# US 2017/0288209 A1 · Lithium titanate structures for lithium ion batteries formed using element selective sputtering

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- Number: US 2017/0288209 A1
- Document ID: US20170288209A1
- Status: Published application
- Kind: A1
- Application number: 15/087,435
- Filed: 2016-03-31
- Published: 2017-10-05
- Earliest claimed: 2016-03-31
- Assignees: GM Global Technology Operations LLC
- Applicants: GM Global Technology Operations LLC
- Inventors: Zhongyi Liu
- Web page: https://patentgrep.com/patent/US20170288209A1

## CPC

- H01M 4/1391: of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- C01G 23/005: {Alkali titanates}
- C04B 35/62259: {Fibres based on titanium oxide}
- C04B 35/62675: {characterised by the treatment temperature}
- C04B 35/62855: {Refractory metal oxides}
- C23C 14/082: {of alkaline earth metals}
- H01M 4/0426: {Sputtering}
- H01M 4/0471: {involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis}
- 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 4/382: {Lithium (H01M4/405 takes precedence)}
- H01M 4/405: {Alloys based on lithium}
- H01M 4/485: of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy (H01M4/505, H01M4/525 take precedence)
- H01M 4/622: {being polymers}
- 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
- C01P 2002/32: spinel-type (AB2O4)
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/16: Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
- C01P 2004/32: Spheres
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2006/12: Surface area
- C01P 2006/40: Electric properties
- C04B 2235/3203: Lithium oxide or oxide-forming salts thereof
- C04B 2235/522: Oxidic
- C04B 2235/5276: Whiskers, spindles, needles or pins
- H01M 4/623: {fluorinated polymers}
- H01M 2004/027: {Negative electrodes}
- Y02E 60/10: Energy storage using batteries
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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)
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- 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

## Abstract

A method is provided in which a lithium titanate precursor structure is subjected to element selective sputtering to form a lithium titanate structure including a lithium titanate core and a conformal layer on the lithium titanate core, wherein the conformal layer includes titanium oxide. A method of preparing an electrode for a lithium ion battery, wherein the electrode includes lithium titanate structures, is also provided.

## Claims

### Claim 1

A method, comprising:
subjecting a lithium titanate precursor structure to element selective sputtering to form a lithium titanate structure including a lithium titanate core and a conformal layer on the lithium titanate core, wherein the conformal layer includes titanium oxide.

### Claim 2 (depends on 1)

The method as defined in claim 1 wherein the element selective sputtering is performed by any of electron sputtering, plasma sputtering, laser sputtering, and X-ray sputtering.

### Claim 3 (depends on 2)

The method as defined in claim 2 wherein the element selective sputtering is performed by a plasma in a rotary plasma system.

### Claim 4 (depends on 1)

The method as defined in claim 1 wherein the lithium titanate has a surface, following the element selective sputtering, that is essentially devoid of lithium.

### Claim 5 (depends on 1)

The method as defined in claim 1 wherein the conformal layer has substantially no lithium.

### Claim 6 (depends on 1)

The method as defined in claim 1, further comprising heat-treating the lithium titanate structure.

### Claim 7 (depends on 6)

The method as defined in claim 6 wherein the lithium titanate structure is heat-treated at a temperature ranging from about 400° C. to about 800° C. for a period of time ranging from about 1 hour to about 24 hours.

### Claim 8 (depends on 1)

The method as defined in claim 1, further comprising reducing gas production in a lithium ion battery by:
incorporating a plurality of the lithium titanate structures into a negative electrode;
incorporating the negative electrode into a lithium ion battery; and
cycling the lithium ion battery.

### Claim 9

A method, comprising:
subjecting a lithium titanate precursor structure to element selective sputtering to form a lithium titanate structure including a lithium titanate core and a conformal layer on the lithium titanate core, wherein the conformal layer includes titanium oxide;
incorporating a plurality of the lithium titanate structures into a negative electrode;
incorporating the negative electrode into a lithium ion battery; and
cycling the lithium ion battery.

### Claim 10 (depends on 9)

The method as defined in claim 9 wherein the element selective sputtering is performed by any of electron sputtering, plasma sputtering, laser sputtering, and X-ray sputtering.

### Claim 11 (depends on 10)

The method as defined in claim 10 wherein the element selective sputtering is performed by a plasma in a rotary plasma system.

### Claim 12 (depends on 9)

The method as defined in claim 9 wherein the lithium titanate has a surface, following the element selective sputtering, that is essentially devoid of lithium.

### Claim 13 (depends on 9)

The method as defined in claim 9 wherein the conformal layer has substantially no lithium.

### Claim 14 (depends on 9)

The method as defined in claim 9, further comprising heat-treating the lithium titanate structure.

### Claim 15 (depends on 14)

The method as defined in claim 14 wherein the lithium titanate structure is heat-treated at a temperature ranging from about 400° C. to about 800° C. for a period of time ranging from about 1 hour to about 24 hours.

### Claim 16 (depends on 9)

The method as defined in claim 9 wherein:
the lithium titanate structures are recovered from the element selective sputtering as lithium titanate powder;
the powder is mixed with conductive carbon and polymer binder in a solvent to form a slurry; and
the slurry is coated onto a current collector material and dried to form the negative electrode.