# US 12,119,442 B2 · Method for producing sulfide solid electrolyte

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- Number: US 12,119,442 B2
- Document ID: US12119442B2
- Status: Granted
- Kind: B2
- Application number: 17/317,951
- Filed: 2021-05-12
- Published: 2021-12-30
- Granted: 2024-10-15
- Earliest claimed: 2020-05-13
- Assignees: Idemitsu Kosan Co., Ltd.
- Applicants: Idemitsu Kosan Co., Ltd.
- Inventors: Fumio Yamakawa; Masao Aida; Yusuke Iseki; Hiroaki Yamada; Shinji Tanaka
- Web page: https://patentgrep.com/patent/US12119442B2

## CPC

- H01M 10/0562: Solid materials
- C01B 17/22: Alkali metal sulfides or polysulfides
- C01B 25/14: Sulfur, selenium, or tellurium compounds of phosphorus
- H01B 1/06: mainly consisting of other non-metallic substances
- H01B 13/00: Apparatus or processes specially adapted for manufacturing conductors or cables
- C01P 2002/54: one element only
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/82: by IR- or Raman-data
- C01P 2006/40: Electric properties
- H01M 2300/0068: inorganic
- Y02E 60/10: Energy storage using batteries
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## 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.

## Claims

### Claim 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.

### Claim 2 (depends on 1)

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/cm3 or more.

### Claim 3 (depends on 1)

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.

### Claim 4 (depends on 1)

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

### Claim 5 (depends on 3)

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.

### Claim 6 (depends on 1)

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

### Claim 7 (depends on 1)

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

### Claim 8 (depends on 1)

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.

### Claim 9 (depends on 1)

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

### Claim 10 (depends on 1)

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.

### Claim 11 (depends on 1)

The method for producing a sulfide solid electrolyte according to claim 1, wherein one or more selected from bromine (Br2) and iodine (I2) are used as the halogen compound.

### Claim 12 (depends on 1)

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

### Claim 13 (depends on 1)

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

### Claim 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.
