Patent
US 9,481,576ENVIRONMENTALLY BENIGN PRODUCTION OF GRAPHENE MATERIALS
Aruna Zhamu
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
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US 9,481,576Patent 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 oxidized NGPs that entails tedious chemical oxidation/intercalation …
FIG.2 Schematic of an electrochemical oxidation/intercalation apparatus.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
FIG.5 The oxidation completion time plotted as a function of the molar ratio between Li₂Fe O₄ and K 2FeO 4, for the series of acetic acid/oxidant-intercalated …
FIG.6 The oxidation completion time plotted as a function of the molar ratio between Na 2FeO₄ 15 and K₂Fe O 4, for the two series of malic acid/oxidant- and …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant or its component ions residing in at least one of said interstices, wherein said intercalant is sulfuric acid-free and comprises a carboxylic acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, LiXCoO 4, Na XCoO 4, K XCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and er a combinations thereof, where x is from 1 to 2.
The intercalated graphite compound of claim 1 wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and or a combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of aromatic carboxylic acid, aliphatic or cycloaliphatic carboxylic acid, straight chain or branched chain carboxylic acid, saturated and unsaturated monocarboxylic acids, dicarboxylic acids and polycarboxylic acids that have 1-10 carbon atoms, alkyl esters thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of saturated aliphatic carboxylic acids of the formula H(CH 2) nCOO H, wherein n is a number o f from 0 to 5, selected from formic, acetic, propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, reactive carboxylic acid derivatives thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein the intercalant consists of a mixture of a carboxylic acid and an oxidant at a weight ratio of 100:1 to 100:50.
The intercalated graphite compound of claim 1 wherein said intercalant further 2 comprises hydrogen peroxide.
The intercalated graphite compound of claim 1, which is prepared by an electrochemical reaction which uses said intercalant as both an electrolyte and an intercalate source.
The intercalated graphite compound of claim 1, wherein said intercalated compound is prepared by a chemical oxidation reaction which includes immersing said layered graphite in a liquid medium containing said intercalant.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 1, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant residing in at least one of said interstices, wherein said intercalant comprises sulfuric acid, and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li XCoO 4, Na XCo₀ 4, K XCo₀ 4, Li xNi₀ 4, Na xNi₀ 4, KxNi₀ 4, a combination thereof, and ef a combinations with K 2 FeO 4, where x is from 1 to 2, and said layered graphite material is selected from the group consisting of synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and er a combinations thereof.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 9, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical reaction process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 0 C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
A method of producing exfoliated graphite or separate sheets of a graphene material from an intercalated graphite compound, said method comprising: a) preparing said intercalated graphite compound from a layered graphite material using an electrochemical reaction process which uses an intercalant as both an electrolyte and an intercalate source, wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and eo a combinations thereof, and said intercalant contains an acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li xCoO 4, Na xCoO 4, K xCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and or a combinations thereof, where x is from 1 to 2; b) bringing said intercalated graphite compound into a dry powder form or a suspension containing said intercalated graphite compound dispersed in a fluid; and c) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or exposing said dry intercalated graphite compound powder to a heat treatment at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
The method of claim 19, wherein said acid is selected from sulfuric acid or a mixture of sulfuric acid and a carboxylic acid.
Materials described outside the worked examples.
intercalated graphite compound
carboxylic acid
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 1200–14400 s | — |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,481,576Patent 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 oxidized NGPs that entails tedious chemical oxidation/intercalation …
FIG.2 Schematic of an electrochemical oxidation/intercalation apparatus.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
FIG.5 The oxidation completion time plotted as a function of the molar ratio between Li₂Fe O₄ and K 2FeO 4, for the series of acetic acid/oxidant-intercalated …
FIG.6 The oxidation completion time plotted as a function of the molar ratio between Na 2FeO₄ 15 and K₂Fe O 4, for the two series of malic acid/oxidant- and …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant or its component ions residing in at least one of said interstices, wherein said intercalant is sulfuric acid-free and comprises a carboxylic acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, LiXCoO 4, Na XCoO 4, K XCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and er a combinations thereof, where x is from 1 to 2.
The intercalated graphite compound of claim 1 wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and or a combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of aromatic carboxylic acid, aliphatic or cycloaliphatic carboxylic acid, straight chain or branched chain carboxylic acid, saturated and unsaturated monocarboxylic acids, dicarboxylic acids and polycarboxylic acids that have 1-10 carbon atoms, alkyl esters thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of saturated aliphatic carboxylic acids of the formula H(CH 2) nCOO H, wherein n is a number o f from 0 to 5, selected from formic, acetic, propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, reactive carboxylic acid derivatives thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein the intercalant consists of a mixture of a carboxylic acid and an oxidant at a weight ratio of 100:1 to 100:50.
