Method for producing cyclic silane using concentration method
View Patent ↗A cyclic silane having high purity, a composition containing a polysilane obtained by polymerization of the cyclic silane, and a silicon thin film are disclosed. A method for producing a cyclic silane of the formula (SiH 2 ) n , where n is an integer of 4 to 6, includes reacting a cyclic silane compound of the formula (SiR 1 R 2 ) n (where R 1 and R 2 are each a hydrogen atom, a C 1-6 alkyl group, or a substituted or unsubstituted phenyl group) with a hydrogen halide in the presence of an aluminum halide to obtain a cyclic silane of the formula (SiR 3 R 4 ) n (where R 3 and R 4 are each a halogen atom), and then distilling the solution, and reducing the cyclic silane of the formula (SiR 3 R 4 ) n with hydrogen or lithium aluminum hydride. The distillation may be carried out at a temperature of 40° C. to 80° C. under a reduced pressure of 0 to 30 Torr.
1. A method for producing a cyclic perhydrosilane of Formula (3):
(SiH 2 ) n (3)
wherein n is an integer of 4 to 6, comprising:
reacting a cyclic silane compound of Formula (1):
(SiR 1 R 2 ) n (1)
wherein R 1 and R 2 are each a C 1-6 alkyl group or a substituted or unsubstituted phenyl group, and n is an integer of 4 to 6, with a hydrogen halide in an alkane, cycloalkane, arene or alkylarene solvent having 6-10 carbon atoms in a presence of an aluminum halide to obtain a solution containing a cyclic perhalosilane compound of Formula (2):
(SiR 3 R 4 ) n (2)
wherein R 3 and R 4 are each a halogen atom, and n is an integer of 4 to 6, then
distilling the solution including the cyclic perhalosilane compound of Formula (2) to purify the cyclic perhalosilane compound of Formula (2), and
dissolving the purified cyclic perhalosilane compound of Formula (2) in an organic solvent, and reducing the purified cyclic perhalosilane compound of Formula (2) with hydrogen or lithium aluminum hydride.
2. The method according to claim 1 , wherein both R 1 and R 2 are phenyl groups, and the alkane, cycloalkane, arene or alkylarene solvent is the cycloalkane, benzene or toluene.
3. The method according to claim 1 , wherein both R 3 and R 4 are chlorine atoms, and the alkane, cycloalkane, arene or alkylarene solvent is the cycloalkane, benzene or toluene.
4. The method according to claim 1 , wherein the cyclic perhydrosilane of Formula (3) contains cyclopentasilane in an amount of 90% or more by moles.
5. The method according to claim 1 , wherein the solution is distilled at a temperature of 40° C. to 80° C.
6. The method according to claim 5 , wherein the solution is distilled at a pressure of 0 to 30 Torr.
7. The method according to claim 2 , wherein the solution is distilled at a temperature of 40° C. to 80° C.
8. The method according to claim 7 , wherein the solution is distilled at a pressure of 0 to 30 Torr.
9. The method according to claim 3 , wherein the solution is distilled at a temperature of 40° C. to 80° C.
10. The method according to claim 9 , wherein the solution is distilled at a pressure of 0 to 30 Torr.
11. The method according to claim 4 , wherein the solution is distilled at a temperature of 40° C. to 80° C. and a pressure of 0 to 30 Torr.
12. The method according to claim 6 , wherein the pressure is 5 to 30 Torr, and the solution is distilled for 2 to 24 hours.
13. The method according to claim 8 , wherein the pressure is 5 to 30 Torr, and the solution is distilled for 2 to 24 hours.
14. The method according to claim 2 , wherein the alkane, cycloalkane, arene or alkylarene solvent is cyclohexane, and distilling the solution removes cyclohexylbenzene from the cyclic perhalosilane compound of Formula (2).
15. The method according to claim 1 , wherein reducing the purified cyclic perhalosilane compound of Formula (2) with hydrogen or lithium aluminum hydride produces the cyclic perhydrosilane of Formula (3), and the method further comprises, after reducing the purified cyclic perhalosilane compound of Formula (2) with hydrogen or lithium aluminum hydride, distilling the cyclic perhydrosilane of Formula (3).
16. The method according to claim 4 , wherein the cyclic perhydrosilane of Formula (3) contains cyclopentasilane in an amount of 99% or more by moles.
17. The method according to claim 1 , further comprising reacting a compound of the formula R 1 R 2 SiX 2 with an alkali metal in an organic solvent, wherein X is a halogen atom, to obtain the cyclic silane of the Formula (1).
18. The method according to claim 1 , further comprising polymerizing the cyclic perhydrosilane of Formula (3) using a catalyst to obtain a polysilane.
19. The method according to claim 18 , wherein the catalyst comprises a palladium catalyst supported on a polymer.
20. The method according to claim 1 , further comprising, after reducing the purified cyclic perhalosilane compound of Formula (2) with hydrogen or lithium aluminum hydride, washing the cyclic perhydrosilane of Formula (3) with water.