# US 10,865,480 B2 · Vapour deposition method for preparing amorphous lithium-containing compounds

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- Number: US 10,865,480 B2
- Document ID: US10865480B2
- Status: Granted
- Kind: B2
- Application number: 15/110,638
- Filed: 2015-01-07
- Published: 2016-11-24
- Granted: 2020-12-15
- Earliest claimed: 2014-01-08
- Assignees: Ilika Technologies Limited; Toyota Motor Corporation
- Applicants: Ilika Technologies Limited; Toyota Motor Corporation
- Inventors: Brian Elliott Hayden; Duncan Clifford Alan Smith; Christopher Edward Lee; Alexandros Anastasopoulos; Chihiro Yada; Laura Mary Perkins; David Michael Laughman
- Web page: https://patentgrep.com/patent/US10865480B2

## CPC

- C23C 16/505: using radio frequency discharges
- C03C 3/04: containing silica
- C03C 3/089: containing boron
- C03C 4/18: for ion-sensitive glass
- C23C 14/0021: {Reactive sputtering or evaporation}
- C23C 14/0676: {Oxynitrides}
- C23C 14/08: Oxides (C23C14/10 takes precedence)
- C23C 14/24: Vacuum evaporation
- C23C 16/308: {Oxynitrides}
- C23C 16/40: Oxides
- C23C 16/452: by activating reactive gas streams before {their} introduction into the reaction chamber, e.g. by {ionisation} or addition of reactive species
- H01M 10/052: Li-accumulators
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- H01M 10/0562: Solid materials
- C03C 2204/00: Glasses, glazes or enamels with special properties
- H01M 2300/0071: Oxides
- Y02E 60/10: Energy storage using batteries
- 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)
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A vapour deposition method for preparing an amorphous lithium-containing oxide or oxynitride compound not containing phosphorous comprises providing a vapour source of each component element of the compound, including at least a source of lithium, a source of oxygen, a source of nitrogen in the case of an oxynitride compound, and a source or sources of one or more glass-forming elements; heating a substrate to substantially 180° C. or above; and co-depositing the component elements from the vapour sources onto the heated substrate wherein the component elements react on the substrate to form the amorphous compound.

## Claims

### Claim 1

A vapour deposition method for preparing an amorphous lithium-containing oxide or oxynitride compound not containing phosphorous, the method comprising:
providing a vapour source of each component element of the compound, wherein the vapour sources comprise at least a source of lithium, a source of oxygen, and a source or sources of one or more glass-forming elements;
heating a substrate to 180° C. or above; and
co-depositing the component elements from the vapour sources onto the heated substrate, wherein the component elements react on the substrate to form the amorphous compound,
in which the source or sources of one or more glass-forming elements comprises:
a. a source of boron and a source of silicon, and the amorphous compound is lithium borosilicate; or
b. a source of boron, a source of silicon and a source of nitrogen, and the amorphous compound is nitrogen-doped lithium borosilicate.

### Claim 2 (depends on 1)

The vapour deposition method according to claim 1, in which the vapour source of oxygen is a vapour source of atomic oxygen.

### Claim 3 (depends on 2)

The vapour deposition method according to claim 2, in which the amorphous compound is a lithium-containing oxynitride compound containing the one or more glass-forming elements and not containing phosphorous, and the method comprises introducing nitrogen into a feed of a plasma source of the atomic oxygen to provide a mixed oxygen-nitrogen plasma for co-deposition onto the heated substrate.

### Claim 4 (depends on 1)

The vapour deposition method according to claim 1, in which co-depositing the component elements onto the heated substrate comprises co-depositing the component elements directly onto a surface of the heated substrate or onto one or more layers supported on the substrate.

### Claim 5 (depends on 1)

The method according to claim 1, in which the source or sources of the one or more glass-forming elements comprises a source of boron and a source of silicon, and the amorphous compound is lithium borosilicate.

### Claim 6 (depends on 5)

The vapour deposition method according to claim 5, wherein the heating the substrate includes heating the substrate to a temperature in a temperature range between 180° C. and 350° C.

### Claim 7 (depends on 1)

The method according to claim 1, in which the source or sources of the one or more glass-forming elements comprises a source of boron, a source of silicon and a source of nitrogen, and the amorphous compound is nitrogen-doped lithium borosilicate.

### Claim 8 (depends on 7)

The vapour deposition method according to claim 7, wherein the heating the substrate includes heating the substrate to a temperature in a temperature range between 180° C. and 350° C.

### Claim 9 (depends on 1)

A method of making a battery, comprising depositing an electrolyte of the battery as a layer of the amorphous lithium-containing oxide or oxynitride compound containing the one or more glass-forming elements and not containing phosphorous using the vapour deposition method according to claim 1.

### Claim 10

A vapour deposition method for preparing an amorphous lithium-containing oxide or oxynitride compound not containing phosphorous, the method comprising:
providing a vapour source of each component element of the compound, wherein the vapour sources comprise at least a source of lithium, a source of molecular oxygen, and source or sources of one or more glass-forming elements;
providing a substrate at a temperature below 100° C.; and
co-depositing the component elements from the vapour sources onto the substrate, wherein the component elements react on the substrate to form the amorphous compound,
in which the source or sources of one or more glass-forming elements comprises:
a. a source of boron and a source of silicon, and the amorphous compound is lithium borosilicate; or
b. a source of boron, a source of silicon and a source of nitrogen, and the amorphous compound is nitrogen-doped lithium borosilicate.

### Claim 11 (depends on 10)

The vapour deposition method according to claim 10, in which co-depositing the component elements onto the substrate comprises co-depositing the component elements directly onto a surface of the substrate or co-depositing the component elements onto one or more layers supported on the substrate.

### Claim 12 (depends on 10)

The method according to claim 10, in which the source or sources of the one or more glass-forming elements comprises a source of boron and a source of silicon, and the amorphous compound is lithium borosilicate.

### Claim 13 (depends on 12)

The vapour deposition method according to claim 12, wherein the providing a substrate at a temperature below 100° C. includes providing the substrate at a temperature in a temperature range between 18° C. and 30° C.

### Claim 14 (depends on 10)

The method according to claim 10, in which the source or sources of the one or more glass-forming elements comprises a source of boron, a source of silicon and a source of nitrogen, and the amorphous compound is nitrogen-doped lithium borosilicate.

### Claim 15 (depends on 14)

The vapour deposition method according to claim 14, wherein the providing a substrate at a temperature below 100° C. includes providing the substrate at a temperature in a temperature range between 18° C. and 30° C.