Patent
US 9,422,164ELECTROCHEMICAL METHOD OF PRODUCING NANO GRAPHENE PLATELETS
Aruna Zhamu
US
Copyright © 2026 Matter42. All rights reserved.
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Atlas literature
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US 9,422,164Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
FIG.2 is an appa r atus that can be used for electrochemical 15 intercalation of graphite according to a preferred embodiment of the present invention. The …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
FIG.5 of Ref. 10). Re-intercalation by liquid eutectic 5 of sodium and potassium (NaK₂) and subsequent exfoliation yielded platelets with thicknesses of 2 -150 …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Previously amended) A method of producing nano-scaled graphene platelets with an average thickness smaller than 30 nm from alayered graphite material, said method comprising: a) forming a carboxylic acid-intercalated graphite compound by an electrochemical reaction which uses a carboxylic acid as both an electrolyte and an intercalate source, said layered graphite material as an anode material, and a metal or graphite as a cathode material, and wherein a current is imposed upon said cathode and said anode at a current density for a duration of time sufficient for effecting said electrochemical reaction, wherein said carboxylic a c id is selected from the group consisting of propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, and combinations thereof; b) exposing said carboxylic acid-intercalated graphite compound to a thermal shock to form exfoliated graphite; and c) subjecting said exfoliated graphite to a mechanical shearing treatment to produce said nano- scaled graphene platelets.
The method of claim 1 wherein said layered graphite material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said mechanical shearing treatment comprises using air milling, airjet milling, ball milling, rotating-blade mechanical shearing, ultrasonication, or a combination thereof. 2
The method of claim 1 wherein the imposing current provides a current density in the range of 50 to 600 A/m 2
(Previously amended) The method of claim 1 wherein said step of exposing comprises heating said carboxylic acid-intercalated graphite to a temperature in the range of 300- 800 0 C for a period of 15 seconds to 2 minutes.
The method of claim 1 wherein said mechanical shearing treatment comprises operating an air mill or air jet mill at a desired air velocity sufficient for breaking up flakes of exfoliated graphite.
The method of claim 1, further comprising additional steps of electrochemically intercalating said nano-scaled graphene platelets to obtain a further intercalated compound and exfoliating said further intercalated compound to produce thinner nano-scaled graphene platelets.
The method of claim 1 wherein the imposing current provides a current density in the range of 100 to 400 A/m 2
canceled
canceled
11-21. canceled
Materials described outside the worked examples.
propionic acid
C₃H₆O₂
butyric acid
C₄H₈O₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Average Thickness | ≤ 30 nm | nano-scaled graphene platelets |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,422,164Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
FIG.2 is an appa r atus that can be used for electrochemical 15 intercalation of graphite according to a preferred embodiment of the present invention. The …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
FIG.5 of Ref. 10). Re-intercalation by liquid eutectic 5 of sodium and potassium (NaK₂) and subsequent exfoliation yielded platelets with thicknesses of 2 -150 …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Previously amended) A method of producing nano-scaled graphene platelets with an average thickness smaller than 30 nm from alayered graphite material, said method comprising: a) forming a carboxylic acid-intercalated graphite compound by an electrochemical reaction which uses a carboxylic acid as both an electrolyte and an intercalate source, said layered graphite material as an anode material, and a metal or graphite as a cathode material, and wherein a current is imposed upon said cathode and said anode at a current density for a duration of time sufficient for effecting said electrochemical reaction, wherein said carboxylic a c id is selected from the group consisting of propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, and combinations thereof; b) exposing said carboxylic acid-intercalated graphite compound to a thermal shock to form exfoliated graphite; and c) subjecting said exfoliated graphite to a mechanical shearing treatment to produce said nano- scaled graphene platelets.
The method of claim 1 wherein said layered graphite material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said mechanical shearing treatment comprises using air milling, airjet milling, ball milling, rotating-blade mechanical shearing, ultrasonication, or a combination thereof. 2
The method of claim 1 wherein the imposing current provides a current density in the range of 50 to 600 A/m 2
(Previously amended) The method of claim 1 wherein said step of exposing comprises heating said carboxylic acid-intercalated graphite to a temperature in the range of 300- 800 0 C for a period of 15 seconds to 2 minutes.
