High purity trisilylamine, methods of making, and use
A composition, comprising: trisilylamine and less than 5 ppmw of halogen. A method of making a silylamine comprising combining ammonia and a compound comprising aminosilane functionality, where the compound comprising aminosilane functionality is according to formula (I) R 1 N(R 2 )a(SiH 3 ) 2−a (I), where R 1 is an organic polymer, a C- 1-20 hydrocarbyl group or —SiR 3 3 1 , where R 3 is C 1-6 hydrocarbyl, R 2 is a C- 1-20 hydrocarbyl group, H, or —SiR 3 3 1 , where R 3 is as defined above, subscript a is 0 or 1, provided that R 1 and R 2 may be the same or different except if R 1 is phenyl, R 2 is not phenyl, under sufficient conditions to cause a reaction to form a silylamine and a byproduct.
1. A method of making a silylamine, the method comprising: combining ammonia and a compound comprising aminosilane functionality, where the compound comprising aminosilane functionality is according to formula (I)
R 1 N(R 2 ) a (SiH 3 ) 2−a (I),
where R 1 is an organic polymer, a C 1-20 hydrocarbyl group or —SiR 3 3 , where R 3 is C 1-6 hydrocarbyl, R 2 is a C 1-20 hydrocarbyl group, H, or —SiR 3 3 1 , where R 3 is as defined above, subscript a is 0 or 1, provided that R 1 and R 2 may be the same or different except if R 1 is phenyl, R 2 is not phenyl,
under sufficient conditions to cause a reaction to form a silylamine and a byproduct; and
wherein the sufficient conditions include a temperature from −20° C. to 150° C. and a pressure greater than 102 kPa.
2. A method according to claim 1 wherein the silylamine is trisilylamine, N(SiH 3 ) 3 .
3. A method as in claim 1 , wherein the temperature is from 0° C. to 75° C.
4. A method as in claim 1 , wherein R 1 is alkyl and each R 2 is independently R 1 or H.
5. A method as in claim 4 , wherein R 1 is branched alkyl having 3 to 6 carbon atoms, and each R 2 is independently R 1 or H.
6. A method according to claim 1 , wherein the combining is in a pressure reactor.
7. A method as in claim 1 , wherein the pressure of the sufficient conditions is up to 300 kPa.
8. A method of making a silylamine, the method comprising: combining ammonia and a compound comprising aminosilane functionality, wherein the compound comprising aminosilane functionality is an organic polymer comprising one or more groups according to formula (II)
—N(R 2 ) a (H) b (SiH 3 ) 2−a−b (II)
where R 2 is H, C 1-20 hydrocarbyl, or —Si(R 3 ) 3 , where R 3 is C 1-6 hydrocarbyl, subscript a and b independently are 0 or 1, and a+b<2, where the groups according to formula (II) are in pendant, terminal, or pendant and terminal positions on the organic polymer.