Method for preparing ceramic solid electrolyte for lithium secondary battery
The present invention relates to a method for preparing a ceramic solid electrolyte having a even particle distribution, excellent crystallinity, and high ionic conductivity. Step 1 for preparing the ceramic solid electrolyte particles may be a step for adding and mixing raw materials to distilled water to prepare a solid electrolyte precursor. Step 2 may be a step for mixing the solid electrolyte precursor with a ball-mill. Step 3 may be a step for drying first by rotary concentrating or spraying. Step 4 may be a step for drying second in a dryer at 80° C. for at least 24 hours to completely remove the distilled water solvent. Step 5 may be a step for calcining first ceramic particles in a heat treatment device and firing second the ceramic particles.
1. A method for preparing a ceramic solid electrolyte comprising:
a step of making a precursor of ceramic solid electrolyte by mixing raw materials of the ceramic solid electrolyte with distilled water;
a step of mixing the precursor of the ceramic solid electrolyte in a solution state by ball-milling;
a step of drying the distilled water to obtain a dried product;
a step of first heat treatment of the dried product at 300° C. to 500° C. for 2 hours to 10 hours to obtain a first heat treatment product; and
a step of second heat treatment of the first heat treatment product at 900° C. to 1200° C. for 2 hours to 10 hours.
2. A method for preparing a ceramic solid electrolyte comprising:
a step of making a precursor of ceramic solid electrolyte by mixing raw materials of the ceramic solid electrolyte with distilled water;
a step of mixing the precursor of the ceramic solid electrolyte in a solution state by ball-milling;
a step of first drying of the distilled water by rotary concentrating process to obtain a first dried product;
a step of second drying of the distilled water in a dryer to obtain a second dried product;
a step of first heat treatment of the second dried product at 300° C. to 500° C. for 2 hours to 10 hours to obtain a first heat treatment product; and
a step of second heat treatment of the first heat treatment product at 900° C. to 1200° C. for 2 hours to 10 hours.
3. A method for preparing a ceramic solid electrolyte comprising:
a step of making a precursor of ceramic solid electrolyte by mixing raw materials of the ceramic solid electrolyte with distilled water;
a step of mixing the precursor of the ceramic solid electrolyte in a solution state by ball-milling;
a step of first drying of the distilled water by spray method to obtain a first dried product;
a step of second drying of the distilled water in a dryer to obtain a second dried product;
a step of first heat treatment of the second dried product at 300° C. to 500° C. for 2 hours to 10 hours to obtain a first heat treatment product; and
a step of second heat treatment of the first heat treatment product at 900° C. to 1,200° C. for 2 hours to 10 hours.
4. The method for preparing the ceramic solid electrolyte according to claim 1 , wherein the ceramic solid electrolyte is an oxide-based ceramic solid electrolyte.
5. The method for preparing the ceramic solid electrolyte according to claim 2 , wherein the temperature of the rotary concentrating process is 60° C. to 100° C.
6. The method for preparing the ceramic solid electrolyte according to claim 3 , wherein the temperature of the spray method process is 80° C. to 300° C.
7. The method for preparing the ceramic solid electrolyte according to claim 1 , wherein the temperature of the first heat treatment is 350° C. to 450° C.
8. The method for preparing the ceramic solid electrolyte according to claim 1 , wherein the temperature of the second heat treatment is 1000° C. to 1100° C.
9. The method for preparing the ceramic solid electrolyte according to claim 1 , wherein the first heat treatment time is 3 hours to 5 hours and the second heat treatment time is 3 hours to 5 hours.