Solid-state {sup 29}Si NMR analysis of amorphous silicon nitride powder
- AlliedSignal Inc., Morristown, NJ (United States)
- Rutgers-the State Univ., Piscataway, NJ (United States). Center for Ceramic Research
Solid-state {sup 29}Si NMR techniques were used to characterize laser-synthesized silicon nitride powder prepared from the reaction of silane with ammonia. When the powder is exposed to water vapor, a hydrated layer rapidly forms at the surface. A comparison of {sup 29}Si cross polarization (CP) and Bloch decay (BD)-MAS-NMR spectra revealed differences between surface and bulk compositions. CP-NMR identified Si-NH{sub x} (x = 1, 2) species with a chemical shift of {minus}45 ppm in the as-synthesized (unexposed) powder. In BD-NMR spectra, the nitride resonance is observed at {minus}48 ppm. For the hydrated powder, CP-NMR identified additional {triple_bond}Si-OH (Q{sup 3}), {double_bond}Si-(OH){sub 2} (Q{sup 2}), and SiO{sub 2} (Q{sup 4}) species present at the surface. The CP-NMR spectra were corrected for T{sub 1pH} relaxation effects and deconvoluted into individual components in order to extract quantitative measurements of the various species present.
- Sponsoring Organization:
- USDOE
- OSTI ID:
- 211715
- Journal Information:
- Journal of the American Ceramic Society, Journal Name: Journal of the American Ceramic Society Journal Issue: 2 Vol. 79; ISSN 0002-7820; ISSN JACTAW
- Country of Publication:
- United States
- Language:
- English
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