The intercalated graphite compound of claim 1 wherein said intercalant further 2 comprises hydrogen peroxide.
The intercalated graphite compound of claim 1, which is prepared by an electrochemical reaction which uses said intercalant as both an electrolyte and an intercalate source.
The intercalated graphite compound of claim 1, wherein said intercalated compound is prepared by a chemical oxidation reaction which includes immersing said layered graphite in a liquid medium containing said intercalant.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 1, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant residing in at least one of said interstices, wherein said intercalant comprises sulfuric acid, and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li XCoO 4, Na XCo₀ 4, K XCo₀ 4, Li xNi₀ 4, Na xNi₀ 4, KxNi₀ 4, a combination thereof, and ef a combinations with K 2 FeO 4, where x is from 1 to 2, and said layered graphite material is selected from the group consisting of synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and er a combinations thereof.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 9, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical reaction process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 0 C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
A method of producing exfoliated graphite or separate sheets of a graphene material from an intercalated graphite compound, said method comprising: a) preparing said intercalated graphite compound from a layered graphite material using an electrochemical reaction process which uses an intercalant as both an electrolyte and an intercalate source, wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and eo a combinations thereof, and said intercalant contains an acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li xCoO 4, Na xCoO 4, K xCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and or a combinations thereof, where x is from 1 to 2; b) bringing said intercalated graphite compound into a dry powder form or a suspension containing said intercalated graphite compound dispersed in a fluid; and c) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or exposing said dry intercalated graphite compound powder to a heat treatment at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
The method of claim 19, wherein said acid is selected from sulfuric acid or a mixture of sulfuric acid and a carboxylic acid.
Materials described outside the worked examples.
intercalated graphite compound
carboxylic acid
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 1200–14400 s | — |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,481,576Patent 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 oxidized NGPs that entails tedious chemical oxidation/intercalation …
FIG.2 Schematic of an electrochemical oxidation/intercalation apparatus.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
FIG.5 The oxidation completion time plotted as a function of the molar ratio between Li₂Fe O₄ and K 2FeO 4, for the series of acetic acid/oxidant-intercalated …
FIG.6 The oxidation completion time plotted as a function of the molar ratio between Na 2FeO₄ 15 and K₂Fe O 4, for the two series of malic acid/oxidant- and …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant or its component ions residing in at least one of said interstices, wherein said intercalant is sulfuric acid-free and comprises a carboxylic acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, LiXCoO 4, Na XCoO 4, K XCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and er a combinations thereof, where x is from 1 to 2.
The intercalated graphite compound of claim 1 wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and or a combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of aromatic carboxylic acid, aliphatic or cycloaliphatic carboxylic acid, straight chain or branched chain carboxylic acid, saturated and unsaturated monocarboxylic acids, dicarboxylic acids and polycarboxylic acids that have 1-10 carbon atoms, alkyl esters thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of saturated aliphatic carboxylic acids of the formula H(CH 2) nCOO H, wherein n is a number o f from 0 to 5, selected from formic, acetic, propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, reactive carboxylic acid derivatives thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein the intercalant consists of a mixture of a carboxylic acid and an oxidant at a weight ratio of 100:1 to 100:50.
The intercalated graphite compound of claim 1 wherein said intercalant further 2 comprises hydrogen peroxide.
The intercalated graphite compound of claim 1, which is prepared by an electrochemical reaction which uses said intercalant as both an electrolyte and an intercalate source.
The intercalated graphite compound of claim 1, wherein said intercalated compound is prepared by a chemical oxidation reaction which includes immersing said layered graphite in a liquid medium containing said intercalant.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 1, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant residing in at least one of said interstices, wherein said intercalant comprises sulfuric acid, and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li XCoO 4, Na XCo₀ 4, K XCo₀ 4, Li xNi₀ 4, Na xNi₀ 4, KxNi₀ 4, a combination thereof, and ef a combinations with K 2 FeO 4, where x is from 1 to 2, and said layered graphite material is selected from the group consisting of synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and er a combinations thereof.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 9, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical reaction process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 0 C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
A method of producing exfoliated graphite or separate sheets of a graphene material from an intercalated graphite compound, said method comprising: a) preparing said intercalated graphite compound from a layered graphite material using an electrochemical reaction process which uses an intercalant as both an electrolyte and an intercalate source, wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and eo a combinations thereof, and said intercalant contains an acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li xCoO 4, Na xCoO 4, K xCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and or a combinations thereof, where x is from 1 to 2; b) bringing said intercalated graphite compound into a dry powder form or a suspension containing said intercalated graphite compound dispersed in a fluid; and c) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or exposing said dry intercalated graphite compound powder to a heat treatment at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
The method of claim 19, wherein said acid is selected from sulfuric acid or a mixture of sulfuric acid and a carboxylic acid.
