Method of producing sulfide solid electrolyte material

Patent metadata

Field	Value
Publication number	US-10784012-B2
Application number	US-201715849897-A
Country	US
Kind code	B2
Filing date	Dec 21, 2017
Priority date	Dec 27, 2016
Publication date	Sep 22, 2020
Grant date	Sep 22, 2020

Abstract

The present disclosure provides a method of producing a sulfide solid electrolyte material which includes a preparing process of preparing composite particles including a solid solution including a Li2S component and a LiBr component; an addition process of adding the composite particles and a phosphorus source to a reaction chamber; and a milling process in which a mechanical milling treatment is performed on the composite particles and the phosphorus source in the reaction chamber while thermal energy is applied.

First claim

What is claimed is:

1. A method of producing a sulfide solid electrolyte material, comprising:
a preparing process of preparing composite particles including a solid solution including a LiI component, a Li 2 S component and a LiBr component, wherein
the LiI component, the Li 2 S component and the LiBr component are solid-solutionized such that the solid solution comprises a LiBr rich phase in which the LiBr component is a main component of the LiBr rich phase, and in an XRD measurement using CuKα rays, a peak position of the (111) plane of the LiBr rich phase is shifted 0.1° or more to a lower angle side of a peak position of the (111) plane of LiBr;

an addition process of adding the composite particles and a phosphorus source to a reaction chamber; and
a milling process in which a mechanical milling treatment is performed on the composite particles and the phosphorus source in the reaction chamber while thermal energy is applied.

2. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein the solid solution further comprises a Li 2 S rich phase in which the Li 2 S component is a main component.

3. The method of producing a sulfide solid electrolyte material according to claim 2 , wherein, in XRD measurement using CuKα rays, a peak position of the (111) plane of the Li 2 S rich phase is shifted to a lower angle side of a peak position of the (111) plane of Li 2 S.

4. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein the peak position of the (111) plane of the LiBr rich phase is shifted 0.3° or more to a lower angle side of a peak position of the (111) plane of LiBr.

5. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein the solid solution further comprises a LiI rich phase in which the LiI component is a main component.

6. The method of producing a sulfide solid electrolyte material according to claim 5 , wherein, in XRD measurement using CuKα rays, a peak position of the (111) plane of the LiI rich phase is shifted to a higher angle side of a peak position of the (111) plane of LiI.

7. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein, in the preparing process, the composite particles are synthesized using a raw material solution including raw materials of the composite particles.

8. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein, in the preparing process, a raw material solution including raw materials of the composite particles and a first solvent is brought into contact with a second solvent heated to a temperature higher than a boiling point of the first solvent so that the composite particles are precipitated while the first solvent is evaporated, wherein
the first solvent is a solvent having a solubility in raw materials of composite particles that is higher than that of the second solvent, and
the second solvent is a solvent having a solubility in composite particles that is lower than that of the first solvent.

9. The method of producing a sulfide solid electrolyte material according to claim 8 , wherein the raw materials of the composite particles include LiHS and LiBr.

10. The method of producing a sulfide solid electrolyte material according to claim 8 , wherein the raw materials of the composite particles include Li 2 S and LiBr.

11. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein, in the preparing process, a raw material solution including raw materials of the composite particles and a first solvent is brought into contact with a solid heated to a temperature higher than a boiling point of the first solvent so that the composite particles are precipitated while the first solvent is evaporated.

12. The method of producing a sulfide solid electrolyte material according to claim 11 , wherein the raw materials of the composite particles include LiHS and LiBr.

13. The method of producing a sulfide solid electrolyte material according to claim 11 , wherein the raw materials of the composite particles include Li 2 S and LiBr.

14. The method of producing a sulfide solid electrolyte material according to claim 7 , wherein the raw materials of the composite particles further include LiI.

15. The method of producing a sulfide solid electrolyte material according to claim 1 ,
wherein the preparing process includes
a drying treatment in which a raw material solution including LiI, LiOH, LiBr, and water is dried to remove moisture such that a raw material mixture including LiI, LiOH and LiBr is obtained;
a sulfurization treatment in which LiOH in the raw material mixture is sulfurized such that LiHS is obtained; and
a hydrodesulfurization treatment in which hydrogen sulfide is desorbed from LiHS such that Li 2 S is obtained.

16. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein the phosphorus source is P 2 S 5 .

17. The method of producing a sulfide solid electrolyte material according to claim 1 , wherein a heating temperature in the milling process is in a range of 70° C. to 150° C.

Assignees

• Toyota Motor Co Ltd

Inventors

• Yanagi Takuo

Classifications

• H01M10/056

  characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes · CPC title

• C01B17/22 Primary

  Alkali metal sulfides or polysulfides · CPC title

• H01M2300/0068

  inorganic · CPC title

• H01M10/0562 Primary

  Solid materials · CPC title

• H01B1/10 Primary

  sulfides · CPC title