# US 10,865,108 B2 · Complex comprising sulfur, a method for manufacturing the same, and a method for manufacturing a solid electrolyte

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- Number: US 10,865,108 B2
- Document ID: US10865108B2
- Status: Granted
- Kind: B2
- Application number: 15/839,400
- Filed: 2017-12-12
- Published: 2018-06-14
- Granted: 2020-12-15
- Earliest claimed: 2016-12-14
- Assignees: Idemitsu Kosan Co., Ltd.
- Applicants: Idemistu Kosan Co., Ltd.
- Inventors: Minoru Senga; Takashi Umeki
- Web page: https://patentgrep.com/patent/US10865108B2

## CPC

- C01B 17/22: Alkali metal sulfides or polysulfides
- C01B 17/16: Hydrogen sulfides
- C01D 15/04: Halides
- H01M 4/5815: {Sulfides}
- C01P 2002/70: defined by measured X-ray, neutron or electron diffraction data
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- H01M 10/0562: Solid materials
- 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}
- 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)
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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

To provide a sulfur-containing complex having few impurities, a method for producing the complex at a higher production efficiency, and a method for producing a solid electrolyte using the complex, a sulfur-containing complex, containing a lithium sulfide and a lithium halide, exhibiting, in X-ray diffractometry using a CuKα ray, the diffraction angle of the peak of lithium halide shifting toward the diffraction angle of the peak of lithium sulfide, and not containing an oxygen-containing lithium halide represented by Li3OX (where X represents a halogen element) is provided. And a production method for a sulfur-containing complex including heating a solution containing a lithium hydrosulfide and a lithium halide in the presence of hydrogen sulfide is also provided.

## Claims

### Claim 1

A method for producing a sulfur-containing complex, comprising:
obtaining a lithium hydrosulfide solution by supplying hydrogen sulfide to a lithium hydroxide solution, wherein the lithium hydroxide solution substantially contains no lithium halide;
mixing the lithium hydrosulfide solution and a lithium halide to provide a mixture comprising lithium hydrosulfide, lithium halide and a solvent;
obtaining a powder by evaporating the solvent from the mixture by supplying hydrogen sulfide to the mixture while heating the mixture; and
heating the powder while supplying hydrogen sulfide.

### Claim 2 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, further comprising mixing a lithium hydrosulfide solution and a lithium halide solution to give the solution containing a lithium hydrosulfide and a lithium halide which is heated for supplying the hydrogen sulfide.

### Claim 3 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, further comprising heating a solution containing a lithium hydroxide and a lithium halide under a temperature condition of 0° C. or higher and 100° C. or lower in the presence of hydrogen sulfide to give the solution containing a lithium hydrosulfide and a lithium halide which is heated for supplying the hydrogen sulfide.

### Claim 4 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, wherein in heating the mixture containing a lithium hydrosulfide and a lithium halide in the presence of hydrogen sulfide, the hydrogen sulfide is supplied at a flow rate of 0.01 N-L/min or more and 20 N-L/min or less relative to 1 kg of the solid content in the mixture.

### Claim 5 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, wherein in heating the mixture containing a lithium hydrosulfide and a lithium halide in the presence of hydrogen sulfide, the heating is carried out at 100° C. or higher and 400° C. or lower.

### Claim 6 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, wherein the lithium halide is at least one selected from lithium chloride, lithium bromide and lithium iodide.

### Claim 7 (depends on 3)

The method for producing a sulfur-containing complex according to claim 3, wherein in obtaining the mixture containing a lithium hydrosulfide and a lithium halide, hydrogen sulfide is supplied at a flow rate of 0.01 N-L/min or more and 20 N-L/min or less relative to 1 kg of the solid content in the mixture.

### Claim 8 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, further comprising reacting the resulting sulfur-containing complex and a phosphorus compound to obtain a sulfide solid electrolyte.

### Claim 9 (depends on 1)

The method for producing a sulfur-containing complex according to claim 1, wherein the sulfur-containing complex comprises a lithium sulfide and a lithium halide, exhibiting, in X-ray diffractometry using a CuKα ray, a diffraction angle of the peak of lithium halide shifting toward the diffraction angle of the peak of lithium sulfide, and not comprising an oxygen-containing lithium halide represented by Li3OX, where X represents a halogen element.