Patent
US 8,388,924METHOD FOR GROWTH OF HIGH QUALITY GRAPHENE FILMS
Gouri Radhakrishnan
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 8,388,924Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an illustration of a reactor for preparing a graphene film according to embodiments of the method herein. [0008]
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
FIGS. 6A-6D are selected area electron diffraction patterns of two hexagon spot patterns at location 13 of the graphene film of Fig. 3 B and graphs of the …
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 forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through a methanol liquid precursor to bring the methanol liquid precursor into contact with the substrate for a time sufficient to form a graphene film, wherein the ratio of the buffer gas partial pressure to the methanol liquid precursor partial pressure is from ab e t 50:1 to ab et 2:1, wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 1, wherein the step of heating the reactor comprises heating the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point.
The method of claim 1, further comprising annealing the substrate by heating and maintaining the reactor at a temperature from ab e t 900 ° C to ab et 1200° C and thereafter heating or cooling the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point prior to passing the buffer gas through the methanol liquid precursor.
The method of claim 1, further comprising cooling the graphene film disposed on the substrate to about room temperature.
The method of claim 1, wherein the buffer gas has a flow rate of about at a flow rate from about 100 seem to about 500 seem.
The method of claim 1, wherein the buffer gas comprises argon.
The method of claim 1, wherein the buffer gas is substantially free of hydrogen gas (H₂).
The method of claim 1, wherein the substrate comprises copper or nickel.
The method of claim 1, wherein the time sufficient to form the graphene film is about 20 minutes.
The method of claim 1, wherein the graphene film comprises a grain size from about 10 to about 30 pm2.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 4.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 5.
The method of claim 1, wherein the substrate has a thickness from about 50 nm to about gm.
A method of forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas by reducing the reactor pressure to a pressure from ab et 1 mT orr to abe t 40 mT orr; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through an oxygen-containing hydrocarbon liquid precursor to bring the oxygen-containing hydrocarbon liquid precursor into contact with the substrate for a time sufficient to form a graphene film, 19483652.1 2 U.S.S.N. 13/091,701 Docket No. 11390-0069 (D-703) Filed: AMENDMENT AND RESPONSE TO OFFICE ACTION wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 2, wherein the reactor is pumped down to a pressure of ab et 10 m T orr to abet 40 m T orr.
. canceled
. canceled
. canceled
Materials described outside the worked examples.
graphene film
methanol
CH₃OH
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene grain size (claimed range) | 10–30 µm² | graphene film |
Raman G'/G intensity ratio (claimed minimum, claim 17) | ≥ 4 dimensionless |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,388,924Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an illustration of a reactor for preparing a graphene film according to embodiments of the method herein. [0008]
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
FIGS. 6A-6D are selected area electron diffraction patterns of two hexagon spot patterns at location 13 of the graphene film of Fig. 3 B and graphs of the …
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 forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through a methanol liquid precursor to bring the methanol liquid precursor into contact with the substrate for a time sufficient to form a graphene film, wherein the ratio of the buffer gas partial pressure to the methanol liquid precursor partial pressure is from ab e t 50:1 to ab et 2:1, wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 1, wherein the step of heating the reactor comprises heating the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point.
The method of claim 1, further comprising annealing the substrate by heating and maintaining the reactor at a temperature from ab e t 900 ° C to ab et 1200° C and thereafter heating or cooling the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point prior to passing the buffer gas through the methanol liquid precursor.
The method of claim 1, further comprising cooling the graphene film disposed on the substrate to about room temperature.
The method of claim 1, wherein the buffer gas has a flow rate of about at a flow rate from about 100 seem to about 500 seem.
The method of claim 1, wherein the buffer gas comprises argon.
The method of claim 1, wherein the buffer gas is substantially free of hydrogen gas (H₂).
The method of claim 1, wherein the substrate comprises copper or nickel.
The method of claim 1, wherein the time sufficient to form the graphene film is about 20 minutes.
The method of claim 1, wherein the graphene film comprises a grain size from about 10 to about 30 pm2.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 4.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 5.
The method of claim 1, wherein the substrate has a thickness from about 50 nm to about gm.
A method of forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas by reducing the reactor pressure to a pressure from ab et 1 mT orr to abe t 40 mT orr; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through an oxygen-containing hydrocarbon liquid precursor to bring the oxygen-containing hydrocarbon liquid precursor into contact with the substrate for a time sufficient to form a graphene film, 19483652.1 2 U.S.S.N. 13/091,701 Docket No. 11390-0069 (D-703) Filed: AMENDMENT AND RESPONSE TO OFFICE ACTION wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 2, wherein the reactor is pumped down to a pressure of ab et 10 m T orr to abet 40 m T orr.
