# US 2022/0045307 A1 · Methods, systems, and compositions for the liquid-phase deposition of thin films onto the surface of battery electrodes

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- Number: US 2022/0045307 A1
- Document ID: US20220045307A1
- Status: Published application
- Kind: A1
- Application number: 17/410,797
- Filed: 2021-08-24
- Published: 2022-02-10
- Earliest claimed: 2017-06-20
- Assignees: Coreshell Technologies, Incorporated
- Applicants: Coreshell Technologies, Inc.
- Inventors: Sourav Basu; Jonathan Tan
- Web page: https://patentgrep.com/patent/US20220045307A1

## CPC

- H01M 4/0402: {Methods of deposition of the material}
- B05C 5/00: Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work (B05C7/00 takes precedence; essentially involving spraying or electrostatic projection B05B)
- B05C 9/00: Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
- H01M 4/0409: {by a doctor blade method, slip-casting or roller coating}
- H01M 4/0419: {involving spraying}
- H01M 4/049: {Manufacturing of an active layer by chemical means}
- H01M 4/139: Processes of manufacture
- H01M 4/587: for inserting or intercalating light metals
- H01M 4/62: Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M 6/005: {Devices for making primary cells}
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- B05C 3/00: Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05D 1/02: performed by spraying
- B05D 1/18: performed by dipping
- B05D 1/26: performed by applying the liquid or other fluent material from an outlet device in contact with, or almost in contact with, the surface
- B05D 1/28: performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers
- B05D 1/38: with intermediate treatment (intermediate treatment per se B05D3/00)
- C23C 18/1655: {Process features}
- H01M 4/36: Selection of substances as active materials, active masses, active liquids
- H01M 4/362: {Composites}
- H01M 4/38: of elements or alloys
- H01M 10/0409: {for cells with wound electrodes}
- H01M 10/0587: of accumulators having only wound construction elements, i.e. wound positive electrodes, wound negative electrodes and wound separators
- H01M 2004/021: {Physical characteristics, e.g. porosity, surface area}
- H01M 2004/027: {Negative electrodes}
- 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
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- B05C: APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (spraying apparatus, atomising apparatus, nozzles B05B; plant for applying liquids or other fluent materials to objects by electrostatic spraying B05B5/08)
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- 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)
- 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

Methods, systems, and compositions for the liquid-phase deposition (LPD) of thin films. The thin films can be coated onto the surface of porous components of electrochemical devices, such as battery electrodes. Embodiments of the present disclosure achieve a faster, safer, and more cost-effective means for forming uniform, conformal layers on non-planar microstructures than known methods. In one aspect, the methods and systems involve exposing the component to be coated to different liquid reagents in sequential processing steps, with optional intervening rinsing and drying steps. Processing may occur in a single reaction chamber or multiple reaction chambers.

## Claims

### Claim 1

(canceled)

### Claim 2

A system for coating a thin film onto a lithium-ion battery electrode, comprising:
a plurality of chambers, the plurality of chambers including:
a first reaction chamber configured to apply a first solution to active material of the lithium-ion battery electrode, the first solution including at least a first reagent that reacts with the active material of the lithium-ion battery electrode to produce a partially coated lithium-ion battery electrode having a layer comprising an adsorbed first reagent on a surface of the active material of the lithium-ion battery electrode;
a second reaction chamber configured to apply a second solution to the partially coated lithium-ion battery electrode, the second solution including at least a second reagent that reacts with the first adsorbed reagent bonded onto the surface of the active material of the partially coated lithium-ion battery electrode to produce a fully coated lithium ion battery electrode having an artificial solid electrolyte interphase (SEI) comprising a monolayer of thin film coated onto the surface of the active material, the monolayer of thin film comprising a compound generated from the reaction of the second reagent and the adsorbed first reagent;
a conveyance apparatus including a series of rollers for conveying the battery electrode to the first reaction chamber and to the second reaction chamber.

### Claim 3 (depends on 2)

The system of claim 2, wherein:
the first reaction chamber holds a quantity of the first solution and the conveyance apparatus causes the active material of the lithium-ion battery electrode to be immersed in the quantity of the first solution; and
the second reaction chamber holds a quantity of the second solution and the conveyance apparatus causes the partially coated lithium-ion battery electrode to be immersed in the quantity of the second solution.

