# US 9,039,926 B2 · Production process for composite oxide, positive-electrode active material for lithium-ion secondary battery and lithium-ion secondary battery

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- Number: US 9,039,926 B2
- Document ID: US9039926B2
- Status: Granted
- Kind: B2
- Application number: 13/577,523
- Filed: 2011-02-07
- Published: 2012-12-20
- Granted: 2015-05-26
- Earliest claimed: 2010-02-08
- Assignees: Kabushiki Kaisha Toyota Jidoshokki
- Applicants: Ryota Isomura; Hitotoshi Murase; Naoto Yasuda
- Inventors: Ryota Isomura; Hitotoshi Murase; Naoto Yasuda
- Web page: https://patentgrep.com/patent/US9039926B2

## CPC

- H01M 4/505: of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01G 45/1228: of the type (MnO2)-, e.g. LiMnO2 or Li(MxMn1-x)O2
- C01P 2002/54: one element only
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/76: by a space-group or by other symmetry indications
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/40: Electric properties
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- H01M 2220/20: Batteries in motive systems, e.g. vehicle, ship, plane
- Y02E 60/10: Energy storage using batteries
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- Y02T 10/70: Energy storage systems for electromobility, e.g. batteries
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- 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)
- 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
- Y02T: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION

## Abstract

A production process for composite oxide expressed by a compositional formula: LiMn1-xAxO2, where “A” is one or more kinds of metallic elements other than Mn; and 0≦“x”<1, obtained by preparing a raw-material mixture by mixing a metallic-compound raw material and a molten-salt raw material with each other, the metallic-compound raw material at least including an Mn-containing nitrate that includes one or more kinds of metallic elements in which Mn is essential, the molten-salt raw material including lithium hydroxide and lithium nitrate, and exhibiting a proportion of the lithium nitrate with respect to the lithium hydroxide (Lithium Nitrate/Lithium Hydroxide) that falls in a range of from 1 or more to 3 or less by molar ratio; reacting the raw-material mixture at 500° C. or less by melting it; and recovering the composite oxide being generated from the raw-material mixture that has undergone the reaction.

## Claims

### Claim 1

A production process for composite oxide being characterized in that:
it is a production process for composite oxide being expressed by a compositional formula: LiMn1-xAxO2, where “A” is one or more kinds of metallic elements other than Mn; 0≦“x”<1; and an averaged oxidation number of Mn falls in a range of from 2.8 to 3.2;
said composite oxide is obtained via the following:
a raw-material mixture preparation step of preparing a raw-material mixture by mixing a metallic-compound raw material and a molten-salt raw material with each other,
the metallic-compound raw material at least including an Mn-containing nitrate that includes one or more kinds of metallic elements in which Mn is essential,
the molten-salt raw material including lithium hydroxide and lithium nitrate, and exhibiting a proportion of the lithium nitrate with respect to the lithium hydroxide, Lithium Nitrate/Lithium Hydroxide, that falls in a range of from 1.2 to 3 by molar ratio;
a molten reaction step of reacting said raw-material mixture at 500° C. or less by melting it; and
a recovery step of recovering said composite oxide being generated from said raw-material mixture that has undergone the reaction,
wherein the molten-salt raw material does not include lithium peroxide; and
said composite oxide has a crystal structure belonging to an orthorhombic-system space group.

### Claim 2 (depends on 1)

The production process for composite oxide as set forth in claim 1, wherein said metallic-compound raw material further includes a second nitrate including one or more kinds of metallic elements other than Mn.

### Claim 3 (depends on 1)

The production process for composite oxide, wherein a mixed-nitrate aqueous-solution preparation step, in which an aqueous solution of nitrate including at least two kinds of metallic elements is prepared, is further carried out before the raw-material mixture preparation step in the production process for composite oxide as set forth in claim 1, and then said metallic-compound raw material including the aqueous solution is employed at the raw-material mixture preparation step.

### Claim 4 (depends on 1)

The production process for composite oxide as set forth in claim 1, wherein said raw-material mixture exhibits a proportion of the metallic elements, which are included in said metallic-compound raw material, with respect to lithium metal, which is included in said molten-salt raw material, Metallic Elements in Metallic-compound Raw Material/Lithium Metal in Molten-salt Raw Material, the proportion falling in a range of from 0.01 to 0.2 by molar ratio.

### Claim 5 (depends on 1)

The production process for composite oxide as set forth in claim 1 further including a proton substitution step, in which a part of Li in said composite oxide is substituted by proton (H), after said recovery step.