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Title: Method of high purity silane preparation

Abstract

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.

Inventors:
 [1];  [2];  [2];  [2];  [2];  [2];  [2];  [2];  [2];  [2];  [2]
  1. Golden, CO
  2. Moscow, RU
Publication Date:
Research Org.:
Midwest Research Institute, Kansas City, MO (United States)
OSTI Identifier:
873162
Patent Number(s):
US 6103942
Assignee:
Midwest Research Institute (Kansas City, MO)
DOE Contract Number:  
AC36-98GO10337
Resource Type:
Patent
Country of Publication:
United States
Language:
English
Subject:
method; purity; silane; preparation; process; suitable; forming; layer; silicon; structures; various; semiconductor; devices; poly-; single; crystal; variety; applications; provided; synthesis; high-purity; starts; temperature; assisted; reaction; metallurgical; alcohol; presence; catalyst; alcoxysilanes; formed; silicon-alcohol; separated; products; purified; simultaneous; reduction; oxidation; produces; gaseous; liquid; secondary; including; active; tetra-alcoxysilanes; impurity; compounds; silicon-hydrogen; bonds; adsorption; technique; unreacted; extracted; returned; concentrated; mixture; undergoes; -20; degree; 40; 50; hours; tetra-alcoxysilane; directed; complete; hydrolysis; results; formation; industrial; silica; sol; dehydrated; silicon structures; silica sol; single crystal; semiconductor device; liquid products; semiconductor devices; liquid product; reduction reaction; crystal silicon; silicon structure; purity silane; metallurgical silicon; hydrogen bonds; layer silicon; /999/423/

Citation Formats

Tsuo, Y Simon, Belov, Eugene P, Gerlivanov, Vadim G, Zadde, Vitali V, Kleschevnikova, Solomonida I, Korneev, Nikolai N, Lebedev, Eugene N, Pinov, Akhsarbek B, Ryabenko, Eugene A, Strebkov, Dmitry S, and Chernyshev, Eugene A. Method of high purity silane preparation. United States: N. p., 2000. Web.
Tsuo, Y Simon, Belov, Eugene P, Gerlivanov, Vadim G, Zadde, Vitali V, Kleschevnikova, Solomonida I, Korneev, Nikolai N, Lebedev, Eugene N, Pinov, Akhsarbek B, Ryabenko, Eugene A, Strebkov, Dmitry S, & Chernyshev, Eugene A. Method of high purity silane preparation. United States.
Tsuo, Y Simon, Belov, Eugene P, Gerlivanov, Vadim G, Zadde, Vitali V, Kleschevnikova, Solomonida I, Korneev, Nikolai N, Lebedev, Eugene N, Pinov, Akhsarbek B, Ryabenko, Eugene A, Strebkov, Dmitry S, and Chernyshev, Eugene A. Sat . "Method of high purity silane preparation". United States. https://www.osti.gov/servlets/purl/873162.
@article{osti_873162,
title = {Method of high purity silane preparation},
author = {Tsuo, Y Simon and Belov, Eugene P and Gerlivanov, Vadim G and Zadde, Vitali V and Kleschevnikova, Solomonida I and Korneev, Nikolai N and Lebedev, Eugene N and Pinov, Akhsarbek B and Ryabenko, Eugene A and Strebkov, Dmitry S and Chernyshev, Eugene A},
abstractNote = {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.},
doi = {},
url = {https://www.osti.gov/biblio/873162}, journal = {},
number = ,
volume = ,
place = {United States},
year = {2000},
month = {1}
}

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