### Claim 4 (depends on 2)

The system of claim 2, wherein:
the first solution is applied to the active material of the lithium-ion battery electrode by spraying the active material of the lithium-ion battery electrode with the first solution in the first reaction chamber; and
the second solution is applied to the battery electrode by spraying the partially coated lithium ion battery electrode with the second reagent in the second reaction chamber.

### Claim 5 (depends on 2)

The system of claim 2, comprising a die coater to dispense the first solution onto the active material of the lithium-ion battery electrode.

### Claim 6 (depends on 2)

The system of claim 2, comprising a gravure roller to apply the first solution to the active material of the lithium-ion battery electrode.

### Claim 7 (depends on 2)

The system of claim 2, wherein:
the lithium-ion battery electrode is a sheet or a foil,
a first portion of the lithium-ion battery electrode is coupled to a leader material to guide the lithium-ion battery electrode through the conveyance apparatus; and
the leader material is free of lithium-ion battery electrode active material.

### Claim 8 (depends on 2)

The system of claim 2, comprising one or more rinsing chambers disposed between the first reaction chamber and the second reaction chamber, individual rinsing chambers of the one or more rinsing chambers configured to apply a rinsing solution comprising a rinsing solvent to rinse excess first solution from the partially coated lithium-ion battery electrode.

### Claim 9 (depends on 8)

The system of claim 8, comprising a filtration apparatus coupled to a rinsing chamber of the one or more rinsing chambers, the filtration apparatus configured to produce a retentate stream that is enriched in unreacted first reagent and depleted in the rinsing solvent and a permeate stream enriched in the rinsing solvent and depleted in unreacted first reagent.

### Claim 10 (depends on 9)

The system of claim 9, wherein the retentate stream is provided to the first reaction chamber and the permeate stream is provided to the rinsing chamber.

### Claim 11 (depends on 8)

The system of claim 8, comprising a first roller disposed above the first reaction chamber, a second roller disposed within the first reaction chamber, and a third roller disposed between the first reaction chamber and a rinsing chamber of the one or more rinsing chambers and above the first reaction chamber and the rinsing chamber;
wherein the first roller operates in conjunction with the second roller to cause the active material of the lithium-ion battery electrode to move down into the first reaction chamber for a residence time and the second roller operates in conjunction with the third roller to cause the partially coated lithium-ion battery electrode to move upward and out of the first reaction chamber.

### Claim 12 (depends on 8)

The system of claim 8, wherein the filtration apparatus operates using at least one of membrane separation, chemical precipitation, ion-exchange, electrochemical removal, physical adsorption, or flow filtration chromatography.

### Claim 13 (depends on 8)

The system of claim 8, comprising:
an additional rinsing chamber disposed after the second reaction chamber, the additional rinsing chamber configured to apply an additional rinsing solution comprising an additional rinsing solvent to rinse excess second solution from the fully coated lithium-ion battery electrode; and
an additional filtration apparatus coupled to the additional rinsing chamber, the additional filtration apparatus configured to produce an additional retentate stream that is enriched in unreacted first reagent and depleted in the rinsing solvent and an additional permeate stream enriched in the rinsing solvent and depleted in unreacted first reagent.

### Claim 14 (depends on 13)

The system of claim 13, wherein the additional retentate stream is provided to the second reaction chamber and the additional permeate stream is provided to the additional rinsing chamber.

### Claim 15 (depends on 13)

The system of claim 13, wherein the second solution is an ionic solution and the second solution is filtered using a filtration column.

### Claim 16 (depends on 13)

The system of claim 13, wherein the second solution comprises an organometallic compound and the second solution is filtered using a tangential flow filtration system.

