Patent
US 10,549,999PRODUCTION OF GRAPHENE
Amr Abdelkader
THE UNIVERSITY OF MANCHESTER·13 April 2017·US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 10,549,999Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are sulfur-containing cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 1, wherein the sulfur-containing cations are organosulfur cations. Original
A method according to claim 1, wherein the counteranions are selected from bis(trifluoromethylsulfonyl)imide, bromide, tetrafluoroborate (BF 4-), perchlorate (ClO 4) and hexafluorophosphate (PF J). Previously presented
A method according to claim 1, wherein the solvent is a non- aqueous solvent,,,, '. Currently amended
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are phosphorous-containing ions and wherein the electrolyte is substantially free of metal cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 7, wherein the phosphorous-containing cations are phosphonium ions. Original
A method according to claim 7, wherein the counteranions are selected from hydroxide, bromide, tetrafluoroborate (BF 4-), perchlorate (C lO 4-) and hexafluorophosphate (PF J). Previously presented
A method according to claim 7, wherein the solvent is a non- aqueous solvent,,,, ',. Currently amended
A method according to claim 7, wherein the negative electrode is an electrode comprising one or more selected from highly ordered pyrolytic graphite, natural graphite and synthetic graphite. Previously presented
A method according to claim 7, which is carried out a temperature from 20 ° C to 150 0 C. Previously presented
A method according to claim 7, wherein the graphene or graphite nanoplatelet structures having a thickness of less than 100 nm are separated from the electrolyte by at least one technique selected from: (a) filtering; (b) using centrifugal forces to precipitate the graphene or graphite nanoplatelet structures; and (c) collecting the graphene or graphite nanoplatelet structures at the interface of two immiscible solvents. Previously presented
A method according to claim 7, wherein the electrochemically exfoliated graphene or graphite nanoplatelet structures are further treated using ultrasonic energy and/or thermal energy. Previously presented
A method according to claim 7, wherein the method further includes the step of isolating the graphene or graphite nanoplatelet structures. Previously presented
Layer stacks claimed or described, ordered top of device to substrate.
electrochemical exfoliation cell
Materials described outside the worked examples.
graphene
graphite nanoplatelet structures
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0–500 nm | — |
Voltage | 20–20 V |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,549,999Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are sulfur-containing cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 1, wherein the sulfur-containing cations are organosulfur cations. Original
A method according to claim 1, wherein the counteranions are selected from bis(trifluoromethylsulfonyl)imide, bromide, tetrafluoroborate (BF 4-), perchlorate (ClO 4) and hexafluorophosphate (PF J). Previously presented
A method according to claim 1, wherein the solvent is a non- aqueous solvent,,,, '. Currently amended
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are phosphorous-containing ions and wherein the electrolyte is substantially free of metal cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 7, wherein the phosphorous-containing cations are phosphonium ions. Original
A method according to claim 7, wherein the counteranions are selected from hydroxide, bromide, tetrafluoroborate (BF 4-), perchlorate (C lO 4-) and hexafluorophosphate (PF J). Previously presented
A method according to claim 7, wherein the solvent is a non- aqueous solvent,,,, ',. Currently amended
A method according to claim 7, wherein the negative electrode is an electrode comprising one or more selected from highly ordered pyrolytic graphite, natural graphite and synthetic graphite. Previously presented
A method according to claim 7, which is carried out a temperature from 20 ° C to 150 0 C. Previously presented
A method according to claim 7, wherein the graphene or graphite nanoplatelet structures having a thickness of less than 100 nm are separated from the electrolyte by at least one technique selected from: (a) filtering; (b) using centrifugal forces to precipitate the graphene or graphite nanoplatelet structures; and (c) collecting the graphene or graphite nanoplatelet structures at the interface of two immiscible solvents. Previously presented
A method according to claim 7, wherein the electrochemically exfoliated graphene or graphite nanoplatelet structures are further treated using ultrasonic energy and/or thermal energy. Previously presented
A method according to claim 7, wherein the method further includes the step of isolating the graphene or graphite nanoplatelet structures. Previously presented
Layer stacks claimed or described, ordered top of device to substrate.
