Method for purifying dodecacarbonyl triruthenium

Patent metadata

Field	Value
Publication number	US-9783429-B2
Application number	US-201515312355-A
Country	US
Kind code	B2
Filing date	Jun 2, 2015
Priority date	Jun 4, 2014
Publication date	Oct 10, 2017
Grant date	Oct 10, 2017

Abstract

An object of the present invention is to provide a purification method to give dodecacarbonyl triruthenium (DCR) which serves as a raw material for chemical vapor deposition and does not cause the contamination of a thin film with impurities even when used to form a ruthenium thin film. The present invention relates to a method in which the dissolved oxygen concentration in the solvent is made 0.2 mg/L or less in at least a dissolution stage, and an organic ruthenium compound including DCR as a raw material for chemical vapor deposition is purified by a recrystallization method. The present invention allows a trace amount of impurities to be separated from DCR. When a ruthenium thin film is formed by use of DCR thus obtained, the formed film is hardly contaminated with impurities. Additionally, the purification method of the present invention is also applicable for recovering/purifying DCR after being used for the formation of a ruthenium thin film.

First claim

The invention claimed is:

1. A method for purifying dodecacarbonyl triruthenium (DCR), for purifying, by a recrystallization method, an organic ruthenium compound including DCR represented by a following formula as a raw material for chemical vapor deposition:

the method comprises a recrystallization step of purifying DCR by a recrystallization method,
the recrystallization step includes a dissolution stage of dissolving DCR in a solvent, a precipitation stage of precipitating DCR from the solvent, and a recovery stage of recovering the precipitated DCR, wherein
at least the dissolution stage is performed with a dissolved oxygen concentration in the solvent being 0.2 mg/L or less.

2. The method for purifying DCR according to claim 1 , wherein at least the dissolution stage is performed in an atmosphere having an oxygen concentration of 0.1 vol % or less.

3. The method for purifying DCR according to claim 1 , wherein the recrystallization step further includes a drying stage of drying the recovered DCR, and the drying stage is performed at a reduced pressure of 500 Pa or less.

4. The method for purifying DCR according to claim 1 , wherein, in the dissolution stage, DCR is dissolved in at least one solvent selected from acetone, dichloromethane, DMF, ethyl acetate, chloroform, toluene, acetonitrile, and THF.

5. The method for purifying DCR according to claim 1 , further comprising a stage of filtering the solvent with dissolved DCR after the dissolution stage and before the precipitation stage.

6. The method for purifying DCR according to claim 1 , wherein the dissolution stage is performed at 55 to 130° C.

7. The method for purifying DCR according to claim 3 , wherein the drying stage is performed at 0 to 40° C.

8. The method for purifying DCR according to claim 1 , wherein the recrystallization step is performed after a sublimation step of purifying DCR by a sublimation method.

9. The method for purifying DCR according to claim 2 , wherein the recrystallization step further includes a drying stage of drying the recovered DCR, and the drying stage is performed at a reduced pressure of 500 Pa or less.

10. The method for purifying DCR according to claim 2 , wherein, in the dissolution stage, DCR is dissolved in at least one solvent selected from acetone, dichloromethane, DMF, ethyl acetate, chloroform, toluene, acetonitrile, and THF.

11. The method for purifying DCR according to claim 3 , wherein, in the dissolution stage, DCR is dissolved in at least one solvent selected from acetone, dichloromethane, DMF, ethyl acetate, chloroform, toluene, acetonitrile, and THF.

12. The method for purifying DCR according to claim 2 , further comprising a stage of filtering the solvent with dissolved DCR after the dissolution stage and before the precipitation stage.

13. The method for purifying DCR according to claim 3 , further comprising a stage of filtering the solvent with dissolved DCR after the dissolution stage and before the precipitation stage.

14. The method for purifying DCR according to claim 4 , further comprising a stage of filtering the solvent with dissolved DCR after the dissolution stage and before the precipitation stage.

15. The method for purifying DCR according to claim 2 , wherein the dissolution stage is performed at 55 to 130° C.

16. The method for purifying DCR according to claim 3 , wherein the dissolution stage is performed at 55 to 130° C.

17. The method for purifying DCR according to claim 4 , wherein the dissolution stage is performed at 55 to 130° C.

18. The method for purifying DCR according to claim 5 , wherein the dissolution stage is performed at 55 to 130° C.

19. The method for purifying DCR according to claim 4 , wherein the drying stage is performed at 0 to 40° C.

20. The method for purifying DCR according to claim 2 , wherein the recrystallization step is performed after a sublimation step of purifying DCR by a sublimation method.

Assignees

• Tanaka Precious Metal Ind

Inventors

• Nakagawa Hirofumi
• Ishizaka Tasuku
• Ishida Hirofumi
• Kumakura Akiko

Classifications

• C01G55/008 Primary

  Carbonyls · CPC title

• C07F15/00

  Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table · CPC title

• C01P2006/80

  Compositional purity · CPC title

• B01D9/00

  Crystallisation (crystallisation directly from the vapour phase B01D7/02; making single crystals C30B {; crystallisation as part of the Bayer process also classified in C01F7/14}) · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title