# US 11,299,645 B2 · Methods and applications for conductive graphene inks

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- Number: US 11,299,645 B2
- Document ID: US11299645B2
- Status: Granted
- Kind: B2
- Application number: 15/956,356
- Filed: 2018-04-18
- Published: 2018-10-25
- Granted: 2022-04-12
- Earliest claimed: 2017-04-21
- Assignees: The Regents of the University of California; Nanotech Energy, Inc.
- Applicants: The Regents of the University of California; Nanotech Energy, Inc.
- Inventors: Maher F. El-Kady; Nahla Mohamed; Jack Kavanaugh; Richard B. Kaner
- Web page: https://patentgrep.com/patent/US11299645B2

## CPC

- C09D 11/52: Electrically conductive inks
- C09D 11/037: characterised by the pigment
- C09D 11/08: based on natural resins
- C09D 11/102: containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D 11/106: containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D 11/324: containing carbon black
- C09D 11/38: characterised by non-macromolecular additives other than solvents, pigments or dyes
- C08K 3/042: {Graphene or derivatives, e.g. graphene oxides}
- C08K 2201/001: Conductive additives
- H05K 1/095: {for polymer thick films, i.e. having a permanent organic polymeric binder}
- H05K 2201/026: Nanotubes or nanowires
- H05K 2201/0323: Carbon
- Y02E 60/13: Energy storage using capacitors
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- H05K: PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

The present disclosure provides for an exemplary energy storage device and methods of forming thereof, comprising an exemplary conductive graphene ink on exemplary substrates to form durable, flexible, and facile graphene films and energy storage devices for use with and within a variety of electronics and devices.

## Claims

### Claim 1

A conductive graphene ink comprising:
a) 20% to about 70% by mass of a binder solution comprising a binder and a first solvent; and
b) a reduced graphene oxide dispersion comprising reduced graphene oxide, and a second solvent;
wherein the conductive graphene ink has a viscosity of at least about 1,000 centipoise.

### Claim 2 (depends on 1)

The conductive graphene ink of claim 1, wherein at least one of the first solvent and the second solvent comprises water, ethanol, isopropyl alcohol, N-methyl-2-pyrrolidone, cyclohexanone, terpineol, 3-methoxy-3-methyl-1-butanol, 4-hydroxyl-4-methyl-pentan-2-one, methyl isobutyl ketone, or any combination thereof.

### Claim 3 (depends on 1)

The conductive graphene ink of claim 1, wherein the binder comprises carboxymethyl cellulose, polyvinylidene fluoride, poly(vinyl alcohol), poly(vinyl pyrrolidone), poly(ethylene oxide), ethyl cellulose, or any combination thereof.

### Claim 4 (depends on 1)

The conductive graphene ink of claim 1, wherein the conductive graphene ink has a viscosity of at most about 10,000 centipoise.

### Claim 5 (depends on 1)

The conductive graphene ink of claim 1, wherein the conductive graphene ink has a C:O mass ratio of about 2:1 to about 40:1.

### Claim 6

A method of forming a conductive graphene ink comprising:
forming a binder solution comprising:
heating a first solvent;
adding a binder to the first solvent;
mixing the binder and the first solvent; and
cooling the binder and the first solvent;
forming a reduced graphene oxide dispersion comprising a second solvent and reduced graphene oxide;
forming a graphene solution comprising the binder solution and the reduced graphene oxide dispersion; and
mixing the graphene solution under a vacuum degree of about −0.05 MPa to about −0.2 MPa to form a conductive graphene ink.

### Claim 7 (depends on 6)

The method of claim 6, wherein at least one of the first solvent and the second solvent comprises water, ethanol, isopropyl alcohol, N-methyl-2-pyrrolidone, cyclohexanone, terpineol, 3-methoxy-3-methyl-1-butanol, 4-hydroxyl-4-methyl-pentan-2-one, methyl isobutyl ketone, or any combination thereof.

### Claim 8 (depends on 6)

The method of claim 6, wherein the binder comprises carboxymethyl cellulose, polyvinylidene fluoride, poly(vinyl alcohol), poly(vinyl pyrrolidone), poly(ethylene oxide), ethyl cellulose, or any combination thereof.

### Claim 9 (depends on 6)

The method of claim 6, wherein the first solvent is heated to a temperature of about 35° C. to about 125° C.

### Claim 10 (depends on 6)

The method of claim 6, wherein the binder is added to the first solvent during the mixing of the binder and the first solvent, over a period of time of about 45 minutes to about 240 minutes.

### Claim 11 (depends on 6)

The method of claim 6, wherein, after the binder is fully added to the first solvent, the binder and the first solvent are mixed for a period of time of about 7 minutes to about 30 minutes.

### Claim 12 (depends on 6)

The method of claim 6, wherein the mixing of the graphene solution is performed with at least one of a stirring speed of about 15 rpm to about 125 rpm, and a dispersing speed of about 50 rpm to about 4,500 rpm.

### Claim 13 (depends on 6)

The method of claim 6, wherein the graphene solution is mixed during one or more intervals, wherein each interval comprises a period of time of about 0.5 minutes to about 30 minutes.

### Claim 14 (depends on 6)

The method of claim 6, wherein the binder and the first solvent are cooled to a temperature of about 10° C. to about 40° C.