Method for producing sulfide solid electrolyte

Patent metadata

Field	Value
Publication number	US-12119442-B2
Application number	US-202117317951-A
Country	US
Kind code	B2
Filing date	May 12, 2021
Priority date	May 13, 2020
Publication date	Oct 15, 2024
Grant date	Oct 15, 2024

Abstract

[Problem] To provide a method for efficiently producing a sulfide solid electrolyte using a liquid-phase method.
[Solution to Problem] A method for producing a sulfide solid electrolyte not using a pulverizer in reacting raw materials, wherein a raw material that contains lithium sulfide, a phosphorus compound and a halogen compound, and a complexing agent are stirred in a reactor while a fluid that contains the contents in the reactor is discharged outside the reactor through a discharging port arranged in the reactor and the fluid that contains the discharged contents is returned back to the reactor through a returning port arranged in the reactor to thereby make the contents-containing fluid circulate therethrough.

First claim

The invention claimed is:

1. A method for producing a sulfide solid electrolyte, comprising:
stirring a reaction fluid in a reactor; and
circulating the reaction fluid out of the reactor via a discharging port, through a circulation line, and back into the reactor via a returning port during stirring;
wherein:
the reaction fluid is obtained by combining a raw material and a complexing agent;
the raw material comprises lithium sulfide, a phosphorus compound, and a halogen compound;
the complexing agent contains a nitrogen atom; and
the circulation line is not provided with a pulverizer, and a pulverizer is not used in stirring and circulating the reaction fluid.

2. The method for producing a sulfide solid electrolyte according to claim 1 , wherein the raw material contains two or more kinds of solid compounds, and the density difference between the compound having a highest density and the compound having a lowest density is 1.0 g/cm 3 or more.

3. The method for producing a sulfide solid electrolyte according to claim 1 , wherein a circulation amount per minute of the reaction fluid is 0.01 times or more and 5.0 times or less a volume of the reaction fluid in the reactor.

4. The method for producing a sulfide solid electrolyte according to claim 1 , wherein a volume of the reactor is 30 L or more.

5. The method for producing a sulfide solid electrolyte according to claim 3 , wherein the circulation amount per minute of the reaction fluid is 3.5 L/min or more and 100 L/min or less.

6. The method for producing a sulfide solid electrolyte according to claim 1 , wherein the reaction fluid is not subjected to a pulverizing step.

7. The method for producing a sulfide solid electrolyte according to claim 1 , wherein the discharging port is arranged at a bottom of the reactor.

8. The method for producing a sulfide solid electrolyte according to claim 1 , wherein the returning port is below a top surface of the reaction fluid in the reactor during operation.

9. The method for producing a sulfide solid electrolyte according to claim 1 , wherein a temperature in the reactor is controlled.

10. The method for producing a sulfide solid electrolyte according to claim 1 , wherein one or more selected from lithium bromide (LiBr), lithium iodide (LiI) and lithium chloride (LiCl) are used as the halogen compound.

11. The method for producing a sulfide solid electrolyte according to claim 1 , wherein one or more selected from bromine (Br 2 ) and iodine (I 2 ) are used as the halogen compound.

12. The method for producing a sulfide solid electrolyte according to claim 1 , wherein the complexing agent has two or more amino groups.

13. The method for producing a sulfide solid electrolyte according to claim 1 , wherein the complexing agent is tetramethylethylenediamine.

14. A method for producing a sulfide solid electrolyte, comprising:
stirring a reaction fluid in a reactor; and
circulating the reaction fluid out of the reactor via a discharging port, through a circulation line, and back into the reactor via a returning port during stirring;
wherein:
the reaction fluid is obtained by combining a raw material and a complexing agent that reacts with the raw material to form a complex;
the raw material comprises lithium sulfide, a phosphorus compound, and a halogen compound; and
the circulation line is not provided with a pulverizer, and a pulverizer is not used in stirring and circulating the reaction fluid.

Assignees

• Idemitsu Kosan Co

Inventors

• Yamakawa Fumio
• Aida Masao
• Iseki Yusuke
• Yamada Hiroaki
• Tanaka Shinji

Classifications

• H01M2300/0068

  inorganic · CPC title

• H01M10/0562 Primary

  Solid materials · CPC title

• C01P2006/40

  Electric properties · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01P2002/72

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