Solid-state {sup 29}Si NMR analysis of amorphous silicon nitride powder

Journal Article · Thu Feb 01 04:00:00 EST 1996 · Journal of the American Ceramic Society

DOI:https://doi.org/10.1111/j.1151-2916.1996.tb08156.x· OSTI ID:211715

Leone, E A; Curran, S; Kotun, M E ^[1]; Carrasquillo, G; Weeren, R van; Danforth, S C ^[2]

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1. AlliedSignal Inc., Morristown, NJ (United States)
2. 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

Related Subjects

36 MATERIALS SCIENCE
40 CHEMISTRY
AMMONIA
CHEMICAL REACTIONS
HYDRATION
LASERS
PARTICLE SIZE
POWDERS
SILANES
SILICON NITRIDES
STRUCTURAL CHEMICAL ANALYSIS
SURFACE AREA
SURFACES
SYNTHESIS
TIME DEPENDENCE