# US 9,437,866 B2 · Process for producing lithium vanadium phosphate-carbon composite

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- Number: US 9,437,866 B2
- Document ID: US9437866B2
- Status: Granted
- Kind: B2
- Application number: 13/823,612
- Filed: 2011-09-22
- Published: 2013-08-22
- Granted: 2016-09-06
- Earliest claimed: 2010-09-27
- Assignees: Nippon Chemical Industrial Co., Ltd.; Fuji Jukogyo Kabushiki Kaisha
- Applicants: Tsutomu Kikuchi; Kazuki Takimoto; Hideo Yanagita
- Inventors: Tsutomu Kikuchi; Kazuki Takimoto; Hideo Yanagita
- Web page: https://patentgrep.com/patent/US9437866B2

## CPC

- H01M 4/1397: of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
- C01B 25/45: containing plural metal, or metal and ammonium
- H01M 4/04: Processes of manufacture in general
- H01M 4/13: Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M 4/136: Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
- H01M 4/5825: {Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines}
- H01M 4/625: {Carbon or graphite}
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- 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
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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 process for producing a lithium vanadium phosphate-carbon composite includes a first step that includes mixing a lithium source, a tetravalent or pentavalent vanadium compound, a phosphorus source, and a conductive carbon material source that produces carbon through pyrolysis, in an aqueous solvent to prepare a raw material mixture, a second step that includes heating the raw material mixture to effect a precipitation reaction to obtain a reaction mixture that includes a precipitate, a third step that includes subjecting the reaction mixture that includes the precipitate to wet grinding using a media mill to obtain a slurry that includes ground particles, a fourth step that includes spray-drying the slurry that includes the ground particles to obtain a reaction precursor, and a fifth step that includes calcining the reaction precursor at 600 to 1300° C. in an inert gas atmosphere or a reducing atmosphere. A lithium vanadium phosphate-carbon composite produced by the process may provide a lithium secondary battery with excellent battery performance (e.g., high discharge capacity) when used as a cathode active material.

## Claims

### Claim 1

A process for producing a lithium vanadium phosphate-carbon composite that includes lithium vanadium phosphate having a NASICON structure, and a conductive carbon material, the process comprising:
a first step that includes mixing a lithium source, a tetravalent or pentavalent vanadium compound, a phosphorus source, and a conductive carbon material source that produces carbon through pyrolysis, in an aqueous solvent to prepare a raw material mixture;
a second step that includes heating the raw material mixture to 60 to 100° C. to effect a precipitation reaction to obtain a reaction mixture that includes a precipitate;
a third step that includes subjecting the reaction mixture that includes the precipitate to wet grinding using a media mill to obtain a slurry that includes ground particles;
a fourth step that includes spray-drying the slurry that includes the ground particles to obtain a reaction precursor; and
a fifth step that includes calcining the reaction precursor at 600 to 1300° C. in an inert gas atmosphere or a reducing atmosphere,
the phosphorus source being at least one phosphorus source selected from phosphoric acid, polyphosphoric acid, phosphoric anhydride, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, and ammonium phosphate, and
the precipitate including at least lithium phosphate and vanadium hydrogen phosphate.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the ground particles included in the slurry obtained by the third step have an average particle size of 2 μm or less.

### Claim 3 (depends on 1)

The process according to claim 1, wherein the lithium source is lithium hydroxide.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the tetravalent or pentavalent vanadium compound is vanadium pentoxide.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the phosphorus source is phosphoric acid.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the conductive carbon material source is a saccharide.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the first step further includes mixing an Me source (Me is a metal element or a transition metal element other than V that has an atomic number equal to or larger than 11) into the raw material mixture.