Patent
US 9,133,562ELECTRODEPOSITION OF GRAPHENE LAYER FROM DOPED GRAPHITE
Young Kwan LEE
US
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Atlas literature
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US 9,133,562Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically illustrates a method of fabricating a graphene layer using electrodeposition. Expanded graphite was prepared, and was doped using a 20 …
FIG. 2D illustrates a Raman shift according to a dopant of H 2S04: 6 FIG 3 is a result of observing delta frequency by scanning at a rate of 10 mV/s in a range …
FIG. 3D is a graph illustrating a result of observing delta frequency according to a dopant of H 2S04. When the graphene was doped with FeC l 3 and FTS, it …
FIG. 4E illustrates graphene doped with H 2SO4. 13 Unlike smooth PEDOT, a rough PEDOT surface caused by the deposition of the graphene was observed. In …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Please CANCEL claims 15-22 without prejudice or disclaimer in accordance with the following:
The method of claim 1, wherein the dispersing is performed using an ultrasonic wave device.
The method of claim 1, wherein the electrodeposition is performed using a platinum plate as the counter electrode, PEDOT- coated gold as the working electrode, and Ag/AgC I/KCI(sat'd) as a reference electrode.
The method of claim 3, wherein the applied voltage is a negative voltage of -1.5 V to -1.0 V.
A method of electrodepositing graphene, comprising: p-doping expanded graphite using a dopant; dispersing the doped expanded graphite in an organic solvent using ultrasonic waves, and obtaining doped graphene dispersed in the solvent; and applying a negative voltage between a counter electrode and a working electrode placed within the solvent in which the doped graphene is dispersed such that a graphene coating is formed at a surface of the working electrode.
The method of claim 8, wherein the dopant is one of HNO3, FeCl3, H₂SO4, and FTS.
The electrodeposited graphene obtained by the
The electrodeposited graphene obtained by the
The method of claim 1, wherein the dopant is voltage of -1.01 V.
- 22. 4 canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled FeCl3, and the negative voltage is -0.5 V or FeCl3, and the negative voltage is -1.5 V to -1.0 method of claim 1. withdrawn method of claim 8. withdrawn FeC l 3, and the applied voltage is a negative
Embodiments described in the patent, grouped by the materials and process steps they use.
9 materials1 process step
Preparation of dopants (HNO₃ 66%, FeCl₃ 98%, H₂SO₄ 99%, FTS, and 40 wt% butanol solution Baytron CB-40) and organic solvent acetonitrile (ACN, 98%). Graphite from Zaval'evsk coal field (Ukraine, ash content <0.05, particle size 200-300 µm) with C₂F~ClF₃ intercalated was used as expanded graphite. Doped graphene was obtained by p-doping expanded graphite with a Lewis acid dopant, dispersing in ACN by ultrasonication, then electrodepositing onto a PEDOT/gold working electrode using a Pt counter electrode and Ag/AgCl/KCl(sat'd) reference electrode at negative voltage (preferably -1.01 V for FeCl₃ dopant).
Materials described outside the worked examples.
platinum plate (counter electrode)
Pt
PEDOT-coated gold (working electrode)
Measurements and analyses referenced in the patent, with their drawing references.
Raman shift measured for graphene doped with each of FeCl3, FTS, HNO3, and H₂SO₄ (FIG. 2A-2D)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0–1 V | — |
Voltage |
Table 1
SVG
SVG 13546268.
p. 6
Table 2
SVG
3 is indicated in the following Table 2.
p. 7
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,133,562Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically illustrates a method of fabricating a graphene layer using electrodeposition. Expanded graphite was prepared, and was doped using a 20 …
FIG. 2D illustrates a Raman shift according to a dopant of H 2S04: 6 FIG 3 is a result of observing delta frequency by scanning at a rate of 10 mV/s in a range …
FIG. 3D is a graph illustrating a result of observing delta frequency according to a dopant of H 2S04. When the graphene was doped with FeC l 3 and FTS, it …
FIG. 4E illustrates graphene doped with H 2SO4. 13 Unlike smooth PEDOT, a rough PEDOT surface caused by the deposition of the graphene was observed. In …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Please CANCEL claims 15-22 without prejudice or disclaimer in accordance with the following:
The method of claim 1, wherein the dispersing is performed using an ultrasonic wave device.
