Complex comprising sulfur, a method for manufacturing the same, and a method for manufacturing a solid electrolyte

Patent metadata

Field	Value
Publication number	US-10865108-B2
Application number	US-201715839400-A
Country	US
Kind code	B2
Filing date	Dec 12, 2017
Priority date	Dec 14, 2016
Publication date	Dec 15, 2020
Grant date	Dec 15, 2020

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.

First claim

The invention claimed is:

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.

2. 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.

3. 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.

4. 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.

5. 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.

6. 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.

7. 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.

8. 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.

9. 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 Li 3 OX, where X represents a halogen element.

Assignees

• Idemitsu Kosan Co

Inventors

• Senga Minoru
• Umeki Takashi

Classifications

• H01M10/0562

  Solid materials · CPC title

• C01P2002/72

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

• Y02E60/10

  Energy storage using batteries · CPC title

• C01P2002/70

  defined by measured X-ray, neutron or electron diffraction data · CPC title

• H01M4/5815

  Sulfides · CPC title