Patent
US 9,187,824Title: RAPID SYNTHESIS OF GRAPHENE AN D F ORMATION OF GRAPHENE STRUCTURES
Timothy S. Fisher, Anurag Kumar
PURDUE RESEARCH FOUNDATION·11 April 2013·US
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Patent
Atlas literature
Patent
US 9,187,824Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1-(a) A schematic diagram of an embodiment of a growth set up showing elevated sample within the hydrogen plasma. (b) A diagram showing different stages of …
FIG. 2-SEM image showing a Cu foil (a) before and (b) after growth. Formation of grains on the Cu foil after growth can be seen. (c) An optical image of the …
FIG. 3-(a) XPS survey spectrum of graphene film on Cu (b) High-resolution spectrum of the C 1 s region. The inset in
FIG. 4-(a) HRTEM image of few-layer graphene.(b) A transmission spectrum collected in the visible range for a graphene film transferred onto a glass slide.
FIG. 5-Raman spectra of graphene grown with different durations of CH₄ flow. A decrease in the D peak intensity with the extension of the CH₄ flow time is seen.
FIG. 6-(a) A high magnification SEM image showing graphene growth across a Cu grain boundary. (b) SEM image showing vertically standing carbon nanowalls …
FIG. 7-a schematic diagram showing the transfer process.
FIG. 8 shows a plurality of vertically aligned C NTs located between copper and silicon substrates. Two enlargements of the C NT-Si interface are shown. The …
FIG. 9-a schematic diagram showing the graphene CNT joint structure. 5 WO 2013/052939 PCT/US₂₀₁₂/05
FIG. 10. is a schematic of the temperature variation in an embodiment of the growth process as a function of time.
FIG. 11. shows Raman spectra of the graphene film with and without any nitrogen doping.
FIG. 12. is a SEM image of Cu foil (a) before and (b) after graphene growth.
FIG. 13. shows a high-resolution TEM image of the graphene film grown without any C H₄ flow.
FIG. 14. is a high-resolution image of graphene surface measured by a UHV STM at 90 K.
FIG. 15. shows XPS spectra of the doped graphene film: (a) Survey spectrum and high resolution spectrum of (b) C i s region (c) N i s region and (d) Cu2p …
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 graphene film synthesis, the method comprising: a. providing a copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. evacuating the chamber to approximately 2 Torr, d. providing hydrogen gas to the chamber, e. exposing the foil to plasma f. providing methane gas maintaining approximately 10 Torr in the chamber, wherein the foil is supported by a ceramic stud elevating the foil above a molybdenum puck.
The method of claim 1 wherein the hydrogen gas is high purity.
The method of claim 1 wherein providing hydrogen gas to the chamber includes raisin g the chamber pressure to approximately 10 Torr.
The method of claim 1 wherein the plasma is 400 W hydrogen plasma.
The method of claim 1 further comprising providing hydrogen gas to the chamber at approximately fifty standard cubic centimeters per minute.
The method of claim 1 wherein exposing the foil to plasma initially occurs for approximately three minutes.
The method of claim 1 further comprising providing methane gas to the chamber at approximately five standard cubic centimeters per minute.
1 4. The method of claim 1 wherein the synthesized graphene film is transferred by use of polymethyl methacrylate.
canceled
canceled
The method of claim [[3]] 1 wherein the foil is elevated above the puck by approximately fifteen millimeters.
A method of doped graphene film synthesis, the method comprising: a. providing an approximately 25 p m thick copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. elevating the foil above a molybdenum puck, d. evacuating the chamber to approximately 2 Torr, e. providing hydrogen gas, to the chamber, f. exposing the foil to 400 W plasma, g. providing methane gas, and nitrogen gas maintaining approximately 10 Page 4 of 8 App. No. 14/350,168 Response Dated Response to Non-compliant Amendment Dated and Office Action Dated Torr in the chamber.
