Preparation of triiodosilanes

Patent metadata

Field	Value
Publication number	US-11203604-B2
Application number	US-201916706347-A
Country	US
Kind code	B2
Filing date	Dec 6, 2019
Priority date	Dec 10, 2018
Publication date	Dec 21, 2021
Grant date	Dec 21, 2021

Abstract

Provided is a process for preparing certain silane precursor compounds, e.g., triiodosilane from trichlorosilane utilizing lithium iodide in powder form and catalyzed by tertiary amines. The process provides triiodosilane in high yields and high purity. Triiodosilane is a precursor compound useful in the atomic layer deposition of silicon onto various microelectronic device structures.

First claim

We claim:

1. A process for preparing compounds of the formula (R 1 ) y Si(I) z , wherein each R 1 is independently chosen from hydrogen, C 1 -C 9 alkyl, vinyl, or a C 2 -C 4 alkynyl group, y is 0, 1, 2, or 3, and z is 1, 2, 3, or 4, and wherein y+z is equal to 4, which comprises contacting a compound of the formula (R 1 ) y Si(Cl) z with lithium iodide in the presence of a tertiary amine, tetraalkylammonium halide, or tetraalkylphosphonium halide wherein the lithium iodide is in the form of a powder having an average particle size of less than about 2 mm.

2. The process of claim 1 , wherein the particle size of the lithium iodide powder is less than about 1 mm.

3. The process of claim 1 , wherein the particle size of the lithium iodide powder is less than about 0.5 mm.

4. The process of claim 1 , wherein the particle size of the lithium iodide powder is less than about 0.1 mm.

5. The process of claim 1 , wherein the compound of the formula (R 1 ) y Si(I) z is triiodosilane.

6. The process of claim 1 , wherein the compound of the formula (R 1 ) y Si(I) z is chosen from CH 3 Si(I) 3 , CH 3 CH 2 Si(I) 3 , CH 3 CH 2 CH 2 Si(I) 3 , CH 3 CH 2 CH 2 CH 2 Si(I) 3 , (CH 3 ) 2 CHSi(I) 3 , CH 3 CH 2 (CH 3 )CHSi(I) 3 , (CH 3 ) 3 CSi(I) 3 , CH 3 CH 2 CH 2 CH 2 Si(I) 3 , (CH 3 ) 3 CCH 2 Si(I) 3 , CH 2 ═CHSi(I) 3 , CH≡CSi(I) 3 , CH≡CCH 2 Si(I) 3 , CH 3 C≡CSi(I) 3 , CH≡CCH 2 CH 2 Si(I) 3 , CH 3 CH≡CCH 2 Si(I) 3 , CH 2 CH 2 CH 2 C≡CSi(I) 3 , (CH 3 ) 2 Si(I) 2 , CH 3 CH 2 ) 2 Si(I) 2 , (CH 3 CH 2 CH 2 ) 2 Si(I) 2 , (CH 3 CH 2 CH 2 CH 2 ) 2 Si(I) 2 , ((CH 3 ) 2 CH) 2 Si(I) 2 , (CH 3 CH 2 (CH 3 )CH) 2 Si(I) 2 , ((CH 3 ) 3 C) 2 Si(I) 2 , (CH 3 CH 2 CH 2 CH 2 ) 2 Si(I) 2 , ((CH 3 ) 3 CCH 2 ) 2 Si(I) 2 , (CH 2 ═CH) 2 Si(I) 2 , (CH≡C) 2 Si(I) 2 , (CH≡CCH 2 ) 2 Si(I) 2 , (CH 3 C≡C) 2 Si(I) 2 , (CH≡CCH 2 CH 2 ) 2 Si(I) 2 , (CH 3 CH≡CCH 2 ) 2 Si(I) 2 , (CH 2 CH 2 CH 2 C≡C) 2 Si(I) 2 , (CH 3 ) 3 SiI, (CH 3 CH 2 ) 3 SiI, (CH 3 CH 2 CH 2 ) 3 SiI, (CH 3 CH 2 CH 2 CH 2 ) 3 SiI, ((CH 3 ) 2 CH) 3 SiI, (CH 3 CH 2 (CH 3 )CH) 3 SiI, ((CH 3 ) 3 C) 3 SiI, (CH 3 CH 2 CH 2 CH 2 ) 3 SiI, ((CH 3 ) 3 CCH 2 ) 3 SiI, (CH 2 ═CH) 3 SiI, (CH≡C) 3 SiI, (CH≡CCH 2 ) 3 SiI, (CH 3 C≡C) 3 Si, (CH≡CCH 2 CH 2 ) 3 SiI, (CH 3 CH≡CCH 2 ) 3 SiI, and (CH 2 CH 2 CH 2 C≡C) 3 SiI.

7. The process of claim 1 , wherein the tertiary amine is a mono-amine.

8. The process of claim 7 , wherein the tertiary amine is triethylamine.

9. The process of claim 1 , wherein the tertiary amine has the formula:

wherein each R is independently hydrogen or a C 1 -C 9 alkyl group, m is an integer of from 1 to 4, and n is an integer of from 2 to 5.

10. The process of claim 9 , wherein the tertiary amine has the formula

wherein each R is independently hydrogen or a C 1 -C 9 alkyl group.

11. The process of claim 9 , wherein the tertiary amine has the formula

wherein each R is independently hydrogen or a C 1 -C 9 alkyl group.

12. The process of claim 9 , wherein each R is independently chosen from methyl and ethyl.

13. The process of claim 1 , wherein the tertiary amine is N,N,N′,N′-tetraethylene diamine.

14. The process of claim 1 , wherein the tertiary amine is N,N,N′,N″,N″-pentamethyldiethylenetriamine.

15. The process of claim 1 , wherein the tetraalkylammonium chloride is tetrabutylammonium chloride.

16. The process of claim 1 , wherein the tetraalkylphosphonium chloride is tetrabutylphosphonium chloride.

Assignees

• Entegris Inc

Inventors

• Kuiper David
• Khandelwal Manish
• Cameron Thomas M
• Baum Thomas H
• Cleary John

Classifications

• C07F7/123 Primary

  by reactions involving the formation of Si-halogen linkages · CPC title

• C07F7/081

  comprising at least one atom selected from the elements N, O, halogen, S, Se or Te · CPC title

• C07F7/0827 Primary

  Syntheses with formation of a Si-C bond · CPC title

• C07F7/083 Primary

  Syntheses without formation of a Si-C bond · CPC title