Patent
US 8,747,623ONE-STEP PRODUCTION OF GRAPHENE MATERIALS
Aruna Zhamu
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 8,747,623Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing highly 30 oxidized NGPs that entails tedious chemical oxidation/intercalation, …
FIG.2 Flowcharts for the comparison of the presently invented one-step process (A) and the conventional, multi-step process of producing graphene materials.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
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 of producing exfoliated graphite or graphene directly from a non- intercalated and non-oxidized graphitic material, said method comprising: a) dispersing said graphitic material in a liquid intercalating agent to form a suspension, wherein said graphitic material has never been previously exposed to chemical intercalation or oxidation; and b) subjecting said suspension to microwave or radio frequency irradiation with a frequency and an intensity for a length of time sufficient for producing said exfoliated graphite or graphene.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is not a mixture of an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is sulfuric acid alone.
The method of claim 1, wherein said liquid intercalating agent is nitric acid alone.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 90% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 50% by weight in water
The method of claim 1, wherein said liquid intercalating agent contains a weak acid selected from formic acid, acetic acid, nitric acid, or ca r boxylic acid.
The method of claim 1, wherein said liquid intercalating agent is a mixture containing an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is a mixture 2 containing an acid and an oxidizing agent dissolved in water wherein said acid or said oxidizing agent has a concentration of less than 50% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a ca r boxylic acid.
The method of claim 1 wherein said intercalating agent is a carboxylic acid selected from the group consisting of a r omatic ca r boxylic acid, aliphatic or cycloaliphatic car boxylic acid, straight chain or branched chain ca r boxylic acid, saturated and unsaturated monoca r boxylic acids, dica r boxylic acids and polyca r boxylic acids that have 1-10 ca r bon atoms, alkyl esters thereof, and combinations thereof.
The method of claim 1 wherein said intercalating agent is a ca r boxylic acid and wherein said suspension further comprises hydrogen peroxide as an oxidizing agent.
The method of claim 1 wherein said intercalating agent contains a carboxylic acid and an oxidizing agent.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 5 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 2 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 1 minute.
The method of claim 1, further comprising a step of subjecting said exfoliated graphite to a mechanical shearing treatment to produce a graphene material.
The method of claim 1, further comprising a step of compressing said exfoliated graphite or graphene to form a flexible graphite product.
The method of claim 1 wherein said graphitic material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano- fiber, graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphitic material is selected from highly oriented pyrolytic graphite, meso-ca r bon micro-bead, graphite fiber, graphitic nano-fiber, gaphite-eide; graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphene contains single-layer graphene sheets.
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets.
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a ca r bon content no less than 95% by weight, or functionalized graphene.
A method of producing a graphene material, said method comprising directly exposing a nonintercalated and non-oxidized graphitic material to microwave irradiation in the presence of a liquid intercalating agent, wherein said graphitic material has never been previously exposed to a chemical or oxidation treatment prior to said microwave irradiation step and said microwave has a frequency and an intensity sufficient for producing a single- layer graphene sheet.
The method of claim 27, wherein said intercalating agent is an acid or an oxidizer, but not a mixture of an acid and an oxidizer.
The method of claim 27, wherein said intercalating agent does not contain sulfuric acid or nitric acid. 4
Materials described outside the worked examples.
graphitic material (non-intercalated, non-oxidized)
graphene
Measurements and analyses referenced in the patent, with their drawing references.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | ≤ 5 minutes | — |
Duration | ≤ 2 minutes |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,747,623Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing highly 30 oxidized NGPs that entails tedious chemical oxidation/intercalation, …
FIG.2 Flowcharts for the comparison of the presently invented one-step process (A) and the conventional, multi-step process of producing graphene materials.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
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 of producing exfoliated graphite or graphene directly from a non- intercalated and non-oxidized graphitic material, said method comprising: a) dispersing said graphitic material in a liquid intercalating agent to form a suspension, wherein said graphitic material has never been previously exposed to chemical intercalation or oxidation; and b) subjecting said suspension to microwave or radio frequency irradiation with a frequency and an intensity for a length of time sufficient for producing said exfoliated graphite or graphene.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is not a mixture of an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is sulfuric acid alone.
The method of claim 1, wherein said liquid intercalating agent is nitric acid alone.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 90% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 50% by weight in water
The method of claim 1, wherein said liquid intercalating agent contains a weak acid selected from formic acid, acetic acid, nitric acid, or ca r boxylic acid.
The method of claim 1, wherein said liquid intercalating agent is a mixture containing an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is a mixture 2 containing an acid and an oxidizing agent dissolved in water wherein said acid or said oxidizing agent has a concentration of less than 50% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a ca r boxylic acid.
The method of claim 1 wherein said intercalating agent is a carboxylic acid selected from the group consisting of a r omatic ca r boxylic acid, aliphatic or cycloaliphatic car boxylic acid, straight chain or branched chain ca r boxylic acid, saturated and unsaturated monoca r boxylic acids, dica r boxylic acids and polyca r boxylic acids that have 1-10 ca r bon atoms, alkyl esters thereof, and combinations thereof.
