Patent
US 11,001,499GRAPHENE OXIDE PARTICLES AND METHOD OF MAKING AND USING THEM
RASUL, Shahid
King Abdullah University of Science and Technology·07 December 2017·US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 11,001,499Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B shows x-ray diffraction of reduced graphene oxides (rIGO1, rIGO2, and rIG O 3) made according to three different methods described herein as compared to …
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
FIG. 3 shows SEMs of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. [0038]
FIG. 4A shows the results of thermogravimetric analysis (TGA) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0039]
FIG. 5A shows Fourier transform infrared spectroscopy (FTIR) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0041]
FIG. 6 shows the values for Brunauer, Emmett and Teller (BET) su r face areas of graphene oxides IG O 1, IGO 2, and IG₀ 3 and reduced graphene oxides rIGO1, …
FIG. 7B shows the results of x-ray photoelectron spectroscopy of reduced graphene oxides rIGO1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. …
FIG. 8D shows the cyclic pe r formance of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO at a current density of …
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 graphene oxide comprising: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric { H 4 (H₂ SO 4) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3-1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture in a graphite to KMn O 4 ratio from about 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
The method of claim 1, wherein the oxidizing step is in the absence of NaNO3. Original
The method of claim 1, wherein the stirring in steps b, d, e takes place in ice bath. Currently amended
The method of-claim 1, wherein the adjusting step comprises adding Na₂ CO3. Currently amended
The method of claim 1, wherein the alcohol is ethanol. Currently amended
The method of claim 1, further comprising reducing the isolated graphene oxide. Currently amended
Claims 9-15. Canceled
Canceled
A method of producing graphene oxide comprising: a. oxidizing graphite in a volume of phosphoric (H₃P O 4) and sulfuric (H 2SO₄ 1 { 4 acids as a graphite-acid mixture wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid volume is from 1:3-1:9 by volume, said volume having a greater than 50% concentration of acid; b. stirring the graphite-acid mixture for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
1 7. The method of claim 16, wherein the oxidizing step is in the absence of NaN O3. Original
1 8. The method of claim 16, wherein the stirring in steps b, d, e takes place in ice bath. Original
The method of claim 16, wherein the adjusting step comprises adding Na₂ CO3. Original
The method of claim 16, wherein the alcohol is ethanol. Original
21. The method of claim 16, wherein the volume of water added is one- fourth the volume of the acid volume in step (a). Original
The method of claim 16, wherein the graphene oxide dispersion is heated to 90 OC for 60 minutes. Original
The method of claim 16, further comprising-reducing the isolated graphene oxide by h y drothermal reduction, which comprises a. dilutin q the isolated q raphene oxide in water; b. dis p ersin q the diluted grap hene oxide of ste p (a) with sonication; c. heating the dispersed g raphene oxide of step (b) for about 24 hours at about 180 C; and d. isolatin q the reduced g raphene oxide. Currently amended
Claims 24-30. Canceled
Canceled
An energy storage device comprising graphene oxide made by the method of: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric (H₂ SO₄) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3- 1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, K C₀ 3, CaCO 3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Original
The energy storage device comprising graphene oxide particles of claim 331, wherein said energy storage device is a battery or a supercapacitor. Currently amended
The energy storage device comprising graphene oxide of claim 331, further comprising the steps of: a. diluting the isolated graphene oxide in water; b. dispersing the diluted graphene oxide of step (a) with sonication; c. heating the dispersed graphene oxide of step (b) for about 24 hours at about 180 C; and d. isolating the reduced graphene oxide. Currently amended
The energy storage device comprising graphene energy storage device is a battery or a supercapacitor. oxide particles of claim 33, wherein said Original
Layer stacks claimed or described, ordered top of device to substrate.
energy storage device
Materials described outside the worked examples.
