Sulfide solid electrolyte particles

Patent metadata

Field	Value
Publication number	US-11355780-B2
Application number	US-201816491659-A
Country	US
Kind code	B2
Filing date	Mar 8, 2018
Priority date	Mar 8, 2017
Publication date	Jun 7, 2022
Grant date	Jun 7, 2022

Abstract

A sulfide solid electrolyte particles comprising lithium, phosphorus and sulfur, having a volume-based average particle size measured by laser diffraction particle size distribution measurement of 0.1 μm to 10 μm, having a diffraction peak having 2θ of 29.0 to 31.0 deg in powder X-ray diffraction measurement using CuKα ray, and an intensity ratio (Ib/Ip) of a peak intensity Ib at a high angle-side low part of the diffraction peak to a peak intensity Ip of the diffraction peak is less than 0.09.

First claim

The invention claimed is:

1. Sulfide solid electrolyte particles, comprising lithium, phosphorus and sulfur,
wherein
a volume-based average particle size measured by laser diffraction particle size distribution measurement is from 0.1 μm to 10 μm,
in powder X-ray diffraction measurement using CuKα ray, the sulfide solid electrolyte particles have a diffraction peak having 2θ of from 29.0 to 31.0 deg,
an intensity ratio (Ib/Ip) of a peak intensity Ib at a high angle-side low part of the diffraction peak to a peak intensity Ip of the diffraction peak is less than 0.09,
the sulfide solid electrolyte particles comprise an argyrodite-type crystal structure, and
the sulfide solid electrolyte particles comprise at least two halogens.

2. The sulfide solid electrolyte particles according to claim 1 , wherein the diffraction peak is at 2θ=29.7±0.5 deg.

3. The sulfide solid electrolyte particles according to claim 2 , further having a diffraction peak at 2θ=25.2±0.5 deg in powder X-ray diffraction measurement using CuKα ray.

4. The sulfide solid electrolyte particles according to claim 1 , wherein a molar ratio of the at least two halogens to the sulfur is from more than 0.23 to less than 0.57.

5. The sulfide solid electrolyte particles according to claim 1 , wherein a ratio of an area of glass-derived peaks to a total area of all peaks at 60 ppm to 120 ppm observed in solid 31 P-NMR measurements is from 0% to 30%.

6. An electrode mix comprising the sulfide solid electrolyte particles of claim 1 and an active material.

7. A lithium ion battery comprising the sulfide solid electrolyte particles of claim 1 .

8. A lithium ion battery comprising the electrode mix of claim 6 .

9. Sulfide solid electrolyte particles, comprising lithium, phosphorus and sulfur,
wherein
a volume-based average particle size measured by laser diffraction particle size distribution measurement is from 0.1 μm to 10 μm,
an ionic conductivity is 4.0 mS/cm or more,
the sulfide solid electrolyte particles comprise an argyrodite-type crystal structure, and
the sulfide solid electrolyte particles comprise at least two halogens.

10. A method for producing sulfide solid electrolyte particles comprising a crystal structure of a stable phase, the method comprising:
pulverizing the sulfide solid electrolyte, followed by subjecting a pulverized product to a heat treatment,
wherein the crystal structure of the stable phase is an argyrodite-type crystal structure, and
the sulfide solid electrolyte particles comprise at least two halogens.

11. The method according to claim 10 , wherein the sulfide solid electrolyte comprises lithium, phosphorus, sulfur and halogen, and comprises an argyrodite-type crystal structure.

12. The method according to claim 10 , wherein a temperature of the heat treatment is from 350° C. to 700° C.

13. The method according to claim 10 , wherein a jet mill, a ball mill or a bead mill is used for the pulverizing.

14. The method according to claim 10 , further comprising:
reacting a raw material comprising lithium, phosphorus and sulfur, thereby producing a glassy sulfide solid electrolyte.

15. The method according to claim 14 , wherein the raw material comprises lithium sulfide, phosphorus sulfide, and lithium halide.

Assignees

• Idemitsu Kosan Co

Inventors

• Utsuno Futoshi
• Tsuno Toshiaki
• Terai Kota
• Kimpara Hironari
• Sato Atsushi

Classifications

• H01M4/13

  Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof · CPC title

• H01B1/06

  mainly consisting of other non-metallic substances · CPC title

• C01P2002/86

  by NMR- or ESR-data · CPC title

• H01M10/0525

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

• Y02E60/10

  Energy storage using batteries · CPC title