### Claim 17 (depends on 13)

The system of claim 13, comprising a fourth roller disposed within the rinsing chamber, a fifth roller disposed between the rinsing chamber and the second reaction chamber and above the rinsing chamber and the second reaction chamber; and a sixth roller disposed within the second reaction chamber; and wherein:
the third roller operates in conjunction with the fourth roller to cause the partially coated lithium-ion battery electrode to move downward into the rinsing chamber;
the fourth roller and the fifth roller cause the partially coated lithium-ion battery electrode to move upward and out of the rinsing chamber; and
the fifth roller and the sixth roller cause the partially coated lithium-ion battery electrode to move downward into the second reaction chamber for an additional residence time to produce the fully coated lithium ion battery electrode having the artificial SEI.

### Claim 18 (depends on 2)

The system of claim 2, comprising:
a first sensor to determine an amount of the first solution in the first reaction chamber,
a second sensor to determine an amount of the second solution in the second reaction chamber;
a first valve for regulating the amount of the first solution in the first reaction chamber;
a second valve for regulating the amount of the second solution in the second reaction chamber,
at least one pump to provide the first solution to the first reaction chamber and the second solution to the second reaction chamber;
a motor for driving the conveyance apparatus; and
a computer for operating the conveyance apparatus.

### Claim 19 (depends on 2)

The system of claim 2, wherein the compound generated by the reaction of the absorbed first reagent and the second reagent comprises one or more transition metal dichalcogenides.

### Claim 20 (depends on 2)

The system of claim 2, wherein the compound generated by the reaction of the absorbed first reagent and the second reagent comprises at least one of polyethylene oxide (PEO), poly vinyl alcohol (PVA), poly methyl methacrylate (PMMA), poly dimethyl siloxane (PDMS), or poly vinyl pyrollidone (PVP).

### Claim 21 (depends on 2)

The system of claim 2, wherein the artificial SEI does not contribute to inter-particle resistance and the compound generated by the reaction of the absorbed first reagent and the second reagent is selected from one of the following:
(a) binary oxides of type AxOy, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x and y are stoichiometric coefficients;
(b) ternary oxides of type AxByOz, where A and B are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x, y and z are stoichiometric coefficients;
(c) quaternary oxides of type AwBxCyOz, where A, B and C are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and w, x, y and z are stoichiometric coefficients;
(d) binary halides of type AxBy, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, B is a halogen and x and y are stoichiometric coefficients;
(e) ternary halides of type AxByCz, where A and B are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, C is a halogen and x, y and z are stoichiometric coefficients;
(f) quaternary halides of type AwBxCyDz, where A, B and C are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, D is a halogen and w, x, y and z are stoichiometric coefficients;
(g) binary nitrides of type AxNy, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x and y are stoichiometric coefficients;
(h) ternary nitrides of type AxByNz, where A and B are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x, y and z are stoichiometric coefficients;
(i) quaternary nitrides of type AwBxCyNz, where A, B and C are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and w, x, y and z are stoichiometric coefficients;
(j) binary chalcogenides of type AxBy, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, B is a chalcogen and x and y are stoichiometric coefficients;
(k) ternary chalcogenides of type AxByCz, where A and B are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, C is a chalcogen and x, y and z are stoichiometric coefficients;
(l) quaternary chalcogenides of type AwBxCyDz, where A, B and C are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, D is a chalcogen and w, x, y and z are stoichiometric coefficients;
(m) binary carbides of type AxCy, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x and y are stoichiometric coefficients;
(n) binary oxyhalides of type AxByOz, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid, B is a halogen and x, y and z are stoichiometric coefficients;
(o) binary arsenides of type AxAsy, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x and y is a stoichiometric coefficient;
(p) ternary arsenides of type AxByAsz, where A and B are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x, y and z are stoichiometric coefficients;
(q) quaternary arsenides of type AwBxCyAsz, where A, B and C are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and w, x, y and z are stoichiometric coefficients;
(r) binary phosphates of type Ax(PO4)y, where A is an alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x and y are stoichiometric coefficients;
(s) ternary phosphates of type AxBy(PO4)z, where A and B are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and x, y and z are stoichiometric coefficients; and
(t) quaternary phosphates of type AwBxCy(PO4)z, where A, B and C are any combination of alkali metal, alkali-earth metal, transition metal, semimetal or metalloid and w, x, y and z are stoichiometric coefficients.