Lithium ion conducting sulfide glass fabrication

Patent metadata

Field	Value
Publication number	US-12294050-B2
Application number	US-202117249864-A
Country	US
Kind code	B2
Filing date	Mar 16, 2021
Priority date	Dec 2, 2014
Publication date	May 6, 2025
Grant date	May 6, 2025

Abstract

Preparation of anhydrous lithium sulfide (Li 2 S) purified suitably for applications in advanced batteries, and, in particular, for synthesis of solid electrolytes based on Li 2 S, including sulfide solid electrolytes of the type that may be described as crystalline (e.g., polycrystalline), amorphous (e.g., glass) and combinations thereof, such as sulfide glass-ceramic solid electrolyte materials.

First claim

What is claimed is:

1. A method of making lithium sulfide for use as a precursor material for making lithium ion conducting sulfide solid electrolyte materials, the method comprising the steps of:
i) providing a liquid lithium precursor; ii) providing a liquid sulfur precursor; and iii) combining the precursors in a dry inert atmosphere to reactively precipitate a lithium sulfide material for use as a precursor material for processing lithium ion conducting sulfide solid electrolyte material;
wherein one or both of the lithium and/or sulfur precursor is a liquid suspension of colloid composed of undissolved active species;
wherein the liquid sulfur precursor comprises a solid organic compound comprising reactive sulfur atoms;
wherein the solid organic compound is thiophene.

2. The method of claim 1 wherein the temperature of the precursors just prior to the combining step is not greater than 30° C.

3. The method of claim 2 wherein the reactive precipitation is a spontaneous process.

4. The method of claim 1 wherein the dry inert atmosphere is dry argon gas.

5. The method of claim 4 wherein the liquid lithium precursor comprises a lithium active liquid solution comprising dissolved active lithium species and a first liquid solvent system and a liquid sulfur precursor comprising a sulfur active liquid solution of dissolved active sulfur species in a second liquid solvent system.

6. The method of claim 5 wherein the method further comprises the step of filtering the lithium sulfide precipitate to yield a substantially anhydrous powder of Li 2 S.

7. The method of claim 6 wherein the combining step involves gradually adding the liquid lithium precursor to the liquid sulfur precursor.

8. The method of claim 6 wherein the first liquid solvent system is amide based.

9. The method of claim 6 wherein the second liquid solvent system is amine based.

10. The method of claim 6 wherein the liquid lithium precursor comprises a solution of lithium ion and solvated electrons.

11. The method of claim 10 wherein the liquid lithium precursor comprises HMPA as a liquid solvent.

12. The method of claim 6 wherein the liquid sulfur precursor comprises a solution of dissolved lithium polysulfide species.

13. The method of claim 12 wherein the liquid sulfur precursor comprises an amine as a liquid solvent.

14. The method of claim 6 wherein the liquid lithium precursor comprises Bu-Li.

15. The method of claim 6 wherein the liquid sulfur precursor comprises a solution of sulfur dissolved in a liquid solvent comprising a liquid selected from the group consisting of toluene, benzene, and CS 2 .

Assignees

• Polyplus Battery Co Inc

Inventors

• Visco Steven J
• Petrov Alexei
• Loginova Valentina
• Nimon Vitaliy
• Nimon Yevgeniy S
• Katz Bruce D

Classifications

• H01M2300/0068

  inorganic · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title

• H01M50/431

  Inorganic material · CPC title

• H01M50/403

  Manufacturing processes of separators, membranes or diaphragms · CPC title

• H01M50/46

  Separators, membranes or diaphragms characterised by their combination with electrodes · CPC title