# US 11,111,576 B2 · Method for producing nanostructured layers

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- Number: US 11,111,576 B2
- Document ID: US11111576B2
- Status: Granted
- Kind: B2
- Application number: 15/578,809
- Filed: 2016-04-27
- Published: 2018-06-14
- Granted: 2021-09-07
- Earliest claimed: 2015-06-10
- Assignees: Forschungszentrum Juelich GmbH
- Applicants: Forschungszentrum Juelich GmbH
- Inventors: Aiko Buenting; Sven Uhlenbruck
- Web page: https://patentgrep.com/patent/US11111576B2

## CPC

- C23C 14/3414: {Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C23C 14/06: characterised by the coating material ({C23C14/0021} , C23C14/04 take precedence)
- C23C 14/0605: {Carbon}
- C23C 14/35: by application of a magnetic field, e.g. magnetron sputtering {(C23C14/3457 takes precedence)}
- H01M 4/0404: {by coating on electrode collectors}
- H01M 4/0426: {Sputtering}
- H01M 4/131: Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 4/136: Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
- H01M 4/1391: of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 4/1397: of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
- H01M 4/525: of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
- H01M 4/5825: {Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines}
- 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)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- 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

According to a method for producing a nanostructured electrode for an electrochemical cell, in which active material is applied to an electrically conductive substrate, the active material is deposited on the electrically conductive substrate by magnetron sputtering in one process step, a ceramic target comprising an electrode material having an additional carbon proportion between 0.1 and 25% by weight is used, the substrate being kept at temperatures between 400° C. and 1200° C. during the deposition, in such a way that a fibrous porous network is formed.

## Claims

### Claim 1

A method for producing a nanostructured electrode for an electrochemical cell, the method comprising:
providing an electrically conductive substrate and a target, wherein the target comprises a ceramic electrode material and carbon, the carbon proportion of the target being between 0.1 and 25% by weight;
heating the electrically conductive substrate to a temperature of between 400° C. and 1200° C.; and
depositing, via a single magnetron sputtering process step, the ceramic electrode material onto the electrically conductive substrate so as to form a fibrous porous network of fibers having a diameter in a range of 10-200 nm,
wherein the temperature of the substrate remains between 400° C. and 1200° C. during the depositing,
wherein the magnetron sputtering process step is performed with a power density of 0.5 to 2 W/cm2, and
wherein the magnetron sputtering process step provides a deposition rate of 0.1 to 1 mg·h/cm2.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the ceramic electrode material comprises one or more of LiFePO4, Li4Ti5O12, lithium metal oxides of the LiMxO2 type, where M=Co, Ni, Mn, Al, LiMn2O4 spinel, lithium metal phosphates of the LiMPO4 type, comprising Fe, Mn, Co, V, V2O5, or conversion materials.

### Claim 3 (depends on 1)

The method according to claim 1, wherein the carbon proportion of the target is between 2 and 7% by weight.

### Claim 4 (depends on 1)

The method according to claim 1, wherein argon, argon/oxygen, argon/nitrogen, argon/hydrogen or argon/hydrocarbons are used as a working gas in the magnetron sputtering process step.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the magnetron sputtering process step is performed with a gas flow of 5 to 50 sccm.

### Claim 6 (depends on 1)

The method according to claim 1, wherein a duration of the magnetron sputtering process step is between 10 minutes and 10 hours.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the power density is 1.0 to 1.5 W/cm2.

### Claim 8 (depends on 5)

The method according to claim 5, wherein the gas flow is 10 to 25 sccm.

### Claim 9 (depends on 1)

The method according to claim 1, wherein the deposition rate is 0.2 to 0.5 mg·h/cm2.

### Claim 10 (depends on 6)

The method according to claim 6, wherein the duration of the magnetron sputtering process step is between 1 and 5 hours.

### Claim 11 (depends on 1)

The method according to claim 1, wherein the ceramic electrode material is LiCoO2.

### Claim 12 (depends on 1)

The method according to claim 1, wherein the electrically conductive substrate is thermally oxidized.

### Claim 13 (depends on 12)

The method according to claim 12, wherein the electrically conductive substrate is a coated, thermally oxidized silicon wafer.

### Claim 14 (depends on 13)

The method according to claim 13, wherein the thermally oxidized silicon wafer is coated with titanium-nitride.