Production method of solid electrolyte

Patent metadata

Field	Value
Publication number	US-10116002-B2
Application number	US-201414893424-A
Country	US
Kind code	B2
Filing date	May 30, 2014
Priority date	May 31, 2013
Publication date	Oct 30, 2018
Grant date	Oct 30, 2018

Abstract

A method of producing a sulfide-based solid electrolyte including bringing an alkali metal sulfide and a sulfur compound into contact in a mixed solvent of a hydrocarbon solvent and a polar aprotic solvent.

First claim

The invention claimed is:

1. A method of producing a sulfide-based solid electrolyte comprising:
contacting an alkali metal sulfide with a sulfur compound without pulverizing in a mixed solvent of an aromatic hydrocarbon solvent and a polar aprotic solvent, wherein:
the polar aprotic solvent is at least one of an ether solvent and a nitrile solvent, and a volume ratio of the aromatic hydrocarbon solvent to the polar aprotic solvent (aromatic hydrocarbon solvent: polar aprotic solvent) is 95:5 to 5:95.

2. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the aromatic hydrocarbon solvent is an aromatic hydrocarbon solvent represented by the following formula (1):
Ph-(R) n   (1)

wherein Ph is an aromatic hydrocarbon group, R is an alkyl group, and n is an integer selected from 1 to 5.

3. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the polar aprotic solvent is an ether solvent.

4. The method of producing a sulfide-based solid electrolyte according to claim 3 , wherein the alkali metal sulfide is lithium sulfide.

5. The method of producing a sulfide-based solid electrolyte according to claim 4 , wherein the sulfur compound is phosphorous sulfide.

6. The method for producing a sulfide-based solid electrolyte according to claim 4 , wherein the sulfur compound is phosphorous pentasulfide, and the alkali metal sulfide and the sulfur compound are brought into contact at a molar ratio of 74:26 to 76:24.

7. The method for producing a sulfide-based solid electrolyte according to claim 3 , wherein the alkali metal sulfide and the sulfur compound are brought into contact at a molar ratio of 74:26 to 76:24.

8. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the alkali metal sulfide is lithium sulfide.

9. The method of producing a sulfide-based solid electrolyte according to claim 8 , wherein the sulfur compound is phosphorous sulfide.

10. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein the alkali metal sulfide and the sulfur compound are brought into contact at a molar ratio of 74:26 to 76:24.

11. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the contacting is carried out at a temperature of 20° C. or higher and 60° C. or lower.

12. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the aromatic hydrocarbon solvent is toluene, xylene, or ethylbenzene.

13. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the polar aprotic solvent comprises an ether solvent selected from anisole, diethoxyethane, diethyl ether, and tetrahydrofuran.

14. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the polar aprotic solvent comprises a cyclic ether solvent.

15. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the polar aprotic solvent comprises tetrahydrofuran.

16. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein the polar aprotic solvent comprises isobutyronitrile or acetonitrile.

17. The method of producing a sulfide-based solid electrolyte according to claim 1 , wherein contacting the alkali metal sulfide with the sulfur compound comprises contacting the alkali metal sulfide, the sulfur compound, and a halogen compound.

18. The method of producing a sulfide-based solid electrolyte according to claim 1 , further comprising drying a reaction product obtained by contacting the alkali metal sulfide with the sulfur compound to remove the mixed solvent.

19. The method of producing a sulfide-based solid electrolyte according to claim 1 , further comprising crystallizing a reaction product obtained by contacting the alkali metal sulfide with the sulfur compound by a heat treatment.

20. The method of producing a sulfide-based solid electrolyte according to claim 1 , further comprising drying and crystallizing a reaction product obtained by contacting the alkali metal sulfide with the sulfur compound in one heating step.

Assignees

• Idemitsu Kosan Co

Inventors

• Sato Koichi
• Senga Minoru
• Seino Yoshikatsu

Classifications

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title

• C01B17/22

  Alkali metal sulfides or polysulfides · CPC title

• H01M10/052

  Li-accumulators · CPC title

• H01M2220/30

  Batteries in portable systems, e.g. mobile phone, laptop · CPC title

• H01M2300/0068

  inorganic · CPC title