Preparation of Si—H containing iodosilanes via halide exchange reaction

Patent metadata

Field	Value
Publication number	US-10384944-B2
Application number	US-201715836518-A
Country	US
Kind code	B2
Filing date	Dec 8, 2017
Priority date	May 19, 2016
Publication date	Aug 20, 2019
Grant date	Aug 20, 2019

Abstract

Methods of synthesizing Si—H containing iodosilanes, such as diiodosilane or pentaiododisilane, using a halide exchange reaction are disclosed.

First claim

What is claimed is:

1. A method of synthesizing a Si—H containing iodosilane having the formula:
Si w H x R y l z   (1)

N(SiH a R b l c ) 3   (2) or

(SiH m R n l o ) 2— CH 2   (3)

wherein w is 1 to 3, x+y+z=2w+2, x is 1 to 2w+1, y is 0 to 2w+1, z is 1 to 2w+1, each a is independently 0 to 3, each b is independently 0 to 3, each c is independently 0 to 3, a+b+c =3 provided that at least one a and at least one c is 1, each m is independently 0to 3, each n is independently 0 to 3, each o is independently 0 to 3, m+n+o =3 provided that at least one m and at least one o is 1, and each R is independently a C1 to C12hydrocarbyl group, CI, Br, or a ER′ 3 group, wherein each E is independently Si or Ge and each R′ is independently H or a C1 to C12 hydrocarbyl group, the method comprising:
reacting a halosilane reactant having the formula Si w H x R y X z or N(SiH a R b X c ) 3 or (SiH m R n X o ) 2— CH 2 , wherein X is CI or Br, and w, x, y, z, a, b, c, m, n, and o are as defined above, and an alkali metal halide reactant having the formula MI, wherein M =Li, Na, K, Rb, or Cs; to produce a mixture of MX with (1), (2) or (3); and
isolating the Si—H containing iodosilane having the formula Si w H x R y l z , N(SiH a R b l c ) 3 , or (SiH m R n l o ) 2— CH 2 from the mixture,
wherein the halosilane reactant is selected from the group consisting of SiH 2 Cl 2 Si 2 HCI 5 (SiH 3 ) 2 N(SiH 2 CI) and combinations thereof.

2. The method of claim 1 , wherein M=Li.

3. The method of claim 1 , further comprising adding a non-coordinating solvent to the reacting step.

4. The method of claim 3 , wherein the non-coordinating solvent is propane, butane, pentane, hexane, heptanes, chloromethane, dichloromethane, chloroform, carbon tetrachloride, methylene chloride, acetonitrile, or combinations thereof.

5. The method of claim 1 , wherein the isolating step comprises filtering the mixture to separate MX from the Si—H containing iodosilane having the formula Si w H x R y l z or N(SiH a R b l c ) 3 .

6. The method of claim 1 , wherein the alkali metal halide reactant is Lil.

7. The method of claim 6 , wherein the halosilane reactant is SiH 2 Cl 2 .

8. The method of claim 1 , wherein the halosilane reactant is SiH 2 Cl 2 .

9. The method of claim 1 , wherein the halosilane reactant is Si 2 HCl 5 .

10. The method of claim 1 , wherein the halosilane reactant is (SiH 3 ) 2 N(SiH 2 Cl).

Assignees

• Air Liquide

Inventors

• Ritter Cole
• Itov Gennadiy
• Khandelwal Manish
• Girard Jean-Marc
• Kuchenbeiser Glenn
• Kerrigan Sean
• Zhang Peng
• Leung Larry Kit-Wing
• Blasco Nicolas

Classifications

• C23C16/4481

  by evaporation using carrier gas in contact with the source material (C23C16/4486 takes precedence) · CPC title

• C01B33/107 Primary

  Halogenated silanes · CPC title

• C23C16/448

  characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials · CPC title

• C23C16/45525

  Atomic layer deposition [ALD] · CPC title

• C23C16/30

  Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides · CPC title