Method for producing trialkylgallium compounds and the use thereof

Patent metadata

Field	Value
Publication number	US-10428089-B2
Application number	US-201515126043-A
Country	US
Kind code	B2
Filing date	Mar 12, 2015
Priority date	Mar 14, 2014
Publication date	Oct 1, 2019
Grant date	Oct 1, 2019

Abstract

The trialkylgallium compounds obtained are very pure and so are particularly useful as organometallic precursor for metal-organic chemical vapor deposition (MOCVD) or metal-organic vapor phase epitaxy (MOVPE) in semiconductor and microsystem technology.

First claim

The invention claimed is:

1. A process for preparing a compound (A), the formula
RGaCl 2 or a mixture of RGaCl 2 with R 2 GaCl,
comprising the reaction steps of
a1) reacting gallium with a gaseous alkyl donor in the presence of an activator to form compound (A) at a pressure of 1.1 bar to 10 bar,
a2) and optionally isolating said compound (A) from the reaction mixture,
where R is branched or unbranched alkyl of 1 to 4 carbon atoms and
wherein the activator is selected from the group consisting of R 2 GaCl, R 3 Ga 2 Cl 3 , RGaCl 2 and mixtures thereof, or is a mixture of R 2 GaCl and RGaCl 2 , or wherein the reaction product, compound (A), is itself used as activator.

2. The process according to claim 1 , wherein the alkyl donor has the general formula:
RCl
where R is as defined above.

3. The process according to claim 1 , wherein R is methyl.

4. The process according to claim 1 , wherein R is ethyl.

5. The process according to claim 1 , wherein the molar ratio of alkyl donor to gallium is at least 1.4:1.

6. The process according to claim 1 , wherein a premix of gallium and activator is initially charged to the reaction vessel in reaction step a1) and the alkyl donor is added subsequently.

7. The process according to claim 1 , wherein reaction step a1) is carried out in the absence of organic solvents.

8. A process for preparing a compound (B) of the general formula:
R 3 Ga
which process comprises providing a compound (A) of the formula
RGaCl 2 or a mixture of RGaCl 2 with R 2 GaCl,

comprising the reaction steps of
a1) reacting gallium with a gaseous alkyl donor in the presence of an activator to form compound (A),
wherein the activator is selected from R 2 GaCl, R 3 Ga 2 Cl 3 , RGaCl 2 and mixtures thereof, or is a mixture of R 2 GaCl and RGaCl 2 , or wherein the reaction product, compound (A), is itself used as activator,

a2) and optionally isolating said compound (A) from the reaction mixture,
where R is branched or unbranched alkyl of 1 to 4 carbon atoms
and
b) reacting said compound (A) with a metal alkyl component to obtain a compound (B) of the general formula:
R 3 Ga

where R is defined above and wherein the metal alkyl component is RMgCl, R 2 AlCl, R 3 Al 2 Cl 3 or RLi.

9. The process according to claim 8 , wherein the metal alkyl component is R 3 Al 2 Cl 3 .

10. The process according to claim 8 , wherein the metal alkyl component is Me 3 Al 2 Cl 3 or Et 3 Al 2 Cl 3 .

11. The process according to claim 8 , wherein an auxiliary base is also added in reaction step b), wherein the auxiliary base is selected from the group consisting of sodium chloride, potassium chloride, aluminium chloride and mixtures thereof.

12. The process according to claim 1 , wherein said compound (A) is a mixture of the compounds R 2 GaCl and RGaCl 2 , where R is as defined above, and the ratio of R 2 GaCl to RGaCl 2 is in the range from 10:90 to 90:10 based on the molar amounts.

13. The process according to claim 1 , wherein said compound (A) is a mixture of the compounds R 2 GaCl and RGaCl 2 , where R is as defined above, and the ratio of R 2 GaCl to RGaCl 2 is in the range from 10:90 to 50:50 based on the molar amounts.

14. The process according to claim 1 , wherein said compound (A) is a mixture of the compounds R 2 GaCl and RGaCl 2 , where R is as defined above, and the ratio of R 2 GaCl to RGaCl 2 is in the range from 20:80 to 40:60 based on the molar amounts.

15. The process according to claim 10 , wherein the metal alkyl component is Me 3 Al 2 Cl 3 .

16. The process according to claim 10 , wherein the metal alkyl component is Et 3 Al 2 Cl 3 .

17. The process according to claim 1 , wherein the gaseous alky donor is condensed in the reaction so that the alkyl donor is liquefied.

18. A process for preparing a compound (A), which is either of the general formula RGaCl 2 or is a mixture of RGaCl 2 with R 2 GaCl,
comprising the reaction steps of
a1) reacting gallium with a gaseous alkyl donor in the presence of an activator to form compound (A), wherein the alkyl donor is introduced during the course of the reaction at a rate just equal to the consumption, maintaining a constant reaction pressure of 2 to 10 bar,
a2) and optionally isolating said compound (A) from the reaction mixture, where R is branched or unbranched alkyl of 1 to 4 carbon atoms and
wherein the activator is selected from R 2 GaCl, R 3 Ga 2 Cl 3 , RGaCl 2 and mixtures thereof, or is a mixture of R 2 GaCl and RGaCl 2 , or wherein the reaction product, compound (A), is itself used as activator.

19. The process according to claim 18 , wherein the reaction pressure is from 2 to 6 bar.

20. The process of claim 1 wherein some of the reaction product is removed from the reactor and the reaction for preparing compound (A) is continued after fresh gallium has been added.

21. A process of preparing a compound (B) of the general formula
R 3 Ga,
comprising
comprising the reaction steps of
a1) reacting gallium with a gaseous alkyl donor in the presence of an activator to form compound (A) at a pressure of 1.1 bar to 10 bar,
a2) and optionally isolating said compound (A) from the reaction mixture,
where R is branched or unbranched alkyl of 1 to 4 carbon atoms and

wherein the activator is selected from the group consisting of R 2 GaCl, R 3 Ga 2 Cl 3 , RGaCl 2 and mixtures thereof, or is a mixture of R 2 GaCl and RGaCl 2 , or wherein the reaction product, compound (A), is itself used as activator
and
b) reacting said compound (A) with a metal alkyl component to obtain a compound (B) of the general formula:
R 3 Ga

where R is a branched or unbranched alkyl of 1 to 4 carbon atoms.

Assignees

• Umicore Ag & Co Kg

Inventors

• Schorn Wolf
• Sundermeyer Jörg
• Frey Annika
• Karch Ralf
• Rivas-Nass Andreas
• Woerner Eileen
• Doppiu Angelino

Classifications

• H10P14/24

  using chemical vapour deposition [CVD] · CPC title

• C23C16/18

  from metallo-organic compounds · CPC title

• C07F5/00 Primary

  Compounds containing elements of Groups 3 or 13 of the Periodic Table · CPC title

• H01L21/0262

  Electricity · mapped topic