Method for producing sulfide solid electrolyte having argyrodite-type crystal structure

Patent metadata

Field	Value
Publication number	US-11916191-B2
Application number	US-201916976976-A
Country	US
Kind code	B2
Filing date	Mar 1, 2019
Priority date	Mar 5, 2018
Publication date	Feb 27, 2024
Grant date	Feb 27, 2024

Abstract

A method for producing a sulfide solid electrolyte having an argyrodite-type crystal structure may involve: mixing a raw material containing elemental phosphorus at an integrated power of 0.5 kWh/kg or more, and heat-treating a precursor obtained in the mixing at 350 to 500° C.

First claim

The invention claimed is:

1. A method for producing a sulfide solid electrolyte having an argyrodite crystal structure, the method comprising:
mixing a raw material comprising elemental phosphorus at an integrated power of 0.5 kWh/kg or more; and
heat-treating a precursor obtained in the mixing at a temperature in a range of from 350 to 500° C.

2. The method of claim 1 , wherein the integrated power in the mixing of the raw material is in a range of from 0.5 to 20 kWh/kg.

3. The method of claim 1 , wherein the raw material further comprises elemental sulfur.

4. The method of claim 1 , wherein the raw material further comprises
lithium and
chlorine and/or bromine.

5. The method of claim 1 , wherein the precursor comprises P 2 S 6 4− glass.

6. The method of claim 5 , wherein, in a solid 31 P-NMR measurement of the precursor, a peak intensity of peaks observed in a range of from 30 to 60 ppm is less than a peak intensity of the P 2 S 6 4− glass.

7. The method of claim 5 , wherein the precursor further comprises P 2 S 7 4− glass.

8. The method of claim 5 , wherein, in a solid 31 P-NMR measurement of the precursor, a peak intensity of P 2 S 6 4− glass or PS 4 3− glass is the largest among the peaks observed in a range of from 30 to 120 ppm.

9. The method of claim 1 , wherein the heat-treating is carried out under atmospheric pressure and in an inert atmosphere.

10. A method for producing a sulfide solid electrolyte having an argyrodite crystal structure, the method comprising:
mixing a raw material comprising elemental phosphorus, to obtain a precursor comprising P 2 S 6 4− glass; and
heat-treating the precursor at a temperature of from 350 to 500° C.

11. The method of claim 1 , wherein a weight loss ratio of the precursor at 600° C. in thermogravimetry is 1.5% or less.

12. The method of claim 5 , wherein the precursor further comprises PS 4 3− glass.

13. The method of claim 1 , wherein the temperature of the heat-treating is at least 360° C.

14. The method of claim 1 , wherein the temperature of the heat-treating is in a range of from 380 to 450° C.

15. The method of claim 1 , wherein the heat-treating is conducted for a tinge in a range of from 0.5 to 12 hours.

16. The method of claim 1 , wherein the heat-treating is conducted for a time in a range of from 1 to 8 hours.

17. The method of claim 1 , wherein the integrated power in the mixing of the raw material is in a range of from 1 to 10 kWh/kg.

18. The method of claim 17 , wherein the integrated power is no more than 7 kWh/kg, and
wherein the mixing is conducted for a mixing time in a range of from 10 minutes to 10 hours.

Assignees

• Idemitsu Kosan Co

Inventors

• Kambara Takayoshi
• Senga Minoru
• Kondo Katsuhito
• Masuda Naoya
• Kimpara Hironari
• Utsuno Futoshi
• Tamura Hiroyuki

Classifications

• H01M10/0562 Primary

  Solid materials · CPC title

• C01B25/14

  Sulfur, selenium, or tellurium compounds of phosphorus · CPC title

• C01P2002/30

  Three-dimensional structures · CPC title

• C01P2002/72

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

• C01P2002/86

  by NMR- or ESR-data · CPC title