electrochemical exfoliation cell
Materials described outside the worked examples.
graphene
graphite nanoplatelet structures
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0–500 nm | — |
Voltage | 20–20 V |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,549,999Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are sulfur-containing cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 1, wherein the sulfur-containing cations are organosulfur cations. Original
A method according to claim 1, wherein the counteranions are selected from bis(trifluoromethylsulfonyl)imide, bromide, tetrafluoroborate (BF 4-), perchlorate (ClO 4) and hexafluorophosphate (PF J). Previously presented
A method according to claim 1, wherein the solvent is a non- aqueous solvent,,,, '. Currently amended
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are phosphorous-containing ions and wherein the electrolyte is substantially free of metal cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 7, wherein the phosphorous-containing cations are phosphonium ions. Original
A method according to claim 7, wherein the counteranions are selected from hydroxide, bromide, tetrafluoroborate (BF 4-), perchlorate (C lO 4-) and hexafluorophosphate (PF J). Previously presented
A method according to claim 7, wherein the solvent is a non- aqueous solvent,,,, ',. Currently amended
A method according to claim 7, wherein the negative electrode is an electrode comprising one or more selected from highly ordered pyrolytic graphite, natural graphite and synthetic graphite. Previously presented
A method according to claim 7, which is carried out a temperature from 20 ° C to 150 0 C. Previously presented
A method according to claim 7, wherein the graphene or graphite nanoplatelet structures having a thickness of less than 100 nm are separated from the electrolyte by at least one technique selected from: (a) filtering; (b) using centrifugal forces to precipitate the graphene or graphite nanoplatelet structures; and (c) collecting the graphene or graphite nanoplatelet structures at the interface of two immiscible solvents. Previously presented
A method according to claim 7, wherein the electrochemically exfoliated graphene or graphite nanoplatelet structures are further treated using ultrasonic energy and/or thermal energy. Previously presented
A method according to claim 7, wherein the method further includes the step of isolating the graphene or graphite nanoplatelet structures. Previously presented
Layer stacks claimed or described, ordered top of device to substrate.
electrochemical exfoliation cell
Materials described outside the worked examples.
graphene
graphite nanoplatelet structures
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0–500 nm | — |
Voltage | 20–20 V |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,549,999Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are sulfur-containing cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 1, wherein the sulfur-containing cations are organosulfur cations. Original
A method according to claim 1, wherein the counteranions are selected from bis(trifluoromethylsulfonyl)imide, bromide, tetrafluoroborate (BF 4-), perchlorate (ClO 4) and hexafluorophosphate (PF J). Previously presented
A method according to claim 1, wherein the solvent is a non- aqueous solvent,,,, '. Currently amended
A method for the production in an electrochemical cell of graphene and graphite nanoplatelet structures having a thickness of less than 100 nm, wherein the electrochemical cell comprises: (a) a negative electrode which is graphitic; (b) a positive electrode which may be graphitic or another material; and (c) an electrolyte having ions in a solvent, wherein the ions include cations and counteranions, and wherein the cations are phosphorous-containing ions and wherein the electrolyte is substantially free of metal cations; and wherein the method comprises the step of passing a current through the electrochemical cell to intercalate ions into the graphitic negative electrode so as to exfoliate the graphitic negative electrode. Currently amended
A method according to claim 7, wherein the phosphorous-containing cations are phosphonium ions. Original
A method according to claim 7, wherein the counteranions are selected from hydroxide, bromide, tetrafluoroborate (BF 4-), perchlorate (C lO 4-) and hexafluorophosphate (PF J). Previously presented
A method according to claim 7, wherein the solvent is a non- aqueous solvent,,,, ',. Currently amended
A method according to claim 7, wherein the negative electrode is an electrode comprising one or more selected from highly ordered pyrolytic graphite, natural graphite and synthetic graphite. Previously presented
A method according to claim 7, which is carried out a temperature from 20 ° C to 150 0 C. Previously presented
A method according to claim 7, wherein the graphene or graphite nanoplatelet structures having a thickness of less than 100 nm are separated from the electrolyte by at least one technique selected from: (a) filtering; (b) using centrifugal forces to precipitate the graphene or graphite nanoplatelet structures; and (c) collecting the graphene or graphite nanoplatelet structures at the interface of two immiscible solvents. Previously presented
A method according to claim 7, wherein the electrochemically exfoliated graphene or graphite nanoplatelet structures are further treated using ultrasonic energy and/or thermal energy. Previously presented
A method according to claim 7, wherein the method further includes the step of isolating the graphene or graphite nanoplatelet structures. Previously presented
Layer stacks claimed or described, ordered top of device to substrate.