The method of claim 1, wherein the electrodeposition is performed using a platinum plate as the counter electrode, PEDOT- coated gold as the working electrode, and Ag/AgC I/KCI(sat'd) as a reference electrode.
The method of claim 3, wherein the applied voltage is a negative voltage of -1.5 V to -1.0 V.
A method of electrodepositing graphene, comprising: p-doping expanded graphite using a dopant; dispersing the doped expanded graphite in an organic solvent using ultrasonic waves, and obtaining doped graphene dispersed in the solvent; and applying a negative voltage between a counter electrode and a working electrode placed within the solvent in which the doped graphene is dispersed such that a graphene coating is formed at a surface of the working electrode.
The method of claim 8, wherein the dopant is one of HNO3, FeCl3, H₂SO4, and FTS.
The electrodeposited graphene obtained by the
The electrodeposited graphene obtained by the
The method of claim 1, wherein the dopant is voltage of -1.01 V.
- 22. 4 canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled FeCl3, and the negative voltage is -0.5 V or FeCl3, and the negative voltage is -1.5 V to -1.0 method of claim 1. withdrawn method of claim 8. withdrawn FeC l 3, and the applied voltage is a negative
Embodiments described in the patent, grouped by the materials and process steps they use.
9 materials1 process step
Preparation of dopants (HNO₃ 66%, FeCl₃ 98%, H₂SO₄ 99%, FTS, and 40 wt% butanol solution Baytron CB-40) and organic solvent acetonitrile (ACN, 98%). Graphite from Zaval'evsk coal field (Ukraine, ash content <0.05, particle size 200-300 µm) with C₂F~ClF₃ intercalated was used as expanded graphite. Doped graphene was obtained by p-doping expanded graphite with a Lewis acid dopant, dispersing in ACN by ultrasonication, then electrodepositing onto a PEDOT/gold working electrode using a Pt counter electrode and Ag/AgCl/KCl(sat'd) reference electrode at negative voltage (preferably -1.01 V for FeCl₃ dopant).
Materials described outside the worked examples.
platinum plate (counter electrode)
Pt
PEDOT-coated gold (working electrode)
Measurements and analyses referenced in the patent, with their drawing references.
Raman shift measured for graphene doped with each of FeCl3, FTS, HNO3, and H₂SO₄ (FIG. 2A-2D)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0–1 V | — |
Voltage |
Table 1
SVG
SVG 13546268.
p. 6
Table 2
SVG
3 is indicated in the following Table 2.
p. 7
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,133,562Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically illustrates a method of fabricating a graphene layer using electrodeposition. Expanded graphite was prepared, and was doped using a 20 …
FIG. 2D illustrates a Raman shift according to a dopant of H 2S04: 6 FIG 3 is a result of observing delta frequency by scanning at a rate of 10 mV/s in a range …
FIG. 3D is a graph illustrating a result of observing delta frequency according to a dopant of H 2S04. When the graphene was doped with FeC l 3 and FTS, it …
FIG. 4E illustrates graphene doped with H 2SO4. 13 Unlike smooth PEDOT, a rough PEDOT surface caused by the deposition of the graphene was observed. In …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Please CANCEL claims 15-22 without prejudice or disclaimer in accordance with the following:
The method of claim 1, wherein the dispersing is performed using an ultrasonic wave device.
The method of claim 1, wherein the electrodeposition is performed using a platinum plate as the counter electrode, PEDOT- coated gold as the working electrode, and Ag/AgC I/KCI(sat'd) as a reference electrode.
The method of claim 3, wherein the applied voltage is a negative voltage of -1.5 V to -1.0 V.