The method of claim 1 wherein said mechanical shearing treatment comprises operating an air mill or air jet mill at a desired air velocity sufficient for breaking up flakes of exfoliated graphite.
The method of claim 1, further comprising additional steps of electrochemically intercalating said nano-scaled graphene platelets to obtain a further intercalated compound and exfoliating said further intercalated compound to produce thinner nano-scaled graphene platelets.
The method of claim 1 wherein the imposing current provides a current density in the range of 100 to 400 A/m 2
canceled
canceled
11-21. canceled
Materials described outside the worked examples.
propionic acid
C₃H₆O₂
butyric acid
C₄H₈O₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Average Thickness | ≤ 30 nm | nano-scaled graphene platelets |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,422,164Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
FIG.2 is an appa r atus that can be used for electrochemical 15 intercalation of graphite according to a preferred embodiment of the present invention. The …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
FIG.5 of Ref. 10). Re-intercalation by liquid eutectic 5 of sodium and potassium (NaK₂) and subsequent exfoliation yielded platelets with thicknesses of 2 -150 …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Previously amended) A method of producing nano-scaled graphene platelets with an average thickness smaller than 30 nm from alayered graphite material, said method comprising: a) forming a carboxylic acid-intercalated graphite compound by an electrochemical reaction which uses a carboxylic acid as both an electrolyte and an intercalate source, said layered graphite material as an anode material, and a metal or graphite as a cathode material, and wherein a current is imposed upon said cathode and said anode at a current density for a duration of time sufficient for effecting said electrochemical reaction, wherein said carboxylic a c id is selected from the group consisting of propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, and combinations thereof; b) exposing said carboxylic acid-intercalated graphite compound to a thermal shock to form exfoliated graphite; and c) subjecting said exfoliated graphite to a mechanical shearing treatment to produce said nano- scaled graphene platelets.
The method of claim 1 wherein said layered graphite material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said mechanical shearing treatment comprises using air milling, airjet milling, ball milling, rotating-blade mechanical shearing, ultrasonication, or a combination thereof. 2
The method of claim 1 wherein the imposing current provides a current density in the range of 50 to 600 A/m 2
(Previously amended) The method of claim 1 wherein said step of exposing comprises heating said carboxylic acid-intercalated graphite to a temperature in the range of 300- 800 0 C for a period of 15 seconds to 2 minutes.
The method of claim 1 wherein said mechanical shearing treatment comprises operating an air mill or air jet mill at a desired air velocity sufficient for breaking up flakes of exfoliated graphite.
The method of claim 1, further comprising additional steps of electrochemically intercalating said nano-scaled graphene platelets to obtain a further intercalated compound and exfoliating said further intercalated compound to produce thinner nano-scaled graphene platelets.
The method of claim 1 wherein the imposing current provides a current density in the range of 100 to 400 A/m 2
canceled
canceled
11-21. canceled
Materials described outside the worked examples.
propionic acid
C₃H₆O₂
butyric acid
C₄H₈O₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Average Thickness | ≤ 30 nm | nano-scaled graphene platelets |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,422,164Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
FIG.2 is an appa r atus that can be used for electrochemical 15 intercalation of graphite according to a preferred embodiment of the present invention. The …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
FIG.5 of Ref. 10). Re-intercalation by liquid eutectic 5 of sodium and potassium (NaK₂) and subsequent exfoliation yielded platelets with thicknesses of 2 -150 …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Previously amended) A method of producing nano-scaled graphene platelets with an average thickness smaller than 30 nm from alayered graphite material, said method comprising: a) forming a carboxylic acid-intercalated graphite compound by an electrochemical reaction which uses a carboxylic acid as both an electrolyte and an intercalate source, said layered graphite material as an anode material, and a metal or graphite as a cathode material, and wherein a current is imposed upon said cathode and said anode at a current density for a duration of time sufficient for effecting said electrochemical reaction, wherein said carboxylic a c id is selected from the group consisting of propionic, butyric, pentanoic, hexanoic acids, anhydrides thereof, and combinations thereof; b) exposing said carboxylic acid-intercalated graphite compound to a thermal shock to form exfoliated graphite; and c) subjecting said exfoliated graphite to a mechanical shearing treatment to produce said nano- scaled graphene platelets.