electrochemical exfoliation cell
Materials described outside the worked examples.
graphene
graphite nanoplatelet structures
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows a typical Raman spectrum of the product produced in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0–500 nm | — |
Voltage | 20–20 V |
Related documents with shared materials, methods, properties, or citations.
sulfur-containing cations
sulfonium ions
trialkyl sulfonium ions
counteranions (bis(trifluoromethylsulfonyl)imide, bromide, BF₄-, ClO4, PF₆-)
non-aqueous solvent
phosphorous-containing cations
phosphonium ions
tetraalkyl phosphonium ions
tetrabutyl phosphonium
tetraethyl phosphonium
tetramethyl phosphonium
counteranions (hydroxide, bromide, BF₄-, ClO₄-, PF₆-)
highly ordered pyrolytic graphite
natural graphite
synthetic graphite
trimethyl sulfonium
N-methyl-2-pyrrolidone
N,N'-dimethyl formamide
dimethyl sulfoxide
DMSO
triethyl sulfonium
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
| — |
Voltage | 15–15 V | — |
Voltage | 12–15 V | — |
Voltage | 12–12 V | — |
Voltage | 10–10 V | — |
Voltage | 1–20 V | — |
Voltage | 1–15 V | — |
Voltage | 1–12 V | — |
Voltage | 1–10 V | — |
Voltage | 2–10 V | — |
Voltage | 2–8 V | — |
Voltage | 2–5 V | — |
Voltage | 3–5 V | — |
Thickness | ≤ 1 nm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 20 nm | — |
Thickness | ≤ 10 nm | — |
Thickness | ≤ 90 nm | — |
Thickness | ≤ 10 cm | — |
Thickness | ≤ 1 mm | — |
Thickness | ≤ 1 µm | — |
Thickness | ≥ 1 nm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 10 cm | — |
Thickness | ≥ 1 mm | — |
Temperature | ≥ 20 °C | — |
Temperature | ≥ 10 °C | — |
Temperature | ≥ 30 °C | — |
Duration | ≥ 5 min | — |
sulfur-containing cations
sulfonium ions
trialkyl sulfonium ions
counteranions (bis(trifluoromethylsulfonyl)imide, bromide, BF₄-, ClO4, PF₆-)
non-aqueous solvent
phosphorous-containing cations
phosphonium ions
tetraalkyl phosphonium ions
tetrabutyl phosphonium
tetraethyl phosphonium
tetramethyl phosphonium
counteranions (hydroxide, bromide, BF₄-, ClO₄-, PF₆-)
highly ordered pyrolytic graphite
natural graphite
synthetic graphite
trimethyl sulfonium
N-methyl-2-pyrrolidone
N,N'-dimethyl formamide
dimethyl sulfoxide
DMSO
triethyl sulfonium
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
| — |
Voltage | 15–15 V | — |
Voltage | 12–15 V | — |
Voltage | 12–12 V | — |
Voltage | 10–10 V | — |
Voltage | 1–20 V | — |
Voltage | 1–15 V | — |
Voltage | 1–12 V | — |
Voltage | 1–10 V | — |
Voltage | 2–10 V | — |
Voltage | 2–8 V | — |
Voltage | 2–5 V | — |
Voltage | 3–5 V | — |
Thickness | ≤ 1 nm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 20 nm | — |
Thickness | ≤ 10 nm | — |
Thickness | ≤ 90 nm | — |
Thickness | ≤ 10 cm | — |
Thickness | ≤ 1 mm | — |
Thickness | ≤ 1 µm | — |
Thickness | ≥ 1 nm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 10 cm | — |
Thickness | ≥ 1 mm | — |
Temperature | ≥ 20 °C | — |