A method of electrodepositing graphene, comprising: p-doping expanded graphite using a dopant; dispersing the doped expanded graphite in an organic solvent using ultrasonic waves, and obtaining doped graphene dispersed in the solvent; and applying a negative voltage between a counter electrode and a working electrode placed within the solvent in which the doped graphene is dispersed such that a graphene coating is formed at a surface of the working electrode.
The method of claim 8, wherein the dopant is one of HNO3, FeCl3, H₂SO4, and FTS.
The electrodeposited graphene obtained by the
The electrodeposited graphene obtained by the
The method of claim 1, wherein the dopant is voltage of -1.01 V.
- 22. 4 canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled FeCl3, and the negative voltage is -0.5 V or FeCl3, and the negative voltage is -1.5 V to -1.0 method of claim 1. withdrawn method of claim 8. withdrawn FeC l 3, and the applied voltage is a negative
Embodiments described in the patent, grouped by the materials and process steps they use.
9 materials1 process step
Preparation of dopants (HNO₃ 66%, FeCl₃ 98%, H₂SO₄ 99%, FTS, and 40 wt% butanol solution Baytron CB-40) and organic solvent acetonitrile (ACN, 98%). Graphite from Zaval'evsk coal field (Ukraine, ash content <0.05, particle size 200-300 µm) with C₂F~ClF₃ intercalated was used as expanded graphite. Doped graphene was obtained by p-doping expanded graphite with a Lewis acid dopant, dispersing in ACN by ultrasonication, then electrodepositing onto a PEDOT/gold working electrode using a Pt counter electrode and Ag/AgCl/KCl(sat'd) reference electrode at negative voltage (preferably -1.01 V for FeCl₃ dopant).
Materials described outside the worked examples.
platinum plate (counter electrode)
Pt
PEDOT-coated gold (working electrode)
Measurements and analyses referenced in the patent, with their drawing references.
Raman shift measured for graphene doped with each of FeCl3, FTS, HNO3, and H₂SO₄ (FIG. 2A-2D)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0–1 V | — |
Voltage |
Table 1
SVG
SVG 13546268.
p. 6
Table 2
SVG
3 is indicated in the following Table 2.
p. 7
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,133,562Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically illustrates a method of fabricating a graphene layer using electrodeposition. Expanded graphite was prepared, and was doped using a 20 …
FIG. 2D illustrates a Raman shift according to a dopant of H 2S04: 6 FIG 3 is a result of observing delta frequency by scanning at a rate of 10 mV/s in a range …
FIG. 3D is a graph illustrating a result of observing delta frequency according to a dopant of H 2S04. When the graphene was doped with FeC l 3 and FTS, it …
FIG. 4E illustrates graphene doped with H 2SO4. 13 Unlike smooth PEDOT, a rough PEDOT surface caused by the deposition of the graphene was observed. In …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Please CANCEL claims 15-22 without prejudice or disclaimer in accordance with the following:
The method of claim 1, wherein the dispersing is performed using an ultrasonic wave device.
The method of claim 1, wherein the electrodeposition is performed using a platinum plate as the counter electrode, PEDOT- coated gold as the working electrode, and Ag/AgC I/KCI(sat'd) as a reference electrode.
The method of claim 3, wherein the applied voltage is a negative voltage of -1.5 V to -1.0 V.
A method of electrodepositing graphene, comprising: p-doping expanded graphite using a dopant; dispersing the doped expanded graphite in an organic solvent using ultrasonic waves, and obtaining doped graphene dispersed in the solvent; and applying a negative voltage between a counter electrode and a working electrode placed within the solvent in which the doped graphene is dispersed such that a graphene coating is formed at a surface of the working electrode.
The method of claim 8, wherein the dopant is one of HNO3, FeCl3, H₂SO4, and FTS.
The electrodeposited graphene obtained by the
The electrodeposited graphene obtained by the
The method of claim 1, wherein the dopant is voltage of -1.01 V.