graphite
C
phosphoric acid/sulfuric acid mixture
H₃PO₄/H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.1–0.9 V | — |
Duration | 600–7200 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,001,499Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B shows x-ray diffraction of reduced graphene oxides (rIGO1, rIGO2, and rIG O 3) made according to three different methods described herein as compared to …
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
FIG. 3 shows SEMs of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. [0038]
FIG. 4A shows the results of thermogravimetric analysis (TGA) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0039]
FIG. 5A shows Fourier transform infrared spectroscopy (FTIR) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0041]
FIG. 6 shows the values for Brunauer, Emmett and Teller (BET) su r face areas of graphene oxides IG O 1, IGO 2, and IG₀ 3 and reduced graphene oxides rIGO1, …
FIG. 7B shows the results of x-ray photoelectron spectroscopy of reduced graphene oxides rIGO1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. …
FIG. 8D shows the cyclic pe r formance of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO at a current density of …
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 graphene oxide comprising: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric { H 4 (H₂ SO 4) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3-1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture in a graphite to KMn O 4 ratio from about 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
The method of claim 1, wherein the oxidizing step is in the absence of NaNO3. Original
The method of claim 1, wherein the stirring in steps b, d, e takes place in ice bath. Currently amended
The method of-claim 1, wherein the adjusting step comprises adding Na₂ CO3. Currently amended
The method of claim 1, wherein the alcohol is ethanol. Currently amended
The method of claim 1, further comprising reducing the isolated graphene oxide. Currently amended
Claims 9-15. Canceled
Canceled
A method of producing graphene oxide comprising: a. oxidizing graphite in a volume of phosphoric (H₃P O 4) and sulfuric (H 2SO₄ 1 { 4 acids as a graphite-acid mixture wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid volume is from 1:3-1:9 by volume, said volume having a greater than 50% concentration of acid; b. stirring the graphite-acid mixture for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
1 7. The method of claim 16, wherein the oxidizing step is in the absence of NaN O3. Original
1 8. The method of claim 16, wherein the stirring in steps b, d, e takes place in ice bath. Original
The method of claim 16, wherein the adjusting step comprises adding Na₂ CO3. Original
The method of claim 16, wherein the alcohol is ethanol. Original
21. The method of claim 16, wherein the volume of water added is one- fourth the volume of the acid volume in step (a). Original
The method of claim 16, wherein the graphene oxide dispersion is heated to 90 OC for 60 minutes. Original
The method of claim 16, further comprising-reducing the isolated graphene oxide by h y drothermal reduction, which comprises a. dilutin q the isolated q raphene oxide in water; b. dis p ersin q the diluted grap hene oxide of ste p (a) with sonication; c. heating the dispersed g raphene oxide of step (b) for about 24 hours at about 180 C; and d. isolatin q the reduced g raphene oxide. Currently amended
Claims 24-30. Canceled
Canceled
An energy storage device comprising graphene oxide made by the method of: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric (H₂ SO₄) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3- 1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, K C₀ 3, CaCO 3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Original
The energy storage device comprising graphene oxide particles of claim 331, wherein said energy storage device is a battery or a supercapacitor. Currently amended
The energy storage device comprising graphene oxide of claim 331, further comprising the steps of: a. diluting the isolated graphene oxide in water; b. dispersing the diluted graphene oxide of step (a) with sonication; c. heating the dispersed graphene oxide of step (b) for about 24 hours at about 180 C; and d. isolating the reduced graphene oxide. Currently amended
The energy storage device comprising graphene energy storage device is a battery or a supercapacitor. oxide particles of claim 33, wherein said Original
Layer stacks claimed or described, ordered top of device to substrate.
energy storage device
Materials described outside the worked examples.