Temperature | ≥ 10 °C | — |
Temperature | ≥ 30 °C | — |
Duration | ≥ 5 min | — |
sulfur-containing cations
sulfonium ions
trialkyl sulfonium ions
counteranions (bis(trifluoromethylsulfonyl)imide, bromide, BF₄-, ClO4, PF₆-)
non-aqueous solvent
phosphorous-containing cations
phosphonium ions
tetraalkyl phosphonium ions
tetrabutyl phosphonium
tetraethyl phosphonium
tetramethyl phosphonium
counteranions (hydroxide, bromide, BF₄-, ClO₄-, PF₆-)
highly ordered pyrolytic graphite
natural graphite
synthetic graphite
trimethyl sulfonium
N-methyl-2-pyrrolidone
N,N'-dimethyl formamide
dimethyl sulfoxide
DMSO
triethyl sulfonium
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
| — |
Voltage | 15–15 V | — |
Voltage | 12–15 V | — |
Voltage | 12–12 V | — |
Voltage | 10–10 V | — |
Voltage | 1–20 V | — |
Voltage | 1–15 V | — |
Voltage | 1–12 V | — |
Voltage | 1–10 V | — |
Voltage | 2–10 V | — |
Voltage | 2–8 V | — |
Voltage | 2–5 V | — |
Voltage | 3–5 V | — |
Thickness | ≤ 1 nm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 20 nm | — |
Thickness | ≤ 10 nm | — |
Thickness | ≤ 90 nm | — |
Thickness | ≤ 10 cm | — |
Thickness | ≤ 1 mm | — |
Thickness | ≤ 1 µm | — |
Thickness | ≥ 1 nm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 10 cm | — |
Thickness | ≥ 1 mm | — |
Temperature | ≥ 20 °C | — |
Temperature | ≥ 10 °C | — |
Temperature | ≥ 30 °C | — |
Duration | ≥ 5 min | — |
sulfur-containing cations
sulfonium ions
trialkyl sulfonium ions
counteranions (bis(trifluoromethylsulfonyl)imide, bromide, BF₄-, ClO4, PF₆-)
non-aqueous solvent
phosphorous-containing cations
phosphonium ions
tetraalkyl phosphonium ions
tetrabutyl phosphonium
tetraethyl phosphonium
tetramethyl phosphonium
counteranions (hydroxide, bromide, BF₄-, ClO₄-, PF₆-)
highly ordered pyrolytic graphite
natural graphite
synthetic graphite
trimethyl sulfonium
N-methyl-2-pyrrolidone
N,N'-dimethyl formamide
dimethyl sulfoxide
DMSO
triethyl sulfonium
Figure 2 shows a typical Raman spectrum of the product produced in Example 2; and
Figure 3 shows a typical Raman spectrum of the product produced in Example 3. The present invention is described in more detail by way of example only with reference to the following Examples.
| — |
Voltage | 15–15 V | — |
Voltage | 12–15 V | — |
Voltage | 12–12 V | — |
Voltage | 10–10 V | — |
Voltage | 1–20 V | — |
Voltage | 1–15 V | — |
Voltage | 1–12 V | — |
Voltage | 1–10 V | — |
Voltage | 2–10 V | — |
Voltage | 2–8 V | — |
Voltage | 2–5 V | — |
Voltage | 3–5 V | — |
Thickness | ≤ 1 nm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 20 nm | — |
Thickness | ≤ 10 nm | — |
Thickness | ≤ 90 nm | — |
Thickness | ≤ 10 cm | — |
Thickness | ≤ 1 mm | — |
Thickness | ≤ 1 µm | — |
Thickness | ≥ 1 nm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 10 cm | — |
Thickness | ≥ 1 mm | — |
Temperature | ≥ 20 °C | — |
Temperature | ≥ 10 °C | — |
Temperature | ≥ 30 °C | — |
Duration | ≥ 5 min | — |