- 22. 4 canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled FeCl3, and the negative voltage is -0.5 V or FeCl3, and the negative voltage is -1.5 V to -1.0 method of claim 1. withdrawn method of claim 8. withdrawn FeC l 3, and the applied voltage is a negative
Embodiments described in the patent, grouped by the materials and process steps they use.
9 materials1 process step
Preparation of dopants (HNO₃ 66%, FeCl₃ 98%, H₂SO₄ 99%, FTS, and 40 wt% butanol solution Baytron CB-40) and organic solvent acetonitrile (ACN, 98%). Graphite from Zaval'evsk coal field (Ukraine, ash content <0.05, particle size 200-300 µm) with C₂F~ClF₃ intercalated was used as expanded graphite. Doped graphene was obtained by p-doping expanded graphite with a Lewis acid dopant, dispersing in ACN by ultrasonication, then electrodepositing onto a PEDOT/gold working electrode using a Pt counter electrode and Ag/AgCl/KCl(sat'd) reference electrode at negative voltage (preferably -1.01 V for FeCl₃ dopant).
Materials described outside the worked examples.
platinum plate (counter electrode)
Pt
PEDOT-coated gold (working electrode)
Measurements and analyses referenced in the patent, with their drawing references.
Raman shift measured for graphene doped with each of FeCl3, FTS, HNO3, and H₂SO₄ (FIG. 2A-2D)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0–1 V | — |
Voltage |
Table 1
SVG
SVG 13546268.
p. 6
Table 2
SVG
3 is indicated in the following Table 2.
p. 7
Related documents with shared materials, methods, properties, or citations.
Ag/AgCl/KCl(sat'd) reference electrode
Delta frequency observed by scanning at 10 mV/s in range 0 to 2 V to confirm potential range for graphene deposition for each dopant (FIG. 3A-3D)
SEM images of graphene deposited on PEDOT/gold electrode for each dopant: PEDOT on gold (FIG. 4A), FeCl₃-doped graphene (FIG. 4B), FTS-doped graphene (FIG. 4C), HNO₃-doped graphene (FIG. 4D), H₂SO₄-doped graphene (FIG. 4E)
| — |
Thickness | 400–500 nm | — |
Ag/AgCl/KCl(sat'd) reference electrode
Delta frequency observed by scanning at 10 mV/s in range 0 to 2 V to confirm potential range for graphene deposition for each dopant (FIG. 3A-3D)
SEM images of graphene deposited on PEDOT/gold electrode for each dopant: PEDOT on gold (FIG. 4A), FeCl₃-doped graphene (FIG. 4B), FTS-doped graphene (FIG. 4C), HNO₃-doped graphene (FIG. 4D), H₂SO₄-doped graphene (FIG. 4E)
| — |
Thickness | 400–500 nm | — |
Ag/AgCl/KCl(sat'd) reference electrode
Delta frequency observed by scanning at 10 mV/s in range 0 to 2 V to confirm potential range for graphene deposition for each dopant (FIG. 3A-3D)
SEM images of graphene deposited on PEDOT/gold electrode for each dopant: PEDOT on gold (FIG. 4A), FeCl₃-doped graphene (FIG. 4B), FTS-doped graphene (FIG. 4C), HNO₃-doped graphene (FIG. 4D), H₂SO₄-doped graphene (FIG. 4E)
| — |
Thickness | 400–500 nm | — |
Ag/AgCl/KCl(sat'd) reference electrode
Delta frequency observed by scanning at 10 mV/s in range 0 to 2 V to confirm potential range for graphene deposition for each dopant (FIG. 3A-3D)
SEM images of graphene deposited on PEDOT/gold electrode for each dopant: PEDOT on gold (FIG. 4A), FeCl₃-doped graphene (FIG. 4B), FTS-doped graphene (FIG. 4C), HNO₃-doped graphene (FIG. 4D), H₂SO₄-doped graphene (FIG. 4E)
| — |
Thickness | 400–500 nm | — |