The method of claim 15 wherein providing hydrogen gas to the chamber includes providing hydrogen gas at approximately fifty standard cubic centimeters per minute.
1 7. The method of claim 15 wherein exposing the foil to plasma includes initially exposing the foil to plasma for approximately three minutes.
The method of claim 15 wherein providing methane gas to the chamber includes providing methane gas at approximately five standard cubic centimeters per minute for approximately one minute.
1 9. The method of claim 15 wherein providing nitrogen gas to the chamber includes providing nitrogen gas at approximately fifty standard cubic centimeters per minute for approximately one minute.
Materials described outside the worked examples.
copper foil
Cu
hydrogen gas
H₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Nitrogen Concentration | up to approximately 2 atomic % | nitrogen-doped graphene film |
Thickness | 1.4–2.8 nm |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,187,824Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1-(a) A schematic diagram of an embodiment of a growth set up showing elevated sample within the hydrogen plasma. (b) A diagram showing different stages of …
FIG. 2-SEM image showing a Cu foil (a) before and (b) after growth. Formation of grains on the Cu foil after growth can be seen. (c) An optical image of the …
FIG. 3-(a) XPS survey spectrum of graphene film on Cu (b) High-resolution spectrum of the C 1 s region. The inset in
FIG. 4-(a) HRTEM image of few-layer graphene.(b) A transmission spectrum collected in the visible range for a graphene film transferred onto a glass slide.
FIG. 5-Raman spectra of graphene grown with different durations of CH₄ flow. A decrease in the D peak intensity with the extension of the CH₄ flow time is seen.
FIG. 6-(a) A high magnification SEM image showing graphene growth across a Cu grain boundary. (b) SEM image showing vertically standing carbon nanowalls …
FIG. 7-a schematic diagram showing the transfer process.
FIG. 8 shows a plurality of vertically aligned C NTs located between copper and silicon substrates. Two enlargements of the C NT-Si interface are shown. The …
FIG. 9-a schematic diagram showing the graphene CNT joint structure. 5 WO 2013/052939 PCT/US₂₀₁₂/05
FIG. 10. is a schematic of the temperature variation in an embodiment of the growth process as a function of time.
FIG. 11. shows Raman spectra of the graphene film with and without any nitrogen doping.
FIG. 12. is a SEM image of Cu foil (a) before and (b) after graphene growth.
FIG. 13. shows a high-resolution TEM image of the graphene film grown without any C H₄ flow.
FIG. 14. is a high-resolution image of graphene surface measured by a UHV STM at 90 K.
FIG. 15. shows XPS spectra of the doped graphene film: (a) Survey spectrum and high resolution spectrum of (b) C i s region (c) N i s region and (d) Cu2p …
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 graphene film synthesis, the method comprising: a. providing a copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. evacuating the chamber to approximately 2 Torr, d. providing hydrogen gas to the chamber, e. exposing the foil to plasma f. providing methane gas maintaining approximately 10 Torr in the chamber, wherein the foil is supported by a ceramic stud elevating the foil above a molybdenum puck.
The method of claim 1 wherein the hydrogen gas is high purity.
The method of claim 1 wherein providing hydrogen gas to the chamber includes raisin g the chamber pressure to approximately 10 Torr.
The method of claim 1 wherein the plasma is 400 W hydrogen plasma.
The method of claim 1 further comprising providing hydrogen gas to the chamber at approximately fifty standard cubic centimeters per minute.
The method of claim 1 wherein exposing the foil to plasma initially occurs for approximately three minutes.
The method of claim 1 further comprising providing methane gas to the chamber at approximately five standard cubic centimeters per minute.
1 4. The method of claim 1 wherein the synthesized graphene film is transferred by use of polymethyl methacrylate.
canceled
canceled
The method of claim [[3]] 1 wherein the foil is elevated above the puck by approximately fifteen millimeters.
