Synthesis of high purity, alpha phase silicon nitride powder

Details Synthesis of high purity, alpha phase silicon nitride powder Synthesis of high purity, alpha phase silicon nitride powder

1974-03-01

1976-05-25

Rutledge, L. Dewayne

Chemistry of inorganic compounds

Silicon or compound thereof

Binary compound

423413, 423463, C01B 3306

Patent

active

039594467

ABSTRACT:
A method is provided for preparing alpha silicon nitride powder in which very high purity, liquid silicon tetrachloride is reacted with an excess of ammonia gas in dry deoxygenated benzene or normal hexane at about 0.degree.C, yielding a precipitate of silicon diimide and ammonium chloride. After removal of the benzene or n-hexane from the precipitate, the mixture of silicon diimide and ammonium chloride powder is heated under a vacuum from room temperature to a temperature in the range of 1200.degree. to 1350.degree.C and maintained at the latter temperature for a period of about 2 to 8 hours. The product obtained is a high purity, submicron, alpha phase silicon nitride powder which is eminently suitable for the fabrication of dense, high strength, creep resistant and thermal shock resistant bodies for use in high performance gas turbine engines and in radome applications.

REFERENCES:
billy, M., "Preparation et Definition du Nitruve de Silicium;" Annales de Chimie Ser. 13, T4 pp. 818-819, 844-845, 850 (1959).
Lengfeld, F.; "The Action of Ammonia and Amines on Chlorides of Silicon," American Chemical Journal, pp. 531-537 Vol. 21, (1899).
Lengfeld, F., The Journal of The American Chemical Society, Vol. 21, p. 107 (1899).
Glemser, et al., Zeit. Anorganic Chem., Vol. 298, pp. 134-141 (1959).

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