Method for preparing needle-like sulfide-based solid electrolyte

Patent metadata

Field	Value
Publication number	US-10777846-B2
Application number	US-201715845065-A
Country	US
Kind code	B2
Filing date	Dec 18, 2017
Priority date	Oct 13, 2017
Publication date	Sep 15, 2020
Grant date	Sep 15, 2020

Abstract

Provided is a method for preparing a needle-like sulfide-based solid electrolyte. The method may include: preparing a solid electrolyte admixture comprising an organic solvent, Li2S, P2S5, and LiCl; synthesizing a solid electrolyte by stirring the solid electrolyte admixture at a temperature of about 30 to 60° C. for about 22 to 26 hours; first stirring the solid electrolyte at a speed of about 80 to 120 rpm for about 5 to 10 minutes; after the first stirring, second stirring the first stirred solid electrolyte at a speed of about 250 to 300 rpm; vacuum-drying the second stirred solid electrolyte for about 12 to 24 hours; and heat-treating the vacuum-dried solid electrolyte at a temperature of about 350 to 550° C. for about 1 to 5 hours.

First claim

What is claimed is:

1. A method for preparing a needle-like sulfide-based solid electrolyte, comprising:
preparing a solid electrolyte admixture comprising an organic solvent, Li 2 S, P 2 S 5 , and LiCl;
synthesizing a solid electrolyte by stirring the solid electrolyte admixture at a temperature of about 30 to 60° C. for about 22 to 26 hours;
first stirring the solid electrolyte at a speed of about 80 to 120 rpm for about 5 to 10 minutes;
after the first stirring, second stirring the first stirred solid electrolyte at a speed of about 250 to 300 rpm;
vacuum-drying the second stirred solid electrolyte for about 12 to 24 hours; and
heat-treating the vacuum-dried solid electrolyte at a temperature of 350 to 550° C. for about 1 to 5 hours to obtain the needle-like sulfide-based solid electrolyte.

2. The method of claim 1 , wherein the organic solvent comprises at least one selected from the group consisting of an ethyl ester-based organic solvent, a methyl ester-based organic solvent, a propyl ester-based organic solvent, a butyl ester-based organic solvent, and an amyl ester-based organic solvent.

3. The method of claim 1 , the organic solvent is ethyl acetate.

4. The method of claim 1 , wherein the solid electrolyte admixture further comprises at least one selected from the group consisting of Li 2 SO 4 , P 2 S 3 , P 2 O 5 , and GeS 2 .

5. The method of claim 1 , wherein the solid electrolyte is synthesized by stirring the solid electrolyte admixture at a temperature of about 30 to 60° C. for about 22 to 26 hours.

6. The method of claim 1 , wherein the vacuum-drying is performed for about 12 to 24 hours.

7. The method of claim 1 , wherein the heat-treating is performed at a temperature of 350 to 550° C. for about 1 to 5 hours.

8. The method of claim 1 , wherein the vacuum-drying of the second stirred solid electrolyte is carried out at a temperature of about 20 to 60° C.

9. The method of claim 1 , wherein the needle-like sulfide-based solid electrolyte has a specific surface area of about 0.2 to 1.0 m 2 /g.

10. The method of claim 1 , wherein, during the first stirring of the solid electrolyte, adhesion of the Li 2 S, the P 2 S 5 , and the LiCl is prevented, and the Li 2 S, the P 2 S 5 , and the LiCl is uniformly mixed.

11. The method of claim 1 , wherein, during the second stirring of the first stirred solid electrolyte, the organic solvent reacts with the Li 2 S, the P 2 S 5 , and the LiCl.

Assignees

• Hyundai Motor Co Ltd
• Kia Motors Corp
• Iucf Hyu

Inventors

• Kwon Oh Min
• Yoon Yong Sub
• Noh Sung Woo
• Oh Seung Hyun
• Choi Sun Ho
• Shin Dong Wook
• Park Chan Hwi

Classifications

• B01F23/511

  characterised by the composition of the liquids or solids · CPC title

• B01F2101/2204

  Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application · CPC title

• H01M10/0562 Primary

  Solid materials · CPC title

• H01M2300/0068

  inorganic · CPC title

• C01P2004/10

  extending in one dimension, e.g. needle-like · CPC title