A method of doped graphene film synthesis, the method comprising: a. providing an approximately 25 p m thick copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. elevating the foil above a molybdenum puck, d. evacuating the chamber to approximately 2 Torr, e. providing hydrogen gas, to the chamber, f. exposing the foil to 400 W plasma, g. providing methane gas, and nitrogen gas maintaining approximately 10 Page 4 of 8 App. No. 14/350,168 Response Dated Response to Non-compliant Amendment Dated and Office Action Dated Torr in the chamber.
The method of claim 15 wherein providing hydrogen gas to the chamber includes providing hydrogen gas at approximately fifty standard cubic centimeters per minute.
1 7. The method of claim 15 wherein exposing the foil to plasma includes initially exposing the foil to plasma for approximately three minutes.
The method of claim 15 wherein providing methane gas to the chamber includes providing methane gas at approximately five standard cubic centimeters per minute for approximately one minute.
1 9. The method of claim 15 wherein providing nitrogen gas to the chamber includes providing nitrogen gas at approximately fifty standard cubic centimeters per minute for approximately one minute.
Materials described outside the worked examples.
copper foil
Cu
hydrogen gas
H₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Nitrogen Concentration | up to approximately 2 atomic % | nitrogen-doped graphene film |
Thickness | 1.4–2.8 nm |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,187,824Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1-(a) A schematic diagram of an embodiment of a growth set up showing elevated sample within the hydrogen plasma. (b) A diagram showing different stages of …
FIG. 2-SEM image showing a Cu foil (a) before and (b) after growth. Formation of grains on the Cu foil after growth can be seen. (c) An optical image of the …
FIG. 3-(a) XPS survey spectrum of graphene film on Cu (b) High-resolution spectrum of the C 1 s region. The inset in
FIG. 4-(a) HRTEM image of few-layer graphene.(b) A transmission spectrum collected in the visible range for a graphene film transferred onto a glass slide.
FIG. 5-Raman spectra of graphene grown with different durations of CH₄ flow. A decrease in the D peak intensity with the extension of the CH₄ flow time is seen.
FIG. 6-(a) A high magnification SEM image showing graphene growth across a Cu grain boundary. (b) SEM image showing vertically standing carbon nanowalls …
FIG. 7-a schematic diagram showing the transfer process.
FIG. 8 shows a plurality of vertically aligned C NTs located between copper and silicon substrates. Two enlargements of the C NT-Si interface are shown. The …
FIG. 9-a schematic diagram showing the graphene CNT joint structure. 5 WO 2013/052939 PCT/US₂₀₁₂/05
FIG. 10. is a schematic of the temperature variation in an embodiment of the growth process as a function of time.
FIG. 11. shows Raman spectra of the graphene film with and without any nitrogen doping.
FIG. 12. is a SEM image of Cu foil (a) before and (b) after graphene growth.
FIG. 13. shows a high-resolution TEM image of the graphene film grown without any C H₄ flow.
FIG. 14. is a high-resolution image of graphene surface measured by a UHV STM at 90 K.
FIG. 15. shows XPS spectra of the doped graphene film: (a) Survey spectrum and high resolution spectrum of (b) C i s region (c) N i s region and (d) Cu2p …
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 graphene film synthesis, the method comprising: a. providing a copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. evacuating the chamber to approximately 2 Torr, d. providing hydrogen gas to the chamber, e. exposing the foil to plasma f. providing methane gas maintaining approximately 10 Torr in the chamber, wherein the foil is supported by a ceramic stud elevating the foil above a molybdenum puck.
The method of claim 1 wherein the hydrogen gas is high purity.
The method of claim 1 wherein providing hydrogen gas to the chamber includes raisin g the chamber pressure to approximately 10 Torr.
The method of claim 1 wherein the plasma is 400 W hydrogen plasma.
The method of claim 1 further comprising providing hydrogen gas to the chamber at approximately fifty standard cubic centimeters per minute.
The method of claim 1 wherein exposing the foil to plasma initially occurs for approximately three minutes.
The method of claim 1 further comprising providing methane gas to the chamber at approximately five standard cubic centimeters per minute.
