Patent
US 9,284,193Method for Preparing Graphene Oxide Films and Fibers
Rodolfo Cruz-Silva
US
Copyright © 2026 Matter42. All rights reserved.
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US 9,284,193Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1). Of course, unless stated in the claims a step such as polishing is not mandatory to the overall film creation process. Dewetting of the film did not …
FIG. 2 is a picture of a large area graphene oxide film prepared in accordance with an example of the present disclosure. [0025]
FIG. 3 is an electron micrograph of a graphene oxide fiber prepared in accordance with an example of the present disclosure. [0026]
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 9 is a picture of a woven fabric made of composite graphene oxide fibers. [0032]
FIG. 10 is a conceptual scheme showing a machine for continuous production of graphene film in accordance with an embodiment of our method. As shown in the …
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing graphene oxide film, comprising: a) preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry; b) depositing the graphene oxide slurry on a surface; c) spreading the graphene oxide slurry on the low-friction surface by bar coating; and d) drying the graphene oxide slurry, thereby preparing graphene oxide film.
The method of claim 1, further comprising preparing graphene oxide by oxidation of graphite with at least one chemical selected from the group consisting of potassium permanganate, sodium permanganate, ammonia permanganate, potassium chromate, sodium chromate, potassium persulfate, sodium persulfate, ammonia persulfate, potassium nitrate, ammonia nitrate, sodium nitrate, sodium chlorate, potassium chlorate, and ammonium chlorate.
The method of claim 1, wherein the graphene oxide slurry is between 0.1 and 1.5% solids by weight, and has a pH between 1.0 and 5.0.
The method of claim 1, wherein the surface is a low-friction surface selected from the group consisting of polytetrafluoroethylene, fluorinated ethylene propylene copolymer (FEP), high density polyethylene (HDPE), perfluorinated alkoxy polymer resin (PFA), and fluorosilane treated glass.
The method of claim 1, wherein the solvent comprises at least one acid selected from the group consisting of sulfuric acid, phosphoric acid, nitric acid, perchloric acid, tr ichloroacetic acid, and dichloroacetic acid.
The method of claim 1, wherein the slurry comprises a plasticizer.
A method for preparing a dual-layer graphene-oxide film, comprising: a) preparing a graphene oxide film according to the method of claim 1; and 16 b) applying a second layer to the graphene oxide film, wherein the second layer is selected from the group consisting of carbon nanotubes, graphene nanoplatelets, molybdenum disulfide, tungsten disulfide, polymer nanofiber, carbon fibers, and metallic nanowires.
A method for preparing a graphene oxide fiber, comprising: a) preparing a graphene oxide film according to the method of claim 1; b) cutting the graphene oxide film into strips; and c) dry-spinning the graphene oxide film strips into a fiber.
A supported graphene oxide film, comprising: a graphene oxide film, said graphene oxide film bound to a support.
The film of claim 15, wherein said support is consisting of paper, polymer fiber non-woven mat, nanotube paper, and carbon fiber.
The film of claim 15, wherein said support is consisting of metallic foil and polymer film. 18 a textile support selected from the group cellulose nanofiber paper, non-woven carbon a non-textile support selected from the group
Layer stacks claimed or described, ordered top of device to substrate.
dual-layer graphene oxide film
supported graphene oxide film
Materials described outside the worked examples.
graphene oxide
graphite oxide
graphite
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elongation to break (GO film, bar-coated) | 6 % | graphene oxide |
Young's modulus (GO film, bar-coated, 6% strain embodiment) |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,284,193Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1). Of course, unless stated in the claims a step such as polishing is not mandatory to the overall film creation process. Dewetting of the film did not …
FIG. 2 is a picture of a large area graphene oxide film prepared in accordance with an example of the present disclosure. [0025]
FIG. 3 is an electron micrograph of a graphene oxide fiber prepared in accordance with an example of the present disclosure. [0026]
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 9 is a picture of a woven fabric made of composite graphene oxide fibers. [0032]
FIG. 10 is a conceptual scheme showing a machine for continuous production of graphene film in accordance with an embodiment of our method. As shown in the …
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing graphene oxide film, comprising: a) preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry; b) depositing the graphene oxide slurry on a surface; c) spreading the graphene oxide slurry on the low-friction surface by bar coating; and d) drying the graphene oxide slurry, thereby preparing graphene oxide film.