Materials described outside the worked examples.
intercalated graphite compound
carboxylic acid
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 1200–14400 s | — |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,481,576Patent 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 oxidized NGPs that entails tedious chemical oxidation/intercalation …
FIG.2 Schematic of an electrochemical oxidation/intercalation apparatus.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
FIG.5 The oxidation completion time plotted as a function of the molar ratio between Li₂Fe O₄ and K 2FeO 4, for the series of acetic acid/oxidant-intercalated …
FIG.6 The oxidation completion time plotted as a function of the molar ratio between Na 2FeO₄ 15 and K₂Fe O 4, for the two series of malic acid/oxidant- and …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant or its component ions residing in at least one of said interstices, wherein said intercalant is sulfuric acid-free and comprises a carboxylic acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, LiXCoO 4, Na XCoO 4, K XCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and er a combinations thereof, where x is from 1 to 2.
The intercalated graphite compound of claim 1 wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and or a combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of aromatic carboxylic acid, aliphatic or cycloaliphatic carboxylic acid, straight chain or branched chain carboxylic acid, saturated and unsaturated monocarboxylic acids, dicarboxylic acids and polycarboxylic acids that have 1-10 carbon atoms, alkyl esters thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein said carboxylic acid is selected from the group consisting of saturated aliphatic carboxylic acids of the formula H(CH 2) nCOO H, wherein n is a number o f from 0 to 5, selected from formic, acetic, propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, reactive carboxylic acid derivatives thereof, and combinations thereof.
The intercalated graphite compound of claim 1 wherein the intercalant consists of a mixture of a carboxylic acid and an oxidant at a weight ratio of 100:1 to 100:50.
The intercalated graphite compound of claim 1 wherein said intercalant further 2 comprises hydrogen peroxide.
The intercalated graphite compound of claim 1, which is prepared by an electrochemical reaction which uses said intercalant as both an electrolyte and an intercalate source.
The intercalated graphite compound of claim 1, wherein said intercalated compound is prepared by a chemical oxidation reaction which includes immersing said layered graphite in a liquid medium containing said intercalant.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 1, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
An intercalated graphite compound for the production of exfoliated graphite, flexible graphite, or nano graphene platelets, said compound comprising a layered graphite with interlayer spaces or interstices and an intercalant residing in at least one of said interstices, wherein said intercalant comprises sulfuric acid, and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li XCoO 4, Na XCo₀ 4, K XCo₀ 4, Li xNi₀ 4, Na xNi₀ 4, KxNi₀ 4, a combination thereof, and ef a combinations with K 2 FeO 4, where x is from 1 to 2, and said layered graphite material is selected from the group consisting of synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and er a combinations thereof.
A method of producing exfoliated graphite or separate sheets of a graphene material from the intercalated graphite compound of claim 9, said method comprising: a) preparing said intercalated graphite compound using a chemical oxidation process or electrochemical reaction process and making said intercalated graphite compound in a dry powder form or in a suspension containing said intercalated graphite compound dispersed in a fluid; and b) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or subjecting said dry intercalated graphite compound powder to a heat exposure at a temperature from 100 0 C to 1,500 0 C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
A method of producing exfoliated graphite or separate sheets of a graphene material from an intercalated graphite compound, said method comprising: a) preparing said intercalated graphite compound from a layered graphite material using an electrochemical reaction process which uses an intercalant as both an electrolyte and an intercalate source, wherein said layered graphite material is selected from the group consisting of natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, exfoliated graphite, expanded graphite, and eo a combinations thereof, and said intercalant contains an acid and an oxidant selected from the group consisting of Li 2 FeO 4, Na 2 FeO 4, Li xCoO 4, Na xCoO 4, K xCoO 4, Li xNiO 4, Na xNiO 4, K xNiO 4, and or a combinations thereof, where x is from 1 to 2; b) bringing said intercalated graphite compound into a dry powder form or a suspension containing said intercalated graphite compound dispersed in a fluid; and c) subjecting said suspension to an ultrasonication or mechanical shearing treatment with a desired sonication or shearing intensity for a length of time sufficient for producing said separate sheets of graphene, or exposing said dry intercalated graphite compound powder to a heat treatment at a temperature from 100 0 C to 1,500 ° C to produce said exfoliated graphite or, directly, said separate sheets of graphene.