. canceled
. canceled
. canceled
Materials described outside the worked examples.
graphene film
methanol
CH₃OH
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene grain size (claimed range) | 10–30 µm² | graphene film |
Raman G'/G intensity ratio (claimed minimum, claim 17) | ≥ 4 dimensionless |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,388,924Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an illustration of a reactor for preparing a graphene film according to embodiments of the method herein. [0008]
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
FIGS. 6A-6D are selected area electron diffraction patterns of two hexagon spot patterns at location 13 of the graphene film of Fig. 3 B and graphs of the …
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 forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through a methanol liquid precursor to bring the methanol liquid precursor into contact with the substrate for a time sufficient to form a graphene film, wherein the ratio of the buffer gas partial pressure to the methanol liquid precursor partial pressure is from ab e t 50:1 to ab et 2:1, wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 1, wherein the step of heating the reactor comprises heating the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point.
The method of claim 1, further comprising annealing the substrate by heating and maintaining the reactor at a temperature from ab e t 900 ° C to ab et 1200° C and thereafter heating or cooling the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point prior to passing the buffer gas through the methanol liquid precursor.
The method of claim 1, further comprising cooling the graphene film disposed on the substrate to about room temperature.
The method of claim 1, wherein the buffer gas has a flow rate of about at a flow rate from about 100 seem to about 500 seem.
The method of claim 1, wherein the buffer gas comprises argon.
The method of claim 1, wherein the buffer gas is substantially free of hydrogen gas (H₂).
The method of claim 1, wherein the substrate comprises copper or nickel.
The method of claim 1, wherein the time sufficient to form the graphene film is about 20 minutes.
The method of claim 1, wherein the graphene film comprises a grain size from about 10 to about 30 pm2.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 4.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 5.
The method of claim 1, wherein the substrate has a thickness from about 50 nm to about gm.
A method of forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas by reducing the reactor pressure to a pressure from ab et 1 mT orr to abe t 40 mT orr; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through an oxygen-containing hydrocarbon liquid precursor to bring the oxygen-containing hydrocarbon liquid precursor into contact with the substrate for a time sufficient to form a graphene film, 19483652.1 2 U.S.S.N. 13/091,701 Docket No. 11390-0069 (D-703) Filed: AMENDMENT AND RESPONSE TO OFFICE ACTION wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 2, wherein the reactor is pumped down to a pressure of ab et 10 m T orr to abet 40 m T orr.
. canceled
. canceled
. canceled
Materials described outside the worked examples.
graphene film
methanol
CH₃OH
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene grain size (claimed range) | 10–30 µm² | graphene film |
Raman G'/G intensity ratio (claimed minimum, claim 17) | ≥ 4 dimensionless |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,388,924Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an illustration of a reactor for preparing a graphene film according to embodiments of the method herein. [0008]
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
FIGS. 6A-6D are selected area electron diffraction patterns of two hexagon spot patterns at location 13 of the graphene film of Fig. 3 B and graphs of the …
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 forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through a methanol liquid precursor to bring the methanol liquid precursor into contact with the substrate for a time sufficient to form a graphene film, wherein the ratio of the buffer gas partial pressure to the methanol liquid precursor partial pressure is from ab e t 50:1 to ab et 2:1, wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 1, wherein the step of heating the reactor comprises heating the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point.
The method of claim 1, further comprising annealing the substrate by heating and maintaining the reactor at a temperature from ab e t 900 ° C to ab et 1200° C and thereafter heating or cooling the reactor to a temperature that is sufficient for decomposition of the methanol liquid precursor and less than the substrate melting point prior to passing the buffer gas through the methanol liquid precursor.
The method of claim 1, further comprising cooling the graphene film disposed on the substrate to about room temperature.
The method of claim 1, wherein the buffer gas has a flow rate of about at a flow rate from about 100 seem to about 500 seem.
The method of claim 1, wherein the buffer gas comprises argon.
The method of claim 1, wherein the buffer gas is substantially free of hydrogen gas (H₂).
The method of claim 1, wherein the substrate comprises copper or nickel.
The method of claim 1, wherein the time sufficient to form the graphene film is about 20 minutes.
The method of claim 1, wherein the graphene film comprises a grain size from about 10 to about 30 pm2.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 4.
The method of claim 1, wherein the ratio of the intensities of G':G peaks as measured from a Raman Spectrum of the graphene film is at least 5.
The method of claim 1, wherein the substrate has a thickness from about 50 nm to about gm.
