# US 12,183,878 B2 · Method of manufacturing sulfide-based inorganic solid electrolyte material

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- Number: US 12,183,878 B2
- Document ID: US12183878B2
- Status: Granted
- Kind: B2
- Application number: 17/598,634
- Filed: 2020-03-06
- Published: 2022-03-17
- Granted: 2024-12-31
- Earliest claimed: 2019-03-29
- Assignees: Furukawa Co., Ltd.
- Applicants: Furukawa Co., Ltd.
- Inventors: Tetsuya Matsubara; Tatsushi Yoshida; Motoshi Tamura; Kazutomi Yamamoto
- Web page: https://patentgrep.com/patent/US12183878B2

## CPC

- C01B 25/14: Sulfur, selenium, or tellurium compounds of phosphorus
- H01M 10/0562: Solid materials
- C01B 17/22: Alkali metal sulfides or polysulfides
- C01D 15/00: Lithium compounds
- C03C 3/321: {Chalcogenide glasses, e.g. containing S, Se, Te}
- C03C 4/14: for electro-conductive glass
- C03C 10/00: Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- H01B 1/08: oxides
- H01B 1/10: sulfides
- H01M 10/052: Li-accumulators
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C03C 2204/00: Glasses, glazes or enamels with special properties
- H01M 2300/0068: inorganic
- Y02E 60/10: Energy storage using batteries
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01D: COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides C01B17/22; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia and cyanogen, containing nitrogen and other non-metals C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; phosphides C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- 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

Provided is a method of manufacturing a sulfide-based inorganic solid electrolyte material including Li, P, and S as constituent elements, the method including: a preparation step of preparing a raw material inorganic composition (A) including at least lithium sulfide, phosphorus sulfide, and a crystal nucleating agent; and a vitrification step of mechanically processing the raw material inorganic composition (A) to vitrify the raw material inorganic composition (A).

## Claims

### Claim 1

A method of manufacturing a sulfide-based inorganic solid electrolyte material including Li, P, and S as constituent elements, the method comprising:
a preparation step of preparing a raw material inorganic composition (A) including at least lithium sulfide, phosphorus sulfide, and a crystal nucleating agent; and
a vitrification step of mechanically processing the raw material inorganic composition (A) to vitrify the raw material inorganic composition (A),
wherein the crystal nucleating agent includes an inorganic solid electrolyte material; and
wherein the crystal nucleating agent includes a sulfide-based inorganic solid electrolyte material including Li, P, and S as constituent elements.

### Claim 2 (depends on 1)

The method of manufacturing a sulfide-based inorganic solid electrolyte material according to claim 1,
wherein a molar ratio (Li/P) of a content of Li to a content of P in the sulfide-based inorganic solid electrolyte material as the crystal nucleating agent is 1.0 or higher and 10.0 or lower, and a molar ratio (S/P) of a content of S to the content of P in the sulfide-based inorganic solid electrolyte material as the crystal nucleating agent is 1.0 or higher and 10.0 or lower.

### Claim 3 (depends on 1)

The method of manufacturing a sulfide-based inorganic solid electrolyte material according to claim 1,
a content of the crystal nucleating agent in the raw material inorganic composition (A) is 5 mass % or higher and 60 mass % or lower.

### Claim 4 (depends on 1)

The method of manufacturing a sulfide-based inorganic solid electrolyte material according to claim 1,
wherein the mechanical process in the vitrification step includes a mechanochemical process.

### Claim 5 (depends on 1)

The method of manufacturing a sulfide-based inorganic solid electrolyte material according to claim 1,
wherein the mechanical process in the vitrification step is performed in a dry condition.

### Claim 6 (depends on 1)

The method of manufacturing a sulfide-based inorganic solid electrolyte material according to claim 1, further comprising:
a crystallization step of heating an inorganic composition (B) obtained after the vitrification step to crystallize at least a part of the inorganic composition (B).