# US 11,078,565 B2 · Thermal evaporation process for manufacture of solid state battery devices

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- Number: US 11,078,565 B2
- Document ID: US11078565B2
- Status: Granted
- Kind: B2
- Application number: 15/495,840
- Filed: 2017-04-24
- Published: 2017-12-14
- Granted: 2021-08-03
- Earliest claimed: 2011-11-08
- Assignees: Sakti3, Inc.
- Applicants: Sakti3, Inc.
- Inventors: Myoungdo Chung; HyonCheol Kim; Ann Marie Sastry; Marc Langlois
- Web page: https://patentgrep.com/patent/US11078565B2

## CPC

- C23C 14/0031: {Bombardment of substrates by reactive ion beams}
- C23C 14/0676: {Oxynitrides}
- C23C 14/083: {of refractory metals or yttrium}
- C23C 14/5833: {Ion beam bombardment}
- H01M 4/0423: {Physical vapour deposition}
- H01M 4/131: Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 4/1391: of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 4/382: {Lithium (H01M4/405 takes precedence)}
- H01M 4/48: of inorganic oxides or hydroxides
- H01M 4/483: {for non-aqueous cells (H01M4/485 takes precedence)}
- H01M 4/5825: {Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines}
- H01M 6/40: Printed batteries {, e.g. thin film batteries}
- H01M 10/0562: Solid materials
- H01M 10/0585: of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators
- H01M 50/403: Manufacturing processes of separators, membranes or diaphragms
- H01M 2004/028: {Positive electrodes}
- Y02E 60/10: Energy storage using batteries
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- 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)
- 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
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A method for manufacturing a solid-state battery device. The method can include providing a substrate within a process region of an apparatus. A cathode source and an anode source can be subjected to one or more energy sources to transfer thermal energy into a portion of the source materials to evaporate into a vapor phase. An ionic species from an ion source can be introduced and a thickness of solid-state battery materials can be formed overlying the surface region by interacting the gaseous species derived from the plurality of electrons and the ionic species. During formation of the thickness of the solid-state battery materials, the surface region can be maintained in a vacuum environment from about 10−6 to 10−4 Torr. Active materials comprising cathode, electrolyte, and anode with non-reactive species can be deposited for the formation of modified modulus layers, such a void or voided porous like materials.

## Claims

### Claim 1

A method for manufacturing a cathode for a solid-state battery device using a flash process comprising:
providing a substrate on a transfer device;
continuously feeding a metal oxide cathode source material to an evaporation source, wherein the evaporation source is located under the substrate;
subjecting the metal oxide cathode source material to thermal energy to cause a portion of the source to evaporate into a vapor phase free from undesirable metal oxide species;
forming a metal oxide material layer overlying the substrate by condensing the vapor phase as the substrate moves either in a first direction or a second direction;
subjecting the metal oxide material layer to an ion source while the thickness of metal oxide material layer is being formed to incorporate a nitrogen content of the metal oxide material layer of 2% to 4% to achieve an electrical conductivity of the metal oxide material layer of 10−6 to 10−5 S/m; and
maintaining the substrate in a vacuum environment during the formation of the metal oxide material layer.

### Claim 2 (depends on 1)

The method of claim 1, wherein the forming of the metal oxide material layer occurs at a rate of about 100 to 10,000 Angstroms per second per 100 square centimeters; wherein the ion source is an ion beam or an ion shower.

### Claim 3 (depends on 1)

The method of claim 1, wherein the substrate moves at a rate of about 1 inches/min to about 10 feet/min.

### Claim 4 (depends on 1)

The method of claim 1, wherein cathode source comprises vanadium oxide.

### Claim 5 (depends on 1)

The method of claim 1, wherein the metal oxide cathode source comprises vanadium oxide, manganese oxide, iron oxide, nickel oxide, sulphur oxide, cobalt oxide, or magnesium oxide.

### Claim 6 (depends on 1)

The method of claim 1, wherein subjecting the metal oxide layer comprises introducing a dopant species into the metal oxide material layer to cause an increase in conductivity of the metal oxide material layer and cause an increase in ionic diffusivity of the metal oxide material layer.

### Claim 7 (depends on 1)

The method of claim 1, further comprising introducing a dopant species into the metal oxide material layer, the dopant comprising nitrogen, oxygen, carbon, fluorine, silver, molybdenum, copper, tin, aluminium, iodine, phosphorous, or silicon.

### Claim 8 (depends on 1)

The method of claim 1, wherein the thermal energy is provided by an e-gun, a sputtering process or on a hot wall reactor region; wherein the hot wall reactor region is characterized by a temperature ranging from about 600 to 1200 Degrees Centigrade; wherein the metal oxide cathode material is vanadium oxide; wherein the ion source is provided at an energy from about 100 to about 400 electron volts.

### Claim 9 (depends on 8)

The method of claim 8, wherein the thermal energy is provided by a region of a hot wall reactor and further comprising a shaped mask device configured between the region of the hot wall reactor and the substrate, the shaped mask device configured to be coupled to a heating device to maintain the shaped mask device essentially free from a residue from the metal oxide cathode source and positioned to allow either demarcation of the cathode source r oblique angle deposition for the formation of voids or a porous cathode or cathode modification layer.

### Claim 10 (depends on 1)

The method of claim 1, wherein the transfer device comprises a first drum coupled to a second drum and configured in a reel to reel.

### Claim 11 (depends on 1)

The method of claim 1, wherein the substrate is configured for single or multiple passes of the substrate in the vacuum environment.

### Claim 12 (depends on 1)

The method of claim 1, wherein the cathode source is one of a plurality of sources within the vacuum environment.

### Claim 13 (depends on 1)

The method of claim 1, wherein the metal oxide material layer comprises a mixture of cathode and anode material co-deposited to form a cathode layer in a partially or fully discharged state with modified intercalation stresses.

### Claim 14 (depends on 1)

The method of claim 1, wherein the vapor phase comprises entrained non-reactive species in the shape of nano rods, cones, columns, fibers, or spheres, with or without a binder, to form voids or a voided porous cathode or cathode modification layer.

### Claim 15 (depends on 1)

The method of claim 1, wherein the energy source comprises a plurality of respective energy sources which are configured to be combined.