Method for producing alkyl-indium compounds and the use thereof

Patent metadata

Field	Value
Publication number	US-10239892-B2
Application number	US-201715460816-A
Country	US
Kind code	B2
Filing date	Mar 16, 2017
Priority date	Aug 22, 2013
Publication date	Mar 26, 2019
Grant date	Mar 26, 2019

Abstract

The invention relates to a method for the cost-effective and environmentally friendly production of alkyl indium sesquichloride in high yield and with high selectivity and purity. The alkyl indium sesquichloride produced according to the invention is particularly suitable, also as a result of the high purity and yield, for the production, on demand, of indium-containing precursors in high yield and with high selectivity and purity. As a result of the high purity, the indium-containing precursors that can be produced are particularly suitable for metal organic chemical vapor deposition (MOCVD) or metal organic vapor phase epitaxy (MOVPE). The novel method according to the invention is characterized by the improved execution of the method, in particular a rapid process control. Owing to targeted and extensive use of raw materials that are cost-effective and have a low environmental impact, the method is also suitable for use on an industrial scale.

First claim

The invention claimed is:

1. A process for preparing a compound (A) of the general formula:
R 3 In 2 Cl 3
comprising:
reacting indium with an alkyl donor by adding alkyl donor at a temperature from 150° to 235° C. in the presence of an activator to form the compound (A), the alkyl donor being alkyl chloride (RCl), and
optionally isolating compound (A) from the reaction mixture,
wherein compound (A) comprises a mixture of dialkylindium chloride (R 2 InCl) and alkylindium dichloride (RInCl 2 ) in a ratio ranging from 60:40 to 40:60,
where R is methyl or ethyl,
wherein the alkyl donor is gaseous alkyl chloride,
wherein the alkyl chloride (RCl) is introduced at a constant gauge pressure, and

wherein the alkyl chloride (RCl) is introduced at a constant gauge pressure of 1 bar to 4.5 bar.

2. The process of claim 1 , Wherein the activator is selected from the group consisting of dialkylindium chloride (R 2 InCl), alkylindium dichloride (RInCl 2 ), a mixture of trialkylindium (R 3 In) and InCl 3 , compound (A), and mixtures thereof.

3. The process of claim 1 , wherein 1.5 to 5 equivalents of alkyl donor per equivalent of indium donor are used.

4. The process of claim 1 , wherein the reaction is carried out at a temperature of about 150° C. to about 250° C.

5. The process of claim 1 , wherein compound (A) comprises a mixture of dialkylindium chloride (R 2 InCl) and alkylindium dichloride (RInCl 2 ) in a ratio of 50:50.

6. A process for preparing a compound (A) of the general formula:
R 3 In 2 Cl 3
comprising:
reacting indium with alkyl chloride (RCl) in the presence of an activator to form the compound (A), and
optionally isolating compound (A) from the reaction mixture,
wherein the activator is selected from the group consisting of compound (A), dialkylindium chloride (R 2 InCl), alkylindium dichloride (RInCl 2 ), and mixtures thereof,
wherein compound (A) comprises a mixture of dialkylindium chloride (R 2 InCl) and alkylindium dichloride (RInCl 2 ) in a ratio ranging from 60:40 to 40:60, wherein the alky chloride (RCl) is introduced in gaseous form and at a constant gauge pressure of 1 bar to 4.5 bar, and
where R is methyl or ethyl.

7. The process of claim 6 , wherein compound (A) comprises a mixture of dialkylindium chloride (R 2 InCl) and alkylindium dichloride (RInCl 2 ) in a ratio of 50:50.

8. The process of claim 6 , wherein the reaction is carried of at a temperature of about 150° C. to about 250° C.

9. The process of claim 6 , wherein 1.5 to 2.9 equivalents of alkyl donor per equivalent of indium donor are used.

10. The process of claim 6 , wherein the purity of the compound (A) is at least 95%.

11. A process for preparing a compound (A) of the general formula:
R 3 In 2 Cl 3
comprising:
reacting indium with alkyl chloride (RCl) by adding alkyl donor at a temperature from 150° to 235° C. in the presence of an activator to form the compound (A), and
optionally isolating compound (A) from the reaction mixture,
wherein the activator is selected from the group consisting of compound (A), dialkylindium chloride (R 2 InCl), alkylindium dichloride (RInCl 2 ), and mixtures thereof,
wherein compound (A) comprises a mixture of dialkylindium chloride (R 2 InCl) and alkylindium dichloride (RInCl 2 ) in a ratio ranging from 60:40 to 40:60,
wherein the alkyl chloride (RCl) is added in gaseous form and at a constant gauge pressure of 1 bar to 4.5 bar,
wherein the indium is present in liquid form and the addition of alkyl chloride is carried out at a temperature of 156° C. or more, and
where R is methyl or ethyl.

12. The process of claim 11 , wherein the reaction is carried out at a temperature of about 150° C. to about 250° C.

13. The process of claim 11 , wherein compound (A) comprises a mixture of dialkylindium chloride (R 2 InCl) and alkylindium dichloride (RInCl 2 ) in a ratio of 50:50.

14. The process of claim 11 , wherein the alkyl chloride (RCl) is introduced at a constant gauge pressure of 2 bar to 4 bar.

15. The process of claim 11 , wherein the reaction is carried out at a temperature of about 180° C. to about 230° C.

16. The process of claim 11 , wherein 1.5 to 5 equivalents of alkyl donor per equivalent of indium donor are used.

Assignees

• Umicore Ag & Co Kg

Inventors

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

Classifications

• C07F5/00 Primary

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