The method of claim 1 wherein said layered graphite material is selected from natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite, or a combination thereof.
The method of claim 1 wherein said mechanical shearing treatment comprises using air milling, airjet milling, ball milling, rotating-blade mechanical shearing, ultrasonication, or a combination thereof. 2
The method of claim 1 wherein the imposing current provides a current density in the range of 50 to 600 A/m 2
(Previously amended) The method of claim 1 wherein said step of exposing comprises heating said carboxylic acid-intercalated graphite to a temperature in the range of 300- 800 0 C for a period of 15 seconds to 2 minutes.
The method of claim 1 wherein said mechanical shearing treatment comprises operating an air mill or air jet mill at a desired air velocity sufficient for breaking up flakes of exfoliated graphite.
The method of claim 1, further comprising additional steps of electrochemically intercalating said nano-scaled graphene platelets to obtain a further intercalated compound and exfoliating said further intercalated compound to produce thinner nano-scaled graphene platelets.
The method of claim 1 wherein the imposing current provides a current density in the range of 100 to 400 A/m 2
canceled
canceled
11-21. canceled
Materials described outside the worked examples.
propionic acid
C₃H₆O₂
butyric acid
C₄H₈O₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 A flow chart showing a two-stage process of producing ultra-thin graphite platelets (NGPs with an average thickness thinner than 2 nm or 5 layers). Both …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Average Thickness | ≤ 30 nm | nano-scaled graphene platelets |
Duration | 10–120 s |
Related documents with shared materials, methods, properties, or citations.
C₅H₁₀O₂
hexanoic acid
C₆H₁₂O₂
layered graphite material
nano-scaled graphene platelets
layered graphite material (natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite)
carboxylic acid-intercalated graphite
nano-scaled graphene platelets (for further intercalation)
formic acid
HCOOH
acetic acid
CH₃COOH
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
| — |
Duration | 2–5 hours | — |
Thickness | ≥ 10 nm | — |
Duration | 15–120 s | — |
C₅H₁₀O₂
hexanoic acid
C₆H₁₂O₂
layered graphite material
nano-scaled graphene platelets
layered graphite material (natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite)
carboxylic acid-intercalated graphite
nano-scaled graphene platelets (for further intercalation)
formic acid
HCOOH
acetic acid
CH₃COOH
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
| — |
Duration | 2–5 hours | — |
Thickness | ≥ 10 nm | — |
Duration | 15–120 s | — |
C₅H₁₀O₂
hexanoic acid
C₆H₁₂O₂
layered graphite material
nano-scaled graphene platelets
layered graphite material (natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite)
carboxylic acid-intercalated graphite
nano-scaled graphene platelets (for further intercalation)
formic acid
HCOOH
acetic acid
CH₃COOH
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
| — |
Duration | 2–5 hours | — |
Thickness | ≥ 10 nm | — |
Duration | 15–120 s | — |
C₅H₁₀O₂
hexanoic acid
C₆H₁₂O₂
layered graphite material
nano-scaled graphene platelets
layered graphite material (natural graphite, synthetic graphite, highly oriented pyrolytic graphite, graphite fiber, graphitic nano-fiber, graphite oxide, graphite fluoride, chemically modified graphite, graphite intercalation compound, exfoliated graphite)
carboxylic acid-intercalated graphite
nano-scaled graphene platelets (for further intercalation)
formic acid
HCOOH
acetic acid
CH₃COOH
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.3(A)). In one preferred embodiment of the present invention, Phase II entails essentially repeating Phase I to further reduce the average platelet …
FIG.4. It is clear that the fo rm ic acid- intercalated graphite led to a narrower thickness distribution (more 10 uniform size) and a smaller average …
| — |
Duration | 2–5 hours | — |
Thickness | ≥ 10 nm | — |
Duration | 15–120 s | — |