1 4. The method of claim 1 wherein the synthesized graphene film is transferred by use of polymethyl methacrylate.
canceled
canceled
The method of claim [[3]] 1 wherein the foil is elevated above the puck by approximately fifteen millimeters.
A method of doped graphene film synthesis, the method comprising: a. providing an approximately 25 p m thick copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. elevating the foil above a molybdenum puck, d. evacuating the chamber to approximately 2 Torr, e. providing hydrogen gas, to the chamber, f. exposing the foil to 400 W plasma, g. providing methane gas, and nitrogen gas maintaining approximately 10 Page 4 of 8 App. No. 14/350,168 Response Dated Response to Non-compliant Amendment Dated and Office Action Dated Torr in the chamber.
The method of claim 15 wherein providing hydrogen gas to the chamber includes providing hydrogen gas at approximately fifty standard cubic centimeters per minute.
1 7. The method of claim 15 wherein exposing the foil to plasma includes initially exposing the foil to plasma for approximately three minutes.
The method of claim 15 wherein providing methane gas to the chamber includes providing methane gas at approximately five standard cubic centimeters per minute for approximately one minute.
1 9. The method of claim 15 wherein providing nitrogen gas to the chamber includes providing nitrogen gas at approximately fifty standard cubic centimeters per minute for approximately one minute.
Materials described outside the worked examples.
copper foil
Cu
hydrogen gas
H₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Nitrogen Concentration | up to approximately 2 atomic % | nitrogen-doped graphene film |
Thickness | 1.4–2.8 nm |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,187,824Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1-(a) A schematic diagram of an embodiment of a growth set up showing elevated sample within the hydrogen plasma. (b) A diagram showing different stages of …
FIG. 2-SEM image showing a Cu foil (a) before and (b) after growth. Formation of grains on the Cu foil after growth can be seen. (c) An optical image of the …
FIG. 3-(a) XPS survey spectrum of graphene film on Cu (b) High-resolution spectrum of the C 1 s region. The inset in
FIG. 4-(a) HRTEM image of few-layer graphene.(b) A transmission spectrum collected in the visible range for a graphene film transferred onto a glass slide.
FIG. 5-Raman spectra of graphene grown with different durations of CH₄ flow. A decrease in the D peak intensity with the extension of the CH₄ flow time is seen.
FIG. 6-(a) A high magnification SEM image showing graphene growth across a Cu grain boundary. (b) SEM image showing vertically standing carbon nanowalls …
FIG. 7-a schematic diagram showing the transfer process.
FIG. 8 shows a plurality of vertically aligned C NTs located between copper and silicon substrates. Two enlargements of the C NT-Si interface are shown. The …
FIG. 9-a schematic diagram showing the graphene CNT joint structure. 5 WO 2013/052939 PCT/US₂₀₁₂/05
FIG. 10. is a schematic of the temperature variation in an embodiment of the growth process as a function of time.
FIG. 11. shows Raman spectra of the graphene film with and without any nitrogen doping.
FIG. 12. is a SEM image of Cu foil (a) before and (b) after graphene growth.
FIG. 13. shows a high-resolution TEM image of the graphene film grown without any C H₄ flow.
FIG. 14. is a high-resolution image of graphene surface measured by a UHV STM at 90 K.
FIG. 15. shows XPS spectra of the doped graphene film: (a) Survey spectrum and high resolution spectrum of (b) C i s region (c) N i s region and (d) Cu2p …
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 graphene film synthesis, the method comprising: a. providing a copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. evacuating the chamber to approximately 2 Torr, d. providing hydrogen gas to the chamber, e. exposing the foil to plasma f. providing methane gas maintaining approximately 10 Torr in the chamber, wherein the foil is supported by a ceramic stud elevating the foil above a molybdenum puck.
The method of claim 1 wherein the hydrogen gas is high purity.
