Method of manufacturing a solid electrolyte for an all-solid-state battery through liquid stirring
A method of manufacturing a solid electrolyte for an all-solid-state battery is provided by allowing a starting material to react through liquid stirring without pulverization.
1. A method of manufacturing a solid electrolyte, the method comprising:
preparing a starting material comprising a lithium powder, a sulfur powder, and a phosphorus compound;
adding the starting material to a solvent and causing a reaction with stirring to provide a reaction product;
drying the reaction product; and
heat-treating the dried reaction product to provide the solid electrolyte,
wherein the lithium powder and the sulfur powder are not soluble in the solvent,
wherein the reaction is carried out using a stirrer,
wherein the stirrer includes
a container in which a space accommodating the solvent and the starting material is formed,
a stirring blade disposed inside the container, and
a stirring rod connected to the stirring blade and extending in a longitudinal direction of the container,
wherein the reaction occurs by inducing a collision or contact between components of the starting material in the solvent due to a rotational force of the stirring blade by rotating the stirring rod, and
wherein a weight ratio of the starting material and the solvent is in a range of 1:20-1:50.
2. The method of claim 1 , wherein the starting material further comprises a lithium halogen compound LiX,
wherein X is selected from the group consisting of Br, Cl, I, and combinations thereof.
3. The method of claim 1 , wherein the starting material does not comprise a lithium sulfur compound.
4. The method of claim 1 , wherein the reaction occurs by causing a collision between powder with stirring in a state in which the lithium powder and the sulfur powder are not dissolved in the solvent.
5. The method of claim 1 , wherein the drying is performed in a vacuum atmosphere at a temperature in a range of 25° C. to 250° C. for 5 hours to 15 hours.
6. The method of claim 1 , wherein the drying is performed in a vacuum atmosphere through:
first drying at a temperature ranging from 25° C. to lower than 50° C. for 1 hour to 3 hours;
second drying at a temperature ranging from 50° C. to lower than 100° C. for 1 hour to 3 hours;
third drying at a temperature ranging from 100° C. to lower than 150° C. for 1 hour to 3 hours;
fourth drying at a temperature ranging from 150° C. to lower than 200° C. for 1 hour to 3 hours; and
fifth drying at a temperature ranging from 200° C. to 250° C. for 1 hour to 3 hours.
7. The method of claim 6 , wherein the first drying to the fifth drying is performed by raising the temperature from 25° C. to a temperature within a range of 200° C. to 250° C.
8. The method of claim 1 , wherein the heat-treating is performed in a range of 400° C. to 600° C. for 1 hour to 5 hours.
9. The method of claim 1 , wherein the solid electrolyte is crystalline.