The method of claim 1, further comprising preparing graphene oxide by oxidation of graphite with at least one chemical selected from the group consisting of potassium permanganate, sodium permanganate, ammonia permanganate, potassium chromate, sodium chromate, potassium persulfate, sodium persulfate, ammonia persulfate, potassium nitrate, ammonia nitrate, sodium nitrate, sodium chlorate, potassium chlorate, and ammonium chlorate.
The method of claim 1, wherein the graphene oxide slurry is between 0.1 and 1.5% solids by weight, and has a pH between 1.0 and 5.0.
The method of claim 1, wherein the surface is a low-friction surface selected from the group consisting of polytetrafluoroethylene, fluorinated ethylene propylene copolymer (FEP), high density polyethylene (HDPE), perfluorinated alkoxy polymer resin (PFA), and fluorosilane treated glass.
The method of claim 1, wherein the solvent comprises at least one acid selected from the group consisting of sulfuric acid, phosphoric acid, nitric acid, perchloric acid, tr ichloroacetic acid, and dichloroacetic acid.
The method of claim 1, wherein the slurry comprises a plasticizer.
A method for preparing a dual-layer graphene-oxide film, comprising: a) preparing a graphene oxide film according to the method of claim 1; and 16 b) applying a second layer to the graphene oxide film, wherein the second layer is selected from the group consisting of carbon nanotubes, graphene nanoplatelets, molybdenum disulfide, tungsten disulfide, polymer nanofiber, carbon fibers, and metallic nanowires.
A method for preparing a graphene oxide fiber, comprising: a) preparing a graphene oxide film according to the method of claim 1; b) cutting the graphene oxide film into strips; and c) dry-spinning the graphene oxide film strips into a fiber.
A supported graphene oxide film, comprising: a graphene oxide film, said graphene oxide film bound to a support.
The film of claim 15, wherein said support is consisting of paper, polymer fiber non-woven mat, nanotube paper, and carbon fiber.
The film of claim 15, wherein said support is consisting of metallic foil and polymer film. 18 a textile support selected from the group cellulose nanofiber paper, non-woven carbon a non-textile support selected from the group
Layer stacks claimed or described, ordered top of device to substrate.
dual-layer graphene oxide film
supported graphene oxide film
Materials described outside the worked examples.
graphene oxide
graphite oxide
graphite
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elongation to break (GO film, bar-coated) | 6 % | graphene oxide |
Young's modulus (GO film, bar-coated, 6% strain embodiment) |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,284,193Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1). Of course, unless stated in the claims a step such as polishing is not mandatory to the overall film creation process. Dewetting of the film did not …
FIG. 2 is a picture of a large area graphene oxide film prepared in accordance with an example of the present disclosure. [0025]
FIG. 3 is an electron micrograph of a graphene oxide fiber prepared in accordance with an example of the present disclosure. [0026]
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 9 is a picture of a woven fabric made of composite graphene oxide fibers. [0032]
FIG. 10 is a conceptual scheme showing a machine for continuous production of graphene film in accordance with an embodiment of our method. As shown in the …
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing graphene oxide film, comprising: a) preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry; b) depositing the graphene oxide slurry on a surface; c) spreading the graphene oxide slurry on the low-friction surface by bar coating; and d) drying the graphene oxide slurry, thereby preparing graphene oxide film.
The method of claim 1, further comprising preparing graphene oxide by oxidation of graphite with at least one chemical selected from the group consisting of potassium permanganate, sodium permanganate, ammonia permanganate, potassium chromate, sodium chromate, potassium persulfate, sodium persulfate, ammonia persulfate, potassium nitrate, ammonia nitrate, sodium nitrate, sodium chlorate, potassium chlorate, and ammonium chlorate.
The method of claim 1, wherein the graphene oxide slurry is between 0.1 and 1.5% solids by weight, and has a pH between 1.0 and 5.0.
The method of claim 1, wherein the surface is a low-friction surface selected from the group consisting of polytetrafluoroethylene, fluorinated ethylene propylene copolymer (FEP), high density polyethylene (HDPE), perfluorinated alkoxy polymer resin (PFA), and fluorosilane treated glass.