A method of forming a graphene film comprising: replacing at least a portion of air in a reactor having a substrate disposed therein with a buffer gas by reducing the reactor pressure to a pressure from ab et 1 mT orr to abe t 40 mT orr; flowing the buffer gas through the reactor and heating the reactor; and passing the buffer gas through an oxygen-containing hydrocarbon liquid precursor to bring the oxygen-containing hydrocarbon liquid precursor into contact with the substrate for a time sufficient to form a graphene film, 19483652.1 2 U.S.S.N. 13/091,701 Docket No. 11390-0069 (D-703) Filed: AMENDMENT AND RESPONSE TO OFFICE ACTION wherein the graphene film is a single-layer comprising a single grain continuity of at least 1 m2.
The method of claim 2, wherein the reactor is pumped down to a pressure of ab et 10 m T orr to abet 40 m T orr.
. canceled
. canceled
. canceled
Materials described outside the worked examples.
graphene film
methanol
CH₃OH
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene grain size (claimed range) | 10–30 µm² | graphene film |
Raman G'/G intensity ratio (claimed minimum, claim 17) | ≥ 4 dimensionless |
Related documents with shared materials, methods, properties, or citations.
buffer gas
oxygen-containing hydrocarbon liquid precursor
argon
Ar
copper
Cu
nickel
Ni
ethanol
C₂H₅OH
iso-propanol
C₃H₇OH
acetone
C₃H₆O
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
Raman G'/G intensity ratio (claimed minimum, claim 18) | ≥ 5 dimensionless | graphene film |
Pressure | 55–60 Torr | — |
Temperature | 23–25 °C | — |
Duration | 15–20 minutes | — |
Thickness | 20–35 cm | — |
Temperature | 600–1200 °C | — |
Temperature | 1000–1200 °C | — |
Duration | 5–30 minutes | — |
Duration | 10–25 minutes | — |
Temperature | 15–25 °C | — |
buffer gas
oxygen-containing hydrocarbon liquid precursor
argon
Ar
copper
Cu
nickel
Ni
ethanol
C₂H₅OH
iso-propanol
C₃H₇OH
acetone
C₃H₆O
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
Raman G'/G intensity ratio (claimed minimum, claim 18) | ≥ 5 dimensionless | graphene film |
Pressure | 55–60 Torr | — |
Temperature | 23–25 °C | — |
Duration | 15–20 minutes | — |
Thickness | 20–35 cm | — |
Temperature | 600–1200 °C | — |
Temperature | 1000–1200 °C | — |
Duration | 5–30 minutes | — |
Duration | 10–25 minutes | — |
Temperature | 15–25 °C | — |
buffer gas
oxygen-containing hydrocarbon liquid precursor
argon
Ar
copper
Cu
nickel
Ni
ethanol
C₂H₅OH
iso-propanol
C₃H₇OH
acetone
C₃H₆O
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
Raman G'/G intensity ratio (claimed minimum, claim 18) | ≥ 5 dimensionless | graphene film |
Pressure | 55–60 Torr | — |
Temperature | 23–25 °C | — |
Duration | 15–20 minutes | — |
Thickness | 20–35 cm | — |
Temperature | 600–1200 °C | — |
Temperature | 1000–1200 °C | — |
Duration | 5–30 minutes | — |
Duration | 10–25 minutes | — |
Temperature | 15–25 °C | — |
buffer gas
oxygen-containing hydrocarbon liquid precursor
argon
Ar
copper
Cu
nickel
Ni
ethanol
C₂H₅OH
iso-propanol
C₃H₇OH
acetone
C₃H₆O
FIGS. 2A-2C are Raman Spectrum of a graphene film on copper (2A), of a graphene film transferred to a holey-C TEM grid (2 B), and of a graphene film transferred …
FIGS. 3A and 3 B are transmission electron microscopy (TEM) of a graphene film on a holey-C grid. [0010]
FIGS. 4A-4C are selected area electron diffraction patterns taken in a TEM at individual hole locations of the graphene film of
FIGS. 5A and 5 B are the selected area electron diffraction pattern at location 4 of the graphene film of Fig. 3 B and the graph of the intensities at spots from …
Raman G'/G intensity ratio (claimed minimum, claim 18) | ≥ 5 dimensionless | graphene film |
Pressure | 55–60 Torr | — |
Temperature | 23–25 °C | — |
Duration | 15–20 minutes | — |
Thickness | 20–35 cm | — |
Temperature | 600–1200 °C | — |
Temperature | 1000–1200 °C | — |
Duration | 5–30 minutes | — |
Duration | 10–25 minutes | — |
Temperature | 15–25 °C | — |