graphite
C
phosphoric acid/sulfuric acid mixture
H₃PO₄/H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.1–0.9 V | — |
Duration | 600–7200 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,001,499Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B shows x-ray diffraction of reduced graphene oxides (rIGO1, rIGO2, and rIG O 3) made according to three different methods described herein as compared to …
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
FIG. 3 shows SEMs of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. [0038]
FIG. 4A shows the results of thermogravimetric analysis (TGA) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0039]
FIG. 5A shows Fourier transform infrared spectroscopy (FTIR) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0041]
FIG. 6 shows the values for Brunauer, Emmett and Teller (BET) su r face areas of graphene oxides IG O 1, IGO 2, and IG₀ 3 and reduced graphene oxides rIGO1, …
FIG. 7B shows the results of x-ray photoelectron spectroscopy of reduced graphene oxides rIGO1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. …
FIG. 8D shows the cyclic pe r formance of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO at a current density of …
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 graphene oxide comprising: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric { H 4 (H₂ SO 4) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3-1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture in a graphite to KMn O 4 ratio from about 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
The method of claim 1, wherein the oxidizing step is in the absence of NaNO3. Original
The method of claim 1, wherein the stirring in steps b, d, e takes place in ice bath. Currently amended
The method of-claim 1, wherein the adjusting step comprises adding Na₂ CO3. Currently amended
The method of claim 1, wherein the alcohol is ethanol. Currently amended
The method of claim 1, further comprising reducing the isolated graphene oxide. Currently amended
Claims 9-15. Canceled
Canceled
A method of producing graphene oxide comprising: a. oxidizing graphite in a volume of phosphoric (H₃P O 4) and sulfuric (H 2SO₄ 1 { 4 acids as a graphite-acid mixture wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid volume is from 1:3-1:9 by volume, said volume having a greater than 50% concentration of acid; b. stirring the graphite-acid mixture for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
1 7. The method of claim 16, wherein the oxidizing step is in the absence of NaN O3. Original
1 8. The method of claim 16, wherein the stirring in steps b, d, e takes place in ice bath. Original
The method of claim 16, wherein the adjusting step comprises adding Na₂ CO3. Original
The method of claim 16, wherein the alcohol is ethanol. Original
21. The method of claim 16, wherein the volume of water added is one- fourth the volume of the acid volume in step (a). Original
The method of claim 16, wherein the graphene oxide dispersion is heated to 90 OC for 60 minutes. Original
The method of claim 16, further comprising-reducing the isolated graphene oxide by h y drothermal reduction, which comprises a. dilutin q the isolated q raphene oxide in water; b. dis p ersin q the diluted grap hene oxide of ste p (a) with sonication; c. heating the dispersed g raphene oxide of step (b) for about 24 hours at about 180 C; and d. isolatin q the reduced g raphene oxide. Currently amended
Claims 24-30. Canceled
Canceled
An energy storage device comprising graphene oxide made by the method of: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric (H₂ SO₄) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3- 1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, K C₀ 3, CaCO 3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Original
The energy storage device comprising graphene oxide particles of claim 331, wherein said energy storage device is a battery or a supercapacitor. Currently amended
The energy storage device comprising graphene oxide of claim 331, further comprising the steps of: a. diluting the isolated graphene oxide in water; b. dispersing the diluted graphene oxide of step (a) with sonication; c. heating the dispersed graphene oxide of step (b) for about 24 hours at about 180 C; and d. isolating the reduced graphene oxide. Currently amended
The energy storage device comprising graphene energy storage device is a battery or a supercapacitor. oxide particles of claim 33, wherein said Original
Layer stacks claimed or described, ordered top of device to substrate.
energy storage device
Materials described outside the worked examples.
graphite
C
phosphoric acid/sulfuric acid mixture
H₃PO₄/H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.1–0.9 V | — |
Duration | 600–7200 s |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,001,499Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B shows x-ray diffraction of reduced graphene oxides (rIGO1, rIGO2, and rIG O 3) made according to three different methods described herein as compared to …
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
FIG. 3 shows SEMs of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. [0038]
FIG. 4A shows the results of thermogravimetric analysis (TGA) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0039]
FIG. 5A shows Fourier transform infrared spectroscopy (FTIR) of graphene oxides IGO1, IGO 2, and IG₀ 3 as compared to graphene oxide HGO. [0041]