The method of claim 19, wherein said acid is selected from sulfuric acid or a mixture of sulfuric acid and a carboxylic acid.
Materials described outside the worked examples.
intercalated graphite compound
carboxylic acid
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 (A) SEM image of a graphite worm (exfoliated graphite from intercalated compound of natural graphite) and (B) SEM image of graphite worms produced from …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 1200–14400 s | — |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Li₂FeO₄
Na₂FeO₄
LixCoO₄
NaxCoO₄
KxCoO₄
LixNiO₄
KxNiO₄
layered graphite
hydrogen peroxide
H₂O₂
sulfuric acid
H₂SO₄
K₂FeO₄
exfoliated graphite
graphene
NaxNiO₄
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
| — |
Duration | 1200–7200 s | — |
Duration | 45–70 minutes | — |
Duration | 5–120 hours | — |
Temperature | 800–1100 °C | — |
Temperature | 100–1500 °C | — |
Duration | 30–60 seconds | — |
Temperature | 100–1200 °C | — |
Duration | 6–96 hours | — |
Duration | 30–90 seconds | — |
Thickness | 0.85–0.93 nm | — |
Duration | 0.5–2 hours | — |
Duration | 0.5–1.2 hours | — |
Duration | 1–3 hours | — |
Duration | ≤ 1 hour | — |
Temperature | 600–1200 °C | — |
Temperature | 100–600 °C | — |
Li₂FeO₄
Na₂FeO₄
LixCoO₄
NaxCoO₄
KxCoO₄
LixNiO₄
KxNiO₄
layered graphite
hydrogen peroxide
H₂O₂
sulfuric acid
H₂SO₄
K₂FeO₄
exfoliated graphite
graphene
NaxNiO₄
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
| — |
Duration | 1200–7200 s | — |
Duration | 45–70 minutes | — |
Duration | 5–120 hours | — |
Temperature | 800–1100 °C | — |
Temperature | 100–1500 °C | — |
Duration | 30–60 seconds | — |
Temperature | 100–1200 °C | — |
Duration | 6–96 hours | — |
Duration | 30–90 seconds | — |
Thickness | 0.85–0.93 nm | — |
Duration | 0.5–2 hours | — |
Duration | 0.5–1.2 hours | — |
Duration | 1–3 hours | — |
Duration | ≤ 1 hour | — |
Temperature | 600–1200 °C | — |
Temperature | 100–600 °C | — |
Li₂FeO₄
Na₂FeO₄
LixCoO₄
NaxCoO₄
KxCoO₄
LixNiO₄
KxNiO₄
layered graphite
hydrogen peroxide
H₂O₂
sulfuric acid
H₂SO₄
K₂FeO₄
exfoliated graphite
graphene
NaxNiO₄
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
| — |
Duration | 1200–7200 s | — |
Duration | 45–70 minutes | — |
Duration | 5–120 hours | — |
Temperature | 800–1100 °C | — |
Temperature | 100–1500 °C | — |
Duration | 30–60 seconds | — |
Temperature | 100–1200 °C | — |
Duration | 6–96 hours | — |
Duration | 30–90 seconds | — |
Thickness | 0.85–0.93 nm | — |
Duration | 0.5–2 hours | — |
Duration | 0.5–1.2 hours | — |
Duration | 1–3 hours | — |
Duration | ≤ 1 hour | — |
Temperature | 600–1200 °C | — |
Temperature | 100–600 °C | — |
Li₂FeO₄
Na₂FeO₄
LixCoO₄
NaxCoO₄
KxCoO₄
LixNiO₄
KxNiO₄
layered graphite
hydrogen peroxide
H₂O₂
sulfuric acid
H₂SO₄
K₂FeO₄
exfoliated graphite
graphene
NaxNiO₄
FIG.4 Transmission electron micrograph of graphe n e sheets produced by the inventive process.
| — |
Duration | 1200–7200 s | — |
Duration | 45–70 minutes | — |
Duration | 5–120 hours | — |
Temperature | 800–1100 °C | — |
Temperature | 100–1500 °C | — |
Duration | 30–60 seconds | — |
Temperature | 100–1200 °C | — |
Duration | 6–96 hours | — |
Duration | 30–90 seconds | — |
Thickness | 0.85–0.93 nm | — |
Duration | 0.5–2 hours | — |
Duration | 0.5–1.2 hours | — |
Duration | 1–3 hours | — |
Duration | ≤ 1 hour | — |
Temperature | 600–1200 °C | — |
Temperature | 100–600 °C | — |