The method of claim 1, wherein the solvent comprises at least one acid selected from the group consisting of sulfuric acid, phosphoric acid, nitric acid, perchloric acid, tr ichloroacetic acid, and dichloroacetic acid.
The method of claim 1, wherein the slurry comprises a plasticizer.
A method for preparing a dual-layer graphene-oxide film, comprising: a) preparing a graphene oxide film according to the method of claim 1; and 16 b) applying a second layer to the graphene oxide film, wherein the second layer is selected from the group consisting of carbon nanotubes, graphene nanoplatelets, molybdenum disulfide, tungsten disulfide, polymer nanofiber, carbon fibers, and metallic nanowires.
A method for preparing a graphene oxide fiber, comprising: a) preparing a graphene oxide film according to the method of claim 1; b) cutting the graphene oxide film into strips; and c) dry-spinning the graphene oxide film strips into a fiber.
A supported graphene oxide film, comprising: a graphene oxide film, said graphene oxide film bound to a support.
The film of claim 15, wherein said support is consisting of paper, polymer fiber non-woven mat, nanotube paper, and carbon fiber.
The film of claim 15, wherein said support is consisting of metallic foil and polymer film. 18 a textile support selected from the group cellulose nanofiber paper, non-woven carbon a non-textile support selected from the group
Layer stacks claimed or described, ordered top of device to substrate.
dual-layer graphene oxide film
supported graphene oxide film
Materials described outside the worked examples.
graphene oxide
graphite oxide
graphite
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elongation to break (GO film, bar-coated) | 6 % | graphene oxide |
Young's modulus (GO film, bar-coated, 6% strain embodiment) |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,284,193Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1). Of course, unless stated in the claims a step such as polishing is not mandatory to the overall film creation process. Dewetting of the film did not …
FIG. 2 is a picture of a large area graphene oxide film prepared in accordance with an example of the present disclosure. [0025]
FIG. 3 is an electron micrograph of a graphene oxide fiber prepared in accordance with an example of the present disclosure. [0026]
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 9 is a picture of a woven fabric made of composite graphene oxide fibers. [0032]
FIG. 10 is a conceptual scheme showing a machine for continuous production of graphene film in accordance with an embodiment of our method. As shown in the …
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing graphene oxide film, comprising: a) preparing a graphene oxide gel slurry by concentration of a graphite oxide aqueous slurry; b) depositing the graphene oxide slurry on a surface; c) spreading the graphene oxide slurry on the low-friction surface by bar coating; and d) drying the graphene oxide slurry, thereby preparing graphene oxide film.
The method of claim 1, further comprising preparing graphene oxide by oxidation of graphite with at least one chemical selected from the group consisting of potassium permanganate, sodium permanganate, ammonia permanganate, potassium chromate, sodium chromate, potassium persulfate, sodium persulfate, ammonia persulfate, potassium nitrate, ammonia nitrate, sodium nitrate, sodium chlorate, potassium chlorate, and ammonium chlorate.
The method of claim 1, wherein the graphene oxide slurry is between 0.1 and 1.5% solids by weight, and has a pH between 1.0 and 5.0.
The method of claim 1, wherein the surface is a low-friction surface selected from the group consisting of polytetrafluoroethylene, fluorinated ethylene propylene copolymer (FEP), high density polyethylene (HDPE), perfluorinated alkoxy polymer resin (PFA), and fluorosilane treated glass.
The method of claim 1, wherein the solvent comprises at least one acid selected from the group consisting of sulfuric acid, phosphoric acid, nitric acid, perchloric acid, tr ichloroacetic acid, and dichloroacetic acid.
The method of claim 1, wherein the slurry comprises a plasticizer.
A method for preparing a dual-layer graphene-oxide film, comprising: a) preparing a graphene oxide film according to the method of claim 1; and 16 b) applying a second layer to the graphene oxide film, wherein the second layer is selected from the group consisting of carbon nanotubes, graphene nanoplatelets, molybdenum disulfide, tungsten disulfide, polymer nanofiber, carbon fibers, and metallic nanowires.