FIG. 6 shows the values for Brunauer, Emmett and Teller (BET) su r face areas of graphene oxides IG O 1, IGO 2, and IG₀ 3 and reduced graphene oxides rIGO1, …
FIG. 7B shows the results of x-ray photoelectron spectroscopy of reduced graphene oxides rIGO1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO. …
FIG. 8D shows the cyclic pe r formance of reduced graphene oxides rIGO 1, rIGO2, and rIGO₃ as compared to reduced graphene oxide rHGO at a current density of …
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 graphene oxide comprising: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric { H 4 (H₂ SO 4) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3-1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture in a graphite to KMn O 4 ratio from about 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
The method of claim 1, wherein the oxidizing step is in the absence of NaNO3. Original
The method of claim 1, wherein the stirring in steps b, d, e takes place in ice bath. Currently amended
The method of-claim 1, wherein the adjusting step comprises adding Na₂ CO3. Currently amended
The method of claim 1, wherein the alcohol is ethanol. Currently amended
The method of claim 1, further comprising reducing the isolated graphene oxide. Currently amended
Claims 9-15. Canceled
Canceled
A method of producing graphene oxide comprising: a. oxidizing graphite in a volume of phosphoric (H₃P O 4) and sulfuric (H 2SO₄ 1 { 4 acids as a graphite-acid mixture wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid volume is from 1:3-1:9 by volume, said volume having a greater than 50% concentration of acid; b. stirring the graphite-acid mixture for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, KC O 3, CaCO3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Currently amended
1 7. The method of claim 16, wherein the oxidizing step is in the absence of NaN O3. Original
1 8. The method of claim 16, wherein the stirring in steps b, d, e takes place in ice bath. Original
The method of claim 16, wherein the adjusting step comprises adding Na₂ CO3. Original
The method of claim 16, wherein the alcohol is ethanol. Original
21. The method of claim 16, wherein the volume of water added is one- fourth the volume of the acid volume in step (a). Original
The method of claim 16, wherein the graphene oxide dispersion is heated to 90 OC for 60 minutes. Original
The method of claim 16, further comprising-reducing the isolated graphene oxide by h y drothermal reduction, which comprises a. dilutin q the isolated q raphene oxide in water; b. dis p ersin q the diluted grap hene oxide of ste p (a) with sonication; c. heating the dispersed g raphene oxide of step (b) for about 24 hours at about 180 C; and d. isolatin q the reduced g raphene oxide. Currently amended
Claims 24-30. Canceled
Canceled
An energy storage device comprising graphene oxide made by the method of: a. oxidizing graphite in a mixture of phosphoric (H₃P O 4) and sulfuric (H₂ SO₄) acids, wherein the ratio of H₃P O 4 to H₂ SO 4 in the acid mixture is from 1:3- 1:9 by volume; b. stirring the graphite and acid mixture in an ice bath for 10 minutes to 2 hours; c. adding KMn O 4 to the graphite-acid mixture, wherein the graphite to KMn O 4 ratio is from 1:3 to 1:9 by weight; d. stirring the resulting mixture from step (c) in an ice bath for 10 minutes to 2 hours to form a graphene oxide-dispersion; e. adding a volume of water to the graphene oxide-dispersion, said water having a pH of 0-3 and a volume about one-fourth of the starting acid volume, and stirring the water and graphene oxide dispersion for 10 minutes to 2 hours; f. heating the graphene oxide-dispersion to 60 -1200C for 6 minutes to 8 hours; g. cooling the graphene oxide-dispersion to room temperature; h. adjusting the graphene oxide-dispersion to a pH of 7.0-7.6, wherein the adjusting step comprises adding Na₂ CO 3, NaOH, KOH, K C₀ 3, CaCO 3, or any mixture thereof; i. adding excess alcohol to the graphene oxide-dispersion, wherein the alcohol is selected from methanol, ethanol, propanol, isopropanol, or butanol; j. isolating the graphene oxide by centrifugation; k. sequentially washing the isolated graphene oxide with acid, then water and then alcohol until the effluent reaches a pH of 7.0-7.2; and I. collecting the graphene oxide solids. Original
The energy storage device comprising graphene oxide particles of claim 331, wherein said energy storage device is a battery or a supercapacitor. Currently amended
The energy storage device comprising graphene oxide of claim 331, further comprising the steps of: a. diluting the isolated graphene oxide in water; b. dispersing the diluted graphene oxide of step (a) with sonication; c. heating the dispersed graphene oxide of step (b) for about 24 hours at about 180 C; and d. isolating the reduced graphene oxide. Currently amended
The energy storage device comprising graphene energy storage device is a battery or a supercapacitor. oxide particles of claim 33, wherein said Original
Layer stacks claimed or described, ordered top of device to substrate.
energy storage device
Materials described outside the worked examples.
graphite
C
phosphoric acid/sulfuric acid mixture
H₃PO₄/H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows scanning electron micrographs (SEMs) of graphene oxides IG O1, IGO2, and IGO 3, as compared to graphene oxide HGO. [0037]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.1–0.9 V | — |
Duration | 600–7200 s |
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