Physicochemical Properties
400800 - Combustion, Pyrolysis, & High-Temperature Chemistry
CARBIDES
CARBON COMPOUNDS
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
CHROMATOGRAPHY
COHERENT SCATTERING
DECOMPOSITION
DIFFRACTION
GAS CHROMATOGRAPHY
GRAVIMETRIC ANALYSIS
HYDRIDES
HYDROGEN COMPOUNDS
INERT ATMOSPHERE
INFRARED SPECTRA
INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY
MAGNETIC RESONANCE
MASS SPECTROSCOPY
NUCLEAR MAGNETIC RESONANCE
ORGANIC COMPOUNDS
ORGANIC SILICON COMPOUNDS
PYROLYSIS
QUANTITATIVE CHEMICAL ANALYSIS
RESONANCE
SCATTERING
SEPARATION PROCESSES
SILANES
SILICON CARBIDES
SILICON COMPOUNDS
SPECTRA
SPECTROSCOPY
THERMAL ANALYSIS
THERMAL GRAVIMETRIC ANALYSIS
THERMOCHEMICAL PROCESSES
VERY HIGH TEMPERATURE
X-RAY DIFFRACTION
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Summary:The cross-linking reactions and decomposition of a vinylic polysilane precursor to silicon carbide were systematically investigated in the course of thermolysis to 1,000{degree}C in N{sub 2}. The polymer-to-ceramic conversion chemistry was studied by means of thermogravimetry, infrared spectroscopy, solid-state NMR spectroscopy ({sup 1}H CRAMPS; {sup 13}C and {sup 29}Si magic-angle spinning), X-ray powder diffraction, and elemental analysis of isolated solid intermediates. Gaseous byproducts were analyzed by gas chromatography, mass spectrometry, and infrared spectroscopy. The polymer primarily undergoes cross-linking through the vinyl groups below 300{degree}C, although there is evidence for some hydrosilylation. Decomposition reactions consist of chain scission, with production of radical species, and methylene insertion, which converts the polysilane backbone to polycarbosilane. Crystallization to carbon-rich {beta}-SiC ceramic occurs above 750{degree}C.
ISSN:0897-4756
1520-5002
DOI:10.1021/cm00014a011