A method for preparing a graphene oxide fiber, comprising: a) preparing a graphene oxide film according to the method of claim 1; b) cutting the graphene oxide film into strips; and c) dry-spinning the graphene oxide film strips into a fiber.
A supported graphene oxide film, comprising: a graphene oxide film, said graphene oxide film bound to a support.
The film of claim 15, wherein said support is consisting of paper, polymer fiber non-woven mat, nanotube paper, and carbon fiber.
The film of claim 15, wherein said support is consisting of metallic foil and polymer film. 18 a textile support selected from the group cellulose nanofiber paper, non-woven carbon a non-textile support selected from the group
Layer stacks claimed or described, ordered top of device to substrate.
dual-layer graphene oxide film
supported graphene oxide film
Materials described outside the worked examples.
graphene oxide
graphite oxide
graphite
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 4B are an SEM picture of a graphene oxide/double walled carbon nanotubes composite fiber prepared in accordance with an example of the present disclosure.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elongation to break (GO film, bar-coated) | 6 % | graphene oxide |
Young's modulus (GO film, bar-coated, 6% strain embodiment) |
Related documents with shared materials, methods, properties, or citations.
carbon nanotubes
molybdenum disulfide
MoS₂
tungsten disulfide
WS₂
graphene nanoplatelets
reduced graphene oxide
sulfuric acid
H₂SO₄
polytetrafluoroethylene (PTFE)
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
| 5.7 GPa |
graphene oxide |
elongation to break (GO film, thickness-controlled) | 10 % | graphene oxide |
Young's modulus (GO film, thickness-controlled, 10% strain embodiment) | 7 GPa | graphene oxide |
Duration | 5–10 minutes | — |
Duration | 600–86400 s | — |
Duration | 10–24 hours | — |
carbon nanotubes
molybdenum disulfide
MoS₂
tungsten disulfide
WS₂
graphene nanoplatelets
reduced graphene oxide
sulfuric acid
H₂SO₄
polytetrafluoroethylene (PTFE)
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
| 5.7 GPa |
graphene oxide |
elongation to break (GO film, thickness-controlled) | 10 % | graphene oxide |
Young's modulus (GO film, thickness-controlled, 10% strain embodiment) | 7 GPa | graphene oxide |
Duration | 5–10 minutes | — |
Duration | 600–86400 s | — |
Duration | 10–24 hours | — |
carbon nanotubes
molybdenum disulfide
MoS₂
tungsten disulfide
WS₂
graphene nanoplatelets
reduced graphene oxide
sulfuric acid
H₂SO₄
polytetrafluoroethylene (PTFE)
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
| 5.7 GPa |
graphene oxide |
elongation to break (GO film, thickness-controlled) | 10 % | graphene oxide |
Young's modulus (GO film, thickness-controlled, 10% strain embodiment) | 7 GPa | graphene oxide |
Duration | 5–10 minutes | — |
Duration | 600–86400 s | — |
Duration | 10–24 hours | — |
carbon nanotubes
molybdenum disulfide
MoS₂
tungsten disulfide
WS₂
graphene nanoplatelets
reduced graphene oxide
sulfuric acid
H₂SO₄
polytetrafluoroethylene (PTFE)
FIG. 5 B shows the low magnification image of the GO/W S₂ composite fiber prepared in accordance with an example of the present disclosure. [0028]
FIG. 6 is a SEM picture of a homochiral two-ply graphene oxide yarn, prepared in accordance with an example of the present disclosure. [0029]
FIG. 7B are SEM pictures of a graphene oxide fiber reduced with hydrazine in vapor in accordance with an example of the present disclosure.
FIG. 8D are SEM pictures of a graphene oxide fiber reduced with different temperature treatments.
FIG. 11 is an application of an electrically conductive graphene fiber as field emitter. The inset shows the fiber used as field emitter while the plot shows its …
FIG. 12A shows a conceptual diagram of a machine to continuously prepare textile or film supported graphene oxide film. This differs from
| 5.7 GPa |
graphene oxide |
elongation to break (GO film, thickness-controlled) | 10 % | graphene oxide |
Young's modulus (GO film, thickness-controlled, 10% strain embodiment) | 7 GPa | graphene oxide |
Duration | 5–10 minutes | — |
Duration | 600–86400 s | — |
Duration | 10–24 hours | — |