# US 2019/0245206 A1 · Manufacturing method of composite oxide and manufacturing method of power storage device

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- Number: US 2019/0245206 A1
- Document ID: US20190245206A1
- Status: Published application
- Kind: A1
- Application number: 16/388,904
- Filed: 2019-04-19
- Published: 2019-08-08
- Earliest claimed: 2011-08-31
- Assignees: Semiconductor Energy Laboratory Co., Ltd.
- Applicants: Semiconductor Energy Laboratory Co., Ltd.
- Inventors: Takuya MIWA; Kuniharu NOMOTO; Junpei MOMO
- Web page: https://patentgrep.com/patent/US20190245206A1

## CPC

- H01M 4/5825: {Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines}
- C01D 15/02: Oxides; Hydroxides
- C01G 45/22: Compounds containing manganese, with or without oxygen or hydrogen, and containing two or more other elements
- C01G 49/009: {Compounds containing iron, with or without oxygen or hydrogen, and containing two or more other elements}
- C01G 51/82: Compounds containing cobalt, with or without oxygen or hydrogen, and containing two or more other elements
- C01G 53/82: Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
- C30B 7/10: by application of pressure, e.g. hydrothermal processes
- H01M 4/364: {as mixtures}
- H01M 4/587: for inserting or intercalating light metals
- C30B 29/14: Phosphates
- H01M 2004/028: {Positive electrodes}
- H01M 2220/30: Batteries in portable systems, e.g. mobile phone, laptop
- Y02E 60/10: Energy storage using batteries
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01D: COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides C01B17/22; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia and cyanogen, containing nitrogen and other non-metals C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; phosphides 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; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- 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)
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

An object is to reduce variation in shape of crystals that are to be formed. Solutions containing respective raw materials are made in an environment where an oxygen concentration is lower than that in air, the solutions containing the respective raw materials are mixed in an environment where an oxygen concentration is lower than that in air to form a mixture solution, and with use of the mixture solution, a composite oxide is formed by a hydrothermal method.

## Claims

### Claim 1

(canceled)

### Claim 2

A production method comprising the steps of:
forming a first solution comprising Li in an atmosphere having an oxygen concentration lower than the oxygen concentration in air by dissolving a compound comprising Li in a first water having an oxygen concentration lower than or equal to 4.5 ppm;
forming a second solution comprising P in an atmosphere having an oxygen concentration lower than the oxygen concentration in air by dissolving a compound comprising P in a second water having an oxygen concentration lower than or equal to 4.5 ppm;
forming a third solution comprising one or more transition metal elements in an atmosphere having an oxygen concentration lower than the oxygen concentration in air by dissolving a compound comprising the one or more transition metal elements in a third water having an oxygen concentration lower than or equal to 4.5 ppm;
mixing the first solution and the second solution in an atmosphere having an oxygen concentration lower than the oxygen concentration in air to form a first mixed solution comprising Li and P;
mixing the third solution and the first mixed solution in an atmosphere having an oxygen concentration lower than the oxygen concentration in air to form a second mixed solution; and
forming a compound represented by Formula LiMPO4 from the second mixed solution by a hydrothermal method in an atmosphere having an oxygen concentration lower than the oxygen concentration in air,
wherein the one or more transition metal elements is one or more elements selected from the group consisting of Fe, Co, Ni and Mn, and
wherein M in LiMPO4 denotes the one or more transition metal elements.

### Claim 3 (depends on 2)

The production method according to claim 2, wherein forming the compound represented by Formula LiMPO4 is formed under a nitrogen atmosphere.

### Claim 4 (depends on 2)

The production method according to claim 2, wherein forming the compound represented by Formula LiMPO4 is formed under a mixed atmosphere of nitrogen and hydrogen.

### Claim 5 (depends on 2)

The production method according to claim 2, wherein the compound represented by Formula LiMPO4 has a crystal shape of a rectangular solid.

### Claim 6 (depends on 2)

A method for manufacturing a power storage device, wherein a positive electrode of the power storage device is formed using the compound formed by the production method according to claim 2.

### Claim 7

A production method comprising the steps of:
forming a first solution comprising Li in an atmosphere having an oxygen concentration lower than the oxygen concentration in air by dissolving a compound comprising Li in a first water performed a nitrogen bubbling;
forming a second solution comprising P in an atmosphere having an oxygen concentration lower than the oxygen concentration in air by dissolving a compound comprising P in a second water performed a nitrogen bubbling;
forming a third solution comprising one or more transition metal elements in an atmosphere having an oxygen concentration lower than the oxygen concentration in air by dissolving a compound comprising the one or more transition metal elements in a third water performed a nitrogen bubbling;
mixing the first solution and the second solution in an atmosphere having an oxygen concentration lower than the oxygen concentration in air to form a first mixed solution comprising Li and P;
mixing the third solution and the first mixed solution in an atmosphere having an oxygen concentration lower than the oxygen concentration in air to form a second mixed solution; and
forming a compound represented by Formula LiMPO4 from the second mixed solution by a hydrothermal method in an atmosphere having an oxygen concentration lower than the oxygen concentration in air,
wherein the one or more transition metal elements is one or more elements selected from the group consisting of Fe, Co, Ni and Mn, and
wherein M in LiMPO4 denotes the one or more transition metal elements.

### Claim 8 (depends on 7)

The production method according to claim 7, wherein each of the first water, the second water and the third water has an oxygen concentration lower than 4.5 ppm.

### Claim 9 (depends on 7)

The production method according to claim 7, wherein forming the compound represented by Formula LiMPO4 is formed under a nitrogen atmosphere.

### Claim 10 (depends on 7)

The production method according to claim 7, wherein forming the compound represented by Formula LiMPO4 is formed under a mixed atmosphere of nitrogen and hydrogen.

### Claim 11 (depends on 7)

The production method according to claim 7, wherein the compound represented by Formula LiMPO4 has a crystal shape of a rectangular solid.

### Claim 12 (depends on 7)

A method for manufacturing a power storage device, wherein a positive electrode of the power storage device is formed using the compound formed by the production method according to claim 7.