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Method of high purity silane preparation

United States Patent

6,103,942
August 15, 2000
View the Complete Patent at the US Patent & Trademark Office
National Renewable Energy Laboratory - Visit the NREL Technology Transfer Website
A process for the preparation of high purity silane, suitable for forming thin layer silicon structures in various semiconductor devices and high purity poly- and single crystal silicon for a variety of applications, is provided. Synthesis of high-purity silane starts with a temperature assisted reaction of metallurgical silicon with alcohol in the presence of a catalyst. Alcoxysilanes formed in the silicon-alcohol reaction are separated from other products and purified. Simultaneous reduction and oxidation of alcoxysilanes produces gaseous silane and liquid secondary products, including, active part of a catalyst, tetra-alcoxysilanes, and impurity compounds having silicon-hydrogen bonds. Silane is purified by an impurity adsorption technique. Unreacted alcohol is extracted and returned to the reaction with silicon. Concentrated mixture of alcoxysilanes undergoes simultaneous oxidation and reduction in the presence of a catalyst at the temperature -20.degree. C. to +40.degree. C. during 1 to 50 hours. Tetra-alcoxysilane extracted from liquid products of simultaneous oxidation and reduction reaction is directed to a complete hydrolysis. Complete hydrolysis of tetra-alcoxysilane results in formation of industrial silica sol and alcohol. Alcohol is dehydrated by tetra-alcoxysilane and returned to the reaction with silicon.
Tsuo; Y. Simon (Golden, CO), Belov; Eugene P. (Moscow, RU), Gerlivanov; Vadim G. (Moscow, RU), Zadde; Vitali V. (Moscow, RU), Kleschevnikova; Solomonida I. (Moscow, RU), Korneev; Nikolai N. (Moscow, RU), Lebedev; Eugene N. (Moscow, RU), Pinov; Akhsarbek B. (Moscow, RU), Ryabenko; Eugene A. (Moscow, RU), Strebkov; Dmitry S. (Moscow, RU), Chernyshev; Eugene A. (Moscow, RU)
Midwest Research Institute (Kansas City, MO)
09/ 288,005
April 8, 1999
CONTRACTUAL ORIGIN OF THE INVENTION The United States Government has rights in this invention pursuant to Contract No. DE-AC36-98GO10337 between the United States Department of Energy and the National Renewable Energy Laboratory, a division of Midwest Research Institute.