The method of claim 1 wherein providing hydrogen gas to the chamber includes raisin g the chamber pressure to approximately 10 Torr.
The method of claim 1 wherein the plasma is 400 W hydrogen plasma.
The method of claim 1 further comprising providing hydrogen gas to the chamber at approximately fifty standard cubic centimeters per minute.
The method of claim 1 wherein exposing the foil to plasma initially occurs for approximately three minutes.
The method of claim 1 further comprising providing methane gas to the chamber at approximately five standard cubic centimeters per minute.
1 4. The method of claim 1 wherein the synthesized graphene film is transferred by use of polymethyl methacrylate.
canceled
canceled
The method of claim [[3]] 1 wherein the foil is elevated above the puck by approximately fifteen millimeters.
A method of doped graphene film synthesis, the method comprising: a. providing an approximately 25 p m thick copper foil, b. placing the foil in a microwave plasma chemical vapor deposition chamber, c. elevating the foil above a molybdenum puck, d. evacuating the chamber to approximately 2 Torr, e. providing hydrogen gas, to the chamber, f. exposing the foil to 400 W plasma, g. providing methane gas, and nitrogen gas maintaining approximately 10 Page 4 of 8 App. No. 14/350,168 Response Dated Response to Non-compliant Amendment Dated and Office Action Dated Torr in the chamber.
The method of claim 15 wherein providing hydrogen gas to the chamber includes providing hydrogen gas at approximately fifty standard cubic centimeters per minute.
1 7. The method of claim 15 wherein exposing the foil to plasma includes initially exposing the foil to plasma for approximately three minutes.
The method of claim 15 wherein providing methane gas to the chamber includes providing methane gas at approximately five standard cubic centimeters per minute for approximately one minute.
1 9. The method of claim 15 wherein providing nitrogen gas to the chamber includes providing nitrogen gas at approximately fifty standard cubic centimeters per minute for approximately one minute.
Materials described outside the worked examples.
copper foil
Cu
hydrogen gas
H₂
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Nitrogen Concentration | up to approximately 2 atomic % | nitrogen-doped graphene film |
Thickness | 1.4–2.8 nm |
Related documents with shared materials, methods, properties, or citations.
methane gas
CH₄
molybdenum puck
Mo
graphene film
polymethyl methacrylate
nitrogen gas
N₂
nitrogen-doped graphene film
few-layer graphene
| — |
Duration | 30–60 sec | — |
Duration | ≤ 5 minutes | — |
Duration | ≥ 300 sec | — |
Pressure | ≥ 5 Torr | — |
Duration | 2–3 minutes | — |
GRAPHENE AND ITS GROWTH
methane gas
CH₄
molybdenum puck
Mo
graphene film
polymethyl methacrylate
nitrogen gas
N₂
nitrogen-doped graphene film
few-layer graphene
| — |
Duration | 30–60 sec | — |
Duration | ≤ 5 minutes | — |
Duration | ≥ 300 sec | — |
Pressure | ≥ 5 Torr | — |
Duration | 2–3 minutes | — |
GRAPHENE AND ITS GROWTH
methane gas
CH₄
molybdenum puck
Mo
graphene film
polymethyl methacrylate
nitrogen gas
N₂
nitrogen-doped graphene film
few-layer graphene
| — |
Duration | 30–60 sec | — |
Duration | ≤ 5 minutes | — |
Duration | ≥ 300 sec | — |
Pressure | ≥ 5 Torr | — |
Duration | 2–3 minutes | — |
GRAPHENE AND ITS GROWTH
methane gas
CH₄
molybdenum puck
Mo
graphene film
polymethyl methacrylate
nitrogen gas
N₂
nitrogen-doped graphene film
few-layer graphene
| — |
Duration | 30–60 sec | — |
Duration | ≤ 5 minutes | — |
Duration | ≥ 300 sec | — |
Pressure | ≥ 5 Torr | — |
Duration | 2–3 minutes | — |
GRAPHENE AND ITS GROWTH