The method of claim 1 wherein said intercalating agent is a ca r boxylic acid and wherein said suspension further comprises hydrogen peroxide as an oxidizing agent.
The method of claim 1 wherein said intercalating agent contains a carboxylic acid and an oxidizing agent.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 5 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 2 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 1 minute.
The method of claim 1, further comprising a step of subjecting said exfoliated graphite to a mechanical shearing treatment to produce a graphene material.
The method of claim 1, further comprising a step of compressing said exfoliated graphite or graphene to form a flexible graphite product.
The method of claim 1 wherein said graphitic material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano- fiber, graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphitic material is selected from highly oriented pyrolytic graphite, meso-ca r bon micro-bead, graphite fiber, graphitic nano-fiber, gaphite-eide; graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphene contains single-layer graphene sheets.
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets.
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a ca r bon content no less than 95% by weight, or functionalized graphene.
A method of producing a graphene material, said method comprising directly exposing a nonintercalated and non-oxidized graphitic material to microwave irradiation in the presence of a liquid intercalating agent, wherein said graphitic material has never been previously exposed to a chemical or oxidation treatment prior to said microwave irradiation step and said microwave has a frequency and an intensity sufficient for producing a single- layer graphene sheet.
The method of claim 27, wherein said intercalating agent is an acid or an oxidizer, but not a mixture of an acid and an oxidizer.
The method of claim 27, wherein said intercalating agent does not contain sulfuric acid or nitric acid. 4
Materials described outside the worked examples.
graphitic material (non-intercalated, non-oxidized)
graphene
Measurements and analyses referenced in the patent, with their drawing references.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | ≤ 5 minutes | — |
Duration | ≤ 2 minutes |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,747,623Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing highly 30 oxidized NGPs that entails tedious chemical oxidation/intercalation, …
FIG.2 Flowcharts for the comparison of the presently invented one-step process (A) and the conventional, multi-step process of producing graphene materials.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
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 of producing exfoliated graphite or graphene directly from a non- intercalated and non-oxidized graphitic material, said method comprising: a) dispersing said graphitic material in a liquid intercalating agent to form a suspension, wherein said graphitic material has never been previously exposed to chemical intercalation or oxidation; and b) subjecting said suspension to microwave or radio frequency irradiation with a frequency and an intensity for a length of time sufficient for producing said exfoliated graphite or graphene.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is not a mixture of an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is sulfuric acid alone.
The method of claim 1, wherein said liquid intercalating agent is nitric acid alone.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 90% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 50% by weight in water
The method of claim 1, wherein said liquid intercalating agent contains a weak acid selected from formic acid, acetic acid, nitric acid, or ca r boxylic acid.
The method of claim 1, wherein said liquid intercalating agent is a mixture containing an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is a mixture 2 containing an acid and an oxidizing agent dissolved in water wherein said acid or said oxidizing agent has a concentration of less than 50% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a ca r boxylic acid.
The method of claim 1 wherein said intercalating agent is a carboxylic acid selected from the group consisting of a r omatic ca r boxylic acid, aliphatic or cycloaliphatic car boxylic acid, straight chain or branched chain ca r boxylic acid, saturated and unsaturated monoca r boxylic acids, dica r boxylic acids and polyca r boxylic acids that have 1-10 ca r bon atoms, alkyl esters thereof, and combinations thereof.
The method of claim 1 wherein said intercalating agent is a ca r boxylic acid and wherein said suspension further comprises hydrogen peroxide as an oxidizing agent.
The method of claim 1 wherein said intercalating agent contains a carboxylic acid and an oxidizing agent.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 5 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 2 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 1 minute.
The method of claim 1, further comprising a step of subjecting said exfoliated graphite to a mechanical shearing treatment to produce a graphene material.
The method of claim 1, further comprising a step of compressing said exfoliated graphite or graphene to form a flexible graphite product.
The method of claim 1 wherein said graphitic material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano- fiber, graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphitic material is selected from highly oriented pyrolytic graphite, meso-ca r bon micro-bead, graphite fiber, graphitic nano-fiber, gaphite-eide; graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphene contains single-layer graphene sheets.
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets.
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a ca r bon content no less than 95% by weight, or functionalized graphene.
A method of producing a graphene material, said method comprising directly exposing a nonintercalated and non-oxidized graphitic material to microwave irradiation in the presence of a liquid intercalating agent, wherein said graphitic material has never been previously exposed to a chemical or oxidation treatment prior to said microwave irradiation step and said microwave has a frequency and an intensity sufficient for producing a single- layer graphene sheet.
The method of claim 27, wherein said intercalating agent is an acid or an oxidizer, but not a mixture of an acid and an oxidizer.
