# US 12,603,276 B2 · Active material, and positive electrode mixture and solid-state battery that use said active material

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- Number: US 12,603,276 B2
- Document ID: US12603276B2
- Status: Granted
- Kind: B2
- Application number: 17/056,339
- Filed: 2019-09-27
- Published: 2021-07-29
- Granted: 2026-04-14
- Earliest claimed: 2018-09-27
- Assignees: Mitsui Kinzoku Company, Limited
- Applicants: Mitsui Mining & Smelting Co., Ltd.
- Inventors: Daisuke Washida; Hitohiko Ide; Tetsuya Mitsumoto; Jun Omura; Yasuo Komoda; Yasuhiro Shibata; Yasunori Tabira; Tomoyuki Maeda
- Web page: https://patentgrep.com/patent/US12603276B2

## CPC

- C01G 53/504: with the molar ratio of nickel with respect to all the metals other than alkali metals higher than or equal to 0.5, e.g. Li(MzNixCoyMn1-x-y-z)O2 with x ≥ 0.5
- C01G 53/502: containing lithium and cobalt
- H01M 4/131: Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 4/366: {as layered products}
- H01M 4/483: {for non-aqueous cells (H01M4/485 takes precedence)}
- H01M 4/505: of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
- H01M 4/525: of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
- H01M 4/62: Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M 10/052: Li-accumulators
- H01M 10/0562: Solid materials
- H01M 10/0585: of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators
- C01P 2002/32: spinel-type (AB2O4)
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/84: one phase coated with the other
- C01P 2006/12: Surface area
- C01P 2006/80: Compositional purity
- C01P 2006/82: water content
- H01M 2004/028: {Positive electrodes}
- H01M 2300/0068: inorganic
- Y02E 60/10: Energy storage using batteries
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Disclosed is an active material that can reduce an interface resistance with a sulfide solid electrolyte and improve the battery performance. The active material exhibits at least one peak in the range of from 0.145 nm to 0.185 nm and at least one peak in the range of from 0.28 nm to 0.31 nm in a radial distribution function obtained through measurement of an X-ray absorption fine structure of the active material. The active material is for use in a solid-state battery. The active material preferably has a core particle, and a coating layer located on the surface of the core particle.

## Claims

### Claim 1

An active material for use in a solid-state battery, exhibiting at least one peak in a range of from 0.145 nm to 0.185 nm and at least one peak in a range of from 0.28 nm to 0.31 nm in a radial distribution function obtained through measurement of an X-ray absorption fine structure of the active material,
wherein the active material comprises a core particle and a coating layer located on a surface of the core particle,
the core particle comprises a lithium-metal complex oxide,
the lithium-metal complex oxide comprises a layered rock salt-type compound or a spinel-type compound,
the coating layer comprises an oxide containing Li and Nb,
the active material has a BET specific surface area A of 0.5 m2/g or more and 5.0 m2/g or less,
a ratio B/A is from 308 to 778 when the lithium-metal complex oxide is a layered rock salt-type compound, and from 223 to 1257 when the lithium-metal complex oxide is a spinel-type compound, wherein A represents the BET specific surface area and B represents a moisture content (mass ppm) as measured up to 110° C. by the Karl-Fischer method,
a proportion of the oxide contained in the active material, in terms of a ratio of a mass of niobium to a mass of the active material is at least 0.01% by mass and at most 3% by mass, and
an amount of carbonic acid ions on a surface of the active material is less than 2.0% by mass, based on the active material.

### Claim 2 (depends on 1)

A positive electrode material mixture comprising the active material according to claim 1, and a sulfide solid electrolyte.

### Claim 3 (depends on 2)

The positive electrode material mixture according to claim 2, wherein the sulfide solid electrolyte contains elements Li and S, and has lithium ion conductivity.

### Claim 4 (depends on 3)

The positive electrode material mixture according to claim 3, wherein the sulfide solid electrolyte has a crystal phase of an argyrodite structure.

### Claim 5 (depends on 4)

A solid-state battery comprising a positive electrode layer, a negative electrode layer, and a solid electrolyte layer, the positive electrode layer containing the positive electrode material mixture according to claim 4.

### Claim 6 (depends on 3)

A solid-state battery comprising a positive electrode layer, a negative electrode layer, and a solid electrolyte layer, the positive electrode layer containing the positive electrode material mixture according to claim 3.

### Claim 7 (depends on 2)

A solid-state battery comprising a positive electrode layer, a negative electrode layer, and a solid electrolyte layer, the positive electrode layer containing the positive electrode material mixture according to claim 2.

### Claim 8 (depends on 1)

A positive electrode material mixture comprising the active material according to claim 1, and a sulfide solid electrolyte.

### Claim 9 (depends on 8)

The positive electrode material mixture according to claim 8, wherein the sulfide solid electrolyte contains elements Li and S, and has lithium ion conductivity.

### Claim 10 (depends on 8)

A solid-state battery comprising a positive electrode layer, a negative electrode layer, and a solid electrolyte layer, the positive electrode layer containing the positive electrode material mixture according to claim 8.

### Claim 11 (depends on 1)

The active material according to claim 1, wherein the active material has a volume cumulative particle size D50, which is a particle size at a cumulative volume 50% in the laser diffraction scattering particle size distribution analysis, of greater than 1 μm and at most 20 μm.