IP Library Granted Patent US 11,688,879
Granted Patent B2
US 11,688,879 · App. 16/979,920 · Granted Jun 27, 2023

Sulfide-based solid electrolyte particles

Inventors: Tsukasa Takahashi (Ageo, JP); Takashi Chikumoto (Ageo, JP); Takahiro Ito (Ageo, JP)
Assignee: Mitsui Mining & Smelting Co., Ltd.
H01M10/0562H01M4/13H01M10/0525H01M2004/027H01M2004/028
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Quick Facts
Patent No.
US 11,688,879
App. No.
16/979,920
Granted
Jun 27, 2023
Kind
B2
Abstract

A sulfide-based solid electrolyte particle having a crystal phase of a cubic argyrodite-type crystal structure composed of Li, P, S and a halogen (Ha. The proposed sulfide-based solid electrolyte particle has a feature such that the ratio (Z Ha2 /Z Ha1 ) of an element ratio Z Ha2 of the halogen (Ha) at the position of 5 nm in depth from the particle surface to an element ratio Z Ha1 of the halogen (Ha) at the position of 100 nm in depth from the particle surface is 0.5 or lower, as measured by XPS; and the ratio (Z O2 /Z A2 ) of an element ratio Z O2 of oxygen to the total Z A2 of element ratios of phosphorus (P), sulfur (S), oxygen (O) and the halogen (Ha) at the position of 5 nm in depth from the particle surface is 0.5 or higher, as measured by XPS.

Claims (16)

1. A sulfide-based solid electrolyte particle, comprising a solid electrolyte particle having a crystal phase of a cubic argyrodite-type crystal structure and comprising lithium (Li), phosphorus (P), sulfur (S) and a halogen (Ha),

wherein the solid electrolyte particle has been subjected to a surface modification treatment in which the solid electrolyte particle is directly exposed to an atmosphere having a dew point of −35° C. to 10° C., the atmosphere reacts with the solid electrolyte particle, and no subsequent drying of the solid electrolyte particle is performed;

a ratio (Z Ha2 /Z Ha1 ) of an element ratio Z Ha2 of the halogen (Ha) at a position, in terms of an SiO 2 sputter rate, of 5 nm in depth from the particle surface to an element ratio Z Ha1 of the halogen (Ha) at a position, in terms of the SiO 2 sputter rate, of 100 nm in depth from the particle surface is higher than 0 and 0.5 or lower, as measured by X-ray photoelectron spectroscopy (XPS); and

a ratio (Z O2 /Z A2 ) of an element ratio Z O2 of oxygen to a total Z A2 of element ratios of phosphorus (P), sulfur (S), oxygen (O) and the halogen (Ha) at the position, in terms of the SiO 2 sputter rate, of 5 nm in depth from the particle surface is 0.5 or higher and 1.0 or lower, as measured by XPS.

2. The sulfide-based solid electrolyte particle according to claim 1 , wherein a ratio (Z Ha2 /Z A2 ) of an element ratio Z Ha2 of the halogen (Ha) to a total Z A2 of element ratios of phosphorus (P), sulfur (S), oxygen (O) and the halogen (Ha) at the position, in terms of SiO 2 sputter rate, of 5 nm in depth from the particle surface is 0.1 or lower.

3. The sulfide-based solid electrolyte particle according to claim 1 , wherein a ratio (Z Ha1 /Z A1 ) of an element ratio Z Ha1 of the halogen (Ha) to a total Z A1 of element ratios of phosphorus (P), sulfur (S), oxygen (O) and the halogen (Ha) at the position, in terms of SiO 2 sputter rate, of 100 nm in depth from the particle surface is 0.03 to 0.3.

4. An electrode material for a lithium secondary battery, comprising: a sulfide-based solid electrolyte particle according to claim 1 ; and a positive electrode active material and/or a negative electrode active material.

5. A lithium secondary battery, having a layer comprising a sulfide-based solid electrolyte particle according to claim 1 .

6. The sulfide-based solid electrolyte particle according to claim 2 , wherein a ratio (Z Ha1 /Z A1 ) of an element ratio Z Ha1 of the halogen (Ha) to a total Z A1 of element ratios of phosphorus (P), sulfur (S), oxygen (O) and the halogen (Ha) at the position, in terms of SiO 2 sputter rate, of 100 nm in depth from the particle surface is 0.03 to 0.3.

7. An electrode material for a lithium secondary battery, comprising: a sulfide-based solid electrolyte particle according to claim 2 ; and a positive electrode active material and/or a negative electrode active material.

8. An electrode material for a lithium secondary battery, comprising: a sulfide-based solid electrolyte particle according to claim 3 ; and a positive electrode active material and/or a negative electrode active material.

9. An electrode material for a lithium secondary battery, comprising: a sulfide-based solid electrolyte particle according to claim 6 ; and a positive electrode active material and/or a negative electrode active material.

10. A lithium secondary battery, having a layer comprising a sulfide-based solid electrolyte particle according to claim 2 .

11. A lithium secondary battery, having a layer comprising a sulfide-based solid electrolyte particle according to claim 3 .

12. A lithium secondary battery, having a layer comprising a sulfide-based solid electrolyte particle according to claim 6 .

13. The sulfide-based solid electrolyte particle according to claim 1 , wherein a ratio (Z Ha2 /Z Ha1 ) of an element ratio Z Ha2 of the halogen (Ha) at a position, in terms of an SiO 2 sputter rate, of 5 nm in depth from the particle surface to an element ratio Z Ha1 of the halogen (Ha) at a position, in terms of the SiO 2 sputter rate, of 100 nm in depth from the particle surface is 0.01 or higher.

Assignments (2)
CHANGE OF NAME Recorded Mar 31, 2026
From: MITSUI MINING AND SMELTING COMPANY, LIMITED
To: MITSUI KINZOKU COMPANY, LIMITED
Reel/Frame 075357/0342 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 11, 2020
From: TAKAHASHI, TSUKASA; CHIKUMOTO, TAKASHI; ITO, TAKAHIRO
To: MITSUI MINING & SMELTING CO., LTD.
Reel/Frame 053742/0118 →
Priority Claims (1)
JP JP2018-044210 · Mar 12, 2018 · national
Continuity (1)
Related Publication 20210013542A1 · Jan 14, 2021