The method of claim 27, wherein said intercalating agent does not contain sulfuric acid or nitric acid. 4
Materials described outside the worked examples.
graphitic material (non-intercalated, non-oxidized)
graphene
Measurements and analyses referenced in the patent, with their drawing references.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | ≤ 5 minutes | — |
Duration | ≤ 2 minutes |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,747,623Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing highly 30 oxidized NGPs that entails tedious chemical oxidation/intercalation, …
FIG.2 Flowcharts for the comparison of the presently invented one-step process (A) and the conventional, multi-step process of producing graphene materials.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
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 of producing exfoliated graphite or graphene directly from a non- intercalated and non-oxidized graphitic material, said method comprising: a) dispersing said graphitic material in a liquid intercalating agent to form a suspension, wherein said graphitic material has never been previously exposed to chemical intercalation or oxidation; and b) subjecting said suspension to microwave or radio frequency irradiation with a frequency and an intensity for a length of time sufficient for producing said exfoliated graphite or graphene.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is not a mixture of an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is sulfuric acid alone.
The method of claim 1, wherein said liquid intercalating agent is nitric acid alone.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 90% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a mixture of sulfuric acid and nitric acid each with a concentration less than 50% by weight in water
The method of claim 1, wherein said liquid intercalating agent contains a weak acid selected from formic acid, acetic acid, nitric acid, or ca r boxylic acid.
The method of claim 1, wherein said liquid intercalating agent is a mixture containing an acid and an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent has a single component only and is an oxidizing agent.
The method of claim 1, wherein said liquid intercalating agent is a mixture 2 containing an acid and an oxidizing agent dissolved in water wherein said acid or said oxidizing agent has a concentration of less than 50% by weight in water.
The method of claim 1, wherein said liquid intercalating agent is a ca r boxylic acid.
The method of claim 1 wherein said intercalating agent is a carboxylic acid selected from the group consisting of a r omatic ca r boxylic acid, aliphatic or cycloaliphatic car boxylic acid, straight chain or branched chain ca r boxylic acid, saturated and unsaturated monoca r boxylic acids, dica r boxylic acids and polyca r boxylic acids that have 1-10 ca r bon atoms, alkyl esters thereof, and combinations thereof.
The method of claim 1 wherein said intercalating agent is a ca r boxylic acid and wherein said suspension further comprises hydrogen peroxide as an oxidizing agent.
The method of claim 1 wherein said intercalating agent contains a carboxylic acid and an oxidizing agent.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 5 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 2 minutes.
The method of claim 1 wherein said microwave or radio frequency irradiation time is less than 1 minute.
The method of claim 1, further comprising a step of subjecting said exfoliated graphite to a mechanical shearing treatment to produce a graphene material.
The method of claim 1, further comprising a step of compressing said exfoliated graphite or graphene to form a flexible graphite product.
The method of claim 1 wherein said graphitic material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano- fiber, graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphitic material is selected from highly oriented pyrolytic graphite, meso-ca r bon micro-bead, graphite fiber, graphitic nano-fiber, gaphite-eide; graphite fluoride, chemically modified graphite, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said graphene contains single-layer graphene sheets.
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets.
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a ca r bon content no less than 95% by weight, or functionalized graphene.
A method of producing a graphene material, said method comprising directly exposing a nonintercalated and non-oxidized graphitic material to microwave irradiation in the presence of a liquid intercalating agent, wherein said graphitic material has never been previously exposed to a chemical or oxidation treatment prior to said microwave irradiation step and said microwave has a frequency and an intensity sufficient for producing a single- layer graphene sheet.
The method of claim 27, wherein said intercalating agent is an acid or an oxidizer, but not a mixture of an acid and an oxidizer.
The method of claim 27, wherein said intercalating agent does not contain sulfuric acid or nitric acid. 4
Materials described outside the worked examples.
graphitic material (non-intercalated, non-oxidized)
graphene
Measurements and analyses referenced in the patent, with their drawing references.
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | ≤ 5 minutes | — |
Duration | ≤ 2 minutes |
Related documents with shared materials, methods, properties, or citations.
liquid intercalating agent
sulfuric acid
H₂SO₄
nitric acid
HNO₃
carboxylic acid
hydrogen peroxide
H₂O₂
graphene fluoride
functionalized graphene
exfoliated graphite
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
| — |
Duration | ≤ 1 minute | — |
liquid intercalating agent
sulfuric acid
H₂SO₄
nitric acid
HNO₃
carboxylic acid
hydrogen peroxide
H₂O₂
graphene fluoride
functionalized graphene
exfoliated graphite
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
| — |
Duration | ≤ 1 minute | — |
liquid intercalating agent
sulfuric acid
H₂SO₄
nitric acid
HNO₃
carboxylic acid
hydrogen peroxide
H₂O₂
graphene fluoride
functionalized graphene
exfoliated graphite
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
| — |
Duration | ≤ 1 minute | — |
liquid intercalating agent
sulfuric acid
H₂SO₄
nitric acid
HNO₃
carboxylic acid
hydrogen peroxide
H₂O₂
graphene fluoride
functionalized graphene
exfoliated graphite
FIG.3 Transmission electron micrographs of (A) NGPs produced by the direct microwave 5 irradiation process (wider and longer graphene sheets) and (B) NGPs …
| — |
Duration | ≤ 1 minute | — |