IP Library › Granted Patent US 11,355,780
Granted Patent B2
US 11,355,780 · App. 16/491,659 · Granted Jun 7, 2022

Sulfide solid electrolyte particles

Inventors: Futoshi Utsuno (Sodegaura, JP); Toshiaki Tsuno (Sodegaura, JP); Kota Terai (Sodegaura, JP); Hironari Kimpara (Sodegaura, JP); Atsushi Sato (Sodegaura, JP)
Assignee: IDEMITSU KOSAN CO., LTD.
H01M10/0562C01B17/22H01B1/10H01M4/13H01M4/62H01M10/0525C01P2002/30C01P2002/72C01P2002/86C01P2004/51
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Quick Facts
Patent No.
US 11,355,780
App. No.
16/491,659
Granted
Jun 7, 2022
Kind
B2
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.

Claims (30)

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.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 6, 2019
From: UTSUNO, FUTOSHI; TSUNO, TOSHIAKI; TERAI, KOTA; KIMPARA, HIRONARI; SATO, ATSUSHI
To: IDEMITSU KOSAN CO., LTD.
Reel/Frame 050303/0766 →
Priority Claims (1)
JP JP2017-044312 · Mar 8, 2017 · national
Continuity (1)
Related Publication 20200006808A1 · Jan 2, 2020