Process for producing liquid polysilanes and isomer enriched higher silanes

Patent metadata

Field	Value
Publication number	US-11377359-B2
Application number	US-202016827186-A
Country	US
Kind code	B2
Filing date	Mar 23, 2020
Priority date	Oct 11, 2018
Publication date	Jul 5, 2022
Grant date	Jul 5, 2022

Abstract

Synthesis of silanes with more than three silicon atoms are disclosed (i.e., SinH(2n+2) with n=4-100). More particularly, the disclosed synthesis methods tune and optimize the isomer ratio by selection of process parameters such as temperature, residence time, and the relative amount of starting compounds, as well as selection of proper catalyst. The disclosed synthesis methods allow facile preparation of silanes containing more than three silicon atoms and particularly, the silanes containing preferably one major isomer. The pure isomers and isomer enriched mixtures are prepared by catalytic transformation of silane (SiH4), disilane (Si2H6), trisilane (Si3H8), and mixtures thereof.

First claim

We claim:

1. A method of producing Si n H (2n+2) , wherein n=4-100, the method comprising:
reacting a liquid Si a H (2a+2) reactant, wherein a=1-4, with a catalyst to produce Si n H (2n+2) , wherein n>a and the catalyst is selected from:
a) a heterogeneous catalyst selected from a Group I, II or III element from the Periodic Table or oxides, alkyls, hydrides, silanides, or silyl amides thereof; or
b) a catalyst comprising a Fe halide combined with an alkyl lithium LiR or lithium amide LiNR 2 , with each R independently a C1-C4 alkyl group,
provided that the catalyst is not alumina.

2. The method of claim 1 , wherein the Si a H (2a+2) reactant is Si 3 H 8 .

3. The method of claim 1 , wherein the Si a H (2a+2) reactant is a mixture of Si 3 H 8 and Si 4 H 10 .

4. The method of claim 1 , wherein n=4-10.

5. The method of claim 4 , wherein the heterogeneous catalyst is sodium bis(2-methoxyethoxy)aluminum hydride.

6. The method of claim 4 , wherein the heterogeneous catalyst is KN(SiMe 3 ) 2 or NaN(SiMe 3 ) 2 .

7. The method of claim 4 , wherein the heterogeneous catalyst is K, Na, Na 2 O, K 2 O, or combinations thereof.

8. The method of claim 1 , wherein n=11-30.

9. The method of claim 8 , wherein the catalyst comprises a Fe halide combined with an alkyl lithium LiR or lithium amide LiNR 2 , with each R independently a C1-C4 alkyl group.

10. The method of claim 1 , further comprising fractionally distilling Si n H (2n+2) to produce a Si-containing film forming composition comprising approximately 95% w/w to approximately 100% w/w n-Si 5 H 12 .

11. The method of claim 1 , further comprising fractionally distilling Si n H (2n+2) to produce a Si-containing film forming composition comprising approximately 95% w/w to approximately 100% w/w n-Si 6 H 14 .

12. The method of claim 1 , further comprising fractionally distilling Si n H (2n+2) to produce a Si-containing film forming composition comprising approximately 95% w/w to approximately 100% w/w n-Si 7 H 16 .

13. The method of claim 1 , further comprising fractionally distilling Si n H (2n+2) to produce a Si-containing film forming composition comprising approximately 95% w/w to approximately 100% w/w n-Si 8 H 18 .

Assignees

• Air Liquide
• Air Liquide American

Inventors

• Nikiforov Grigory
• Husson Guillaume
• Itov Gennadiy
• Wang Yang

Classifications

• B01J31/22

  Organic complexes · CPC title

• C01B33/04 Primary

  Hydrides of silicon · CPC title

• C08G77/60

  in which all the silicon atoms are connected by linkages other than oxygen atoms · CPC title

• B01J31/122

  Metal aryl or alkyl compounds · CPC title

• Y02P20/582

  Recycling of unreacted starting or intermediate materials · CPC title