Method for producing solid electrolyte

Patent metadata

Field	Value
Publication number	US-9793574-B2
Application number	US-201414786808-A
Country	US
Kind code	B2
Filing date	Apr 21, 2014
Priority date	Apr 24, 2013
Publication date	Oct 17, 2017
Grant date	Oct 17, 2017

Abstract

A method for producing a solid electrolyte including step of bringing the following into contact with each other in a solvent having a solubility parameter of 9.0 or more: an alkali metal sulfide; one or two or more sulfur compounds selected from phosphorus sulfide, germanium sulfide, silicon sulfide and boron sulfide; and a halogen compound.

First claim

The invention claimed is:

1. A method for producing a solid electrolyte, comprising contacting the following (i), (ii) and (iii) with each other in a solvent having a solubility parameter of 9.0 or more without using a mixing and grinding apparatus:
(i) an alkali metal sulfide;
(ii) one or more sulfur compounds selected from the group consisting of phosphorus sulfide, germanium sulfide, silicon sulfide and boron sulfide; and
(iii) a halogen compound.

2. The method of claim 1 , wherein the solvent is an ether.

3. The method of claim 2 , wherein a boiling point of the solvent is 65 to 200° C.

4. The method of claim 2 , wherein the alkali metal sulfide has a particle size of 100 μm or less.

5. The method of claim 2 , wherein the alkali metal sulfide is lithium sulfide (Li 2 S) and the sulfur compound is phosphorus pentasulfide (P 2 S 5 ), and a mixing ratio of Li 2 S and P 2 S 5 (Li 2 S:P 2 S 5 ) is in a range of 74:26 to 76:24 in terms of molar ratio.

6. The method of claim 5 , wherein the halogen compound is a bromine compound.

7. The method of claim 2 , wherein the contacting is performed at a temperature of 20 to 200° C. and the contacting is performed for a time of 1 to 40 hours.

8. The method of claim 1 , wherein a boiling point of the solvent is 65 to 200° C.

9. The method of claim 1 , wherein the alkali metal sulfide has a particle size of 100 μm or less.

10. The method of claim 1 , wherein the alkali metal sulfide is lithium sulfide (Li 2 S) and the sulfur compound comprises phosphorus sulfide.

11. The method of claim 10 , wherein the halogen compound is a bromine compound.

12. The method of claim 11 , wherein the solvent is an ether.

13. The method of claim 12 , wherein the contacting is performed at a temperature of 20 to 200° C. and the contacting is performed for a time of 1 to 40 hours.

14. The method of claim 10 , wherein the halogen compound is LiBr or PBr 3 .

15. The method of claim 1 , wherein said contacting produces a solid electrolyte in which no raw materials are present.

16. The method of claim 1 , wherein the alkali metal sulfide is lithium sulfide (Li 2 S) and the sulfur compound is phosphorus pentasulfide (P 2 S 5 ), and a mixing ratio of Li 2 S and P 2 S 5 (Li 2 S:P 2 S 5 ) is in a range of 68:32 to 80:20 in terms of molar ratio.

17. The method of claim 16 , wherein the mixing ratio of Li 2 S and P 2 S 5 is in a range of 74:26 to 76:24 in terms of molar ratio.

18. A method for producing a solid electrolyte, comprising contacting the following (i), (ii) and (iii) with each other in tetrahydrofuran without using a mixing and grinding apparatus:
(i) an alkali metal sulfide;
(ii) one or more sulfur compounds selected from the group consisting of phosphorus sulfide, germanium sulfide, silicon sulfide and boron sulfide; and
(iii) a halogen compound.

19. The method of claim 18 , wherein said contacting produces a solid electrolyte in which no raw materials are present.

20. A method for producing a solid electrolyte, comprising contacting the following (i), (ii) and (iii) with each other in an ether of the formula R 1 —O—R 2 where R 1 and R 2 are independently C 1 -C 6 alkyl groups without using a mixing and grinding apparatus:
(i) an alkali metal sulfide;
(ii) one or more sulfur compounds selected from the group consisting of phosphorus sulfide, germanium sulfide, silicon sulfide and boron sulfide; and
(iii) a halogen compound.

21. The method of claim 20 , wherein the alkali metal sulfide has a particle size of 100 μm or less.

22. The method of claim 20 , wherein the alkali metal sulfide is lithium sulfide (Li 2 S), the sulfur compound is phosphorus pentasulfide (P 2 S 5 ), and a mixing ratio of Li 2 S and P 2 S 5 (Li 2 S:P 2 S 5 ) is in a range of 74:26 to 76:24 in terms of molar ratio, and the halogen compound is a bromine compound.

23. The method of claim 20 , wherein said contacting produces a solid electrolyte in which no raw materials are present.

Assignees

• Idemitsu Kosan Co

Inventors

• Seino Yoshikatsu
• Kambara Takayoshi
• Senga Minoru
• Aburatani Ryo
• Junke Tadanori
• Kimura Masakatsu

Classifications

• Y02E60/10

  Energy storage using batteries · CPC title

• C01P2006/12

  Surface area · CPC title

• C01B17/22

  Alkali metal sulfides or polysulfides · CPC title

• H01M2220/30

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

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title