Alkali metal halide production method, and sulfide solid electrolyte production method
US-2020168944-A1 · May 28, 2020 · US
US11038198B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11038198-B2 |
| Application number | US-201716084114-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 14, 2017 |
| Priority date | Mar 14, 2016 |
| Publication date | Jun 15, 2021 |
| Grant date | Jun 15, 2021 |
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Provided is a solid electrolyte having a high ion conductivity and excellent in battery performance not going through a step of removing water such as a drying step, while simplifying the production process and reducing the production cost. Specifically, provided is a method for producing a sulfide-based solid electrolyte, including causing a reaction of an alkali metal sulfide and a specific substance in a solvent.
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The invention claimed is: 1. A method for producing a sulfide-based solid electrolyte comprising an alkali metal, sulfur, phosphorus, and halogen, wherein the alkali metal sulfide is reacted with a substance represented by the formula (1) in an organic solvent by mixing, stirring, grinding, or a combination thereof: X 2 (1) wherein X represents a halogen element. 2. A method for producing a sulfide-based solid electrolyte comprising an alkai metal sulfur phosphorus, and halogen, wherein, the alkali metal sulfide and a substance represented by the formula (1) and a phosphorus compound in an organic solvent by mixing, stirring, grinding, or a combination thereof: X 2 (1) wherein X represents a halogen element. 3. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein the phosphorus compound is phosphorus sulfide. 4. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein the alkali metal sulfide is at least one selected from lithium sulfide and sodium sulfide. 5. The method for producing a sulfide-based solid electrolyte according to claim 2 , wherein the substance is at least one selected from iodine and bromine. 6. The method for producing a sulfide-based solid electrolyte according to claim 2 , wherein the content of the substance X 2 relative to the total amount of the alkali metal sulfide, the phosphorus compound and the substance X 2 is 1 to 50 mol %. 7. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein the alkali metal sulfide is lithium sulfide, the phosphorus compound is diphosphorus pentasulfide, and the ratio of the molar number of lithium sulfide excluding the same molar number of lithium sulfide as the molar number of the substance X 2 , relative to the total molar number of lithium sulfide and diphosphorus pentasulfide excluding the same molar number of lithium sulfide as the molar number of the substance X 2 is 60 to 90%. 8. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein the solvent is a hydrocarbon solvent. 9. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein the solvent is one in which the solubility of the substance represented by the formula (1) is 0.01% by mass or more. 10. The method for producing a sulfide-based solid electrolyte according to claim 1 , wherein a grinding machine is used for the reaction. 11. A sulfide-based solid electrolyte comprising an alkali metal element, a sulfur element and a halogen element, which is such that the absolute value of the heat quantity H 380 of an endothermic peak that has a peak top at 380±15° C., as measured in differential heat analysis under a heating condition of 10° C./min, is 10 (J/g) or more. 12. The sulfide-based solid electrolyte according to claim 11 , further comprising a phosphorus atom. 13. The sulfide-based solid electrolyte according to claim 11 , wherein the ratio of the absolute value of the heat quantity H 380 of the endothermic peak to the total H 350-450 of the absolute values of the heat quantities of the endothermic peaks each having a peak top at 350 to 450° C. (H 380 /H 350-450 ) is 50% or more. 14. The sulfide-based solid electrolyte according to claim 11 , wherein the alkali metal element is at least one selected from a lithium element and a sodium element. 15. The sulfide-based solid electrolyte according to claim 11 , wherein the halogen element is at least one selected from bromine and iodine. 16. The sulfide-based solid electrolyte according to claim 12 , wherein the molar ratio of the alkali metal element, the sulfur element, the phosphorus element and the halogen element is (1.0 to 1.8)/(1.0 to 2.0)/(0.1 to 0.8)/(0.01 to 0.6). 17. The sulfide-based solid electrolyte according to claim 12 , wherein the halogen element contains bromine and iodine and the molar ratio of the alkali metal element, the sulfur element, the phosphorus element, bromine and iodine is (1.0 to 1.8)/(1.0 to 2.0)/(0.1 to 0.8)/(0.01 to 0.3)/(0.01 to 0.3). 18. The sulfide-based solid electrolyte according to claim 11 , having a crystal structure that has peaks at 2θ=20.2°±0.5° and 23.6°±0.5°.
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