Method for producing sulfide solid electrolyte
A method for producing a sulfide glass ceramic, including reacting a lithium compound, a phosphorus compound and a halogen compound in a solvent that contains a hydrocarbon and an ether compound to produce a sulfide glass that contains a Li element, a P element, a S element and one or more halogen elements, and heating the sulfide glass to produce a sulfide glass ceramic.
1. A method for producing a sulfide glass ceramic, comprising:
reacting a lithium compound, a phosphorus compound and a halogen compound in a solvent that contains a hydrocarbon and an ether compound to produce a sulfide glass that contains a Li element, a P element, a S element and one or more halogen elements, wherein the blending ratio of the hydrocarbon to the ether compound is from 480/1 to 50/1 by volume ratio and
heating the sulfide glass to produce a sulfide glass ceramic.
2. The method for producing a sulfide glass ceramic according to claim 1 , wherein the lithium compound is lithium sulfide.
3. The method for producing a sulfide glass ceramic according to claim 1 , wherein the phosphorus compound is diphosphorus pentasulfide.
4. The method for producing a sulfide glass ceramic according to claim 3 , wherein the proportion of the lithium sulfide to the total of the lithium sulfide and the diphosphorus pentasufide is from 68 mol % to 82 mol %.
5. The method for producing a sulfide glass ceramic according to claim 1 , wherein the halogen compound is at least one of lithium iodide and lithium bromide.
6. The method for producing a sulfide glass ceramic according to claim 5 , wherein, when lithium iodide and lithium bromide are the starting materials, the proportion of the lithium bromide to the total of the lithium iodide and the lithium bromide is from 1 mol % to 99 mol %.
7. The method for producing a sulfide glass ceramic according to claim 1 , wherein the heating includes a first heating of heating the sulfide glass at a temperature of 100° C. or higher and lower than the crystallization temperature (Tc) of the crystalline structure that the sulfide glass ceramic to be obtained has, and after the first heating, a second heating of further heating the sulfide glass ceramic at a temperature of not lower than crystallization temperature (Tc) and up to the crystallization temperature (Tc)+60° C.
8. The method for producing a sulfide glass ceramic according to claim 7 , wherein the heat treatment time in the first heating is 1 minute or more and 10 hours or less, and the heat treatment time in the second heating is 1 minute or more and 10 hours or less.
9. The method for producing a sulfide glass ceramic according to claim 7 , wherein the heat treatment time in the first heating is 30 minutes or more and 10 hours or less, and the heat treatment time in the second heating is 30 minutes or more and 10 hours or less.
10. The method for producing a sulfide glass ceramic according to claim 7 , wherein the first heating is carried out under such a condition that the sulfide glass becomes a sulfide glass ceramic having a degree of crystallization of 1% or more and 50% or less, and the second heating is carried out under such a condition that the degree of crystallization of the sulfide glass ceramic obtained in the first heating is further increased.
11. The method for producing a sulfide glass ceramic according claim 1 , wherein the heating includes a first heating of heating the sulfide glass at a temperature of 100° C. or higher and 140° C. or lower, and after the first heating, a second heating of further heating at a temperature of 150° C. or higher and 300° C. or lower.
12. The method for producing a sulfide glass ceramic according to claim 11 , wherein the first heating is at a temperature of 120° C. or higher and 140° C. or lower, and the second heating is at a temperature of 170° C. or higher and 280° C. or lower.
13. The method for producing a sulfide glass ceramic according to claim 1 , wherein the hydrocarbon is an aromatic hydrocarbon.
14. The method for producing a sulfide glass ceramic according to claim 13 , wherein the aromatic hydrocarbon is toluene.
15. The method for producing a sulfide glass ceramic according to claim 1 , wherein the ether compound is a linear ether.
16. The method for producing a sulfide glass ceramic according to claim 15 , wherein the linear ether is dibutyl ether.
17. The method for producing a sulfide glass ceramic according to claim 1 , wherein the amount of the ether compound is from 0.01% by weight to 100% by weight relative to the total amount of the starting materials.
18. The method for producing a sulfide glass ceramic according to claim 1 , wherein the blending ratio of the hydrocarbon to the ether compound is from 400/1 to 120/1 by volume ratio.
19. The method for producing a sulfide glass ceramic according to claim 1 , wherein the blending ratio of the hydrocarbon to the ether compound is from 240/1 to 150/1 by volume ratio.
20. A method for producing a sulfide solid electrolyte that contains a Li element, a P element, a S element and one or more halogen elements, the method comprising reacting a lithium compound, a phosphorus compound and a halogen compound in a solvent that contains a hydrocarbon and an ether compound, wherein the blending ratio of the hydrocarbon to the ether compound is from 480/1 to 50/1 by volume ratio.