Patent
US 9,691,612Process for Preparing Graphene on a SiC Substrate Based on Metal Film-Assisted Annealing
Hui Guo
US
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Patent
Atlas literature
Patent
US 9,691,612Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic view of the device used to prepare graphene in accordance with the present invention.
Figure 2 is a flow diagram schematically representing the process for preparing graphene in accordance with the present invention.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
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A process for preparing graphene on a SiC substrate, based on metal film- assisted annealing, comprising the following steps: (1) subjecting a SiC substrate to a standard cleaning process so as to remove contaminants from the surface of the SiC substrate; (2) placing the cleaned SiC substrate into a quartz tube and heating the quartz tube up to a temperature of 750 to 1150 ° C; and introducing CC 1 4 vapor into the quartz tube to react with SiC for a period of 20 to 100 minutes so as to generate a double-layered carbon film, wherein the CC 4 vapor is carried by Ar gas; (3) forming a metal film with a thickness of 350 to 600 nm on a Si substrate by electron beam deposition, wherein the metal film is capable of catalyzing carbon to reconstitute into graphene; (4) placing the obtained double-layered carbon film sample onto the metal film, and subsequently annealing them in an Ar atmosphere at a temperature of 900 to 1100 C for 10-30 minutes so as to reconstitute the double-layered carbon film into double-layered graphene; and (5) removing the metal film from the double-layered graphene, and thereby obtaining double-layered graphene. 2 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 913-0001
The process for preparing graphene according to claim 10, characterized in that step (1) subjecting a SiC substrate to a standard cleaning process is carried out by: (l a) immersing the SiC substrate in a medium of NH 4 0H+H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove organic residues from the surface of the SiC substrate; and (l b) immersing the SiC substrate in a medium of HC l +H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove ionic contaminants.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas in step (2) is 40 to 90 ml/min.
The process for preparing graphene according to claim 10, characterized in that the electron beam deposition in step (3) is carried out under the following conditions: the distance between the SiC substrate and the target being 50 cm, the chamber pressure being 5 x 10- 4 Pa, the beam current being 40mA, and the evaporation time being 10 to 20 minutes.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas during annealing in step (4) is 20-1 00ml/min.
The process for preparing graphene according to claim 10, characterized in that the SiC substrate is in a crystal form of 4H-SiC or 6H-SiC. 3 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 9130001
The process for preparing graphene according to claim 10, characterized in that the CC l 4 vapor in step (2) is obtained by heating CCl₄ liquid to a temperature of 60 to 90°C.
The process for preparing graphene according to claim 10, characterized in that the metal film is a Ni film.
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Materials described outside the worked examples.
double-layered graphene
SiC substrate
SiC
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 20–100 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,691,612Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic view of the device used to prepare graphene in accordance with the present invention.
Figure 2 is a flow diagram schematically representing the process for preparing graphene in accordance with the present invention.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-9. canceled
canceled
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A process for preparing graphene on a SiC substrate, based on metal film- assisted annealing, comprising the following steps: (1) subjecting a SiC substrate to a standard cleaning process so as to remove contaminants from the surface of the SiC substrate; (2) placing the cleaned SiC substrate into a quartz tube and heating the quartz tube up to a temperature of 750 to 1150 ° C; and introducing CC 1 4 vapor into the quartz tube to react with SiC for a period of 20 to 100 minutes so as to generate a double-layered carbon film, wherein the CC 4 vapor is carried by Ar gas; (3) forming a metal film with a thickness of 350 to 600 nm on a Si substrate by electron beam deposition, wherein the metal film is capable of catalyzing carbon to reconstitute into graphene; (4) placing the obtained double-layered carbon film sample onto the metal film, and subsequently annealing them in an Ar atmosphere at a temperature of 900 to 1100 C for 10-30 minutes so as to reconstitute the double-layered carbon film into double-layered graphene; and (5) removing the metal film from the double-layered graphene, and thereby obtaining double-layered graphene. 2 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 913-0001
The process for preparing graphene according to claim 10, characterized in that step (1) subjecting a SiC substrate to a standard cleaning process is carried out by: (l a) immersing the SiC substrate in a medium of NH 4 0H+H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove organic residues from the surface of the SiC substrate; and (l b) immersing the SiC substrate in a medium of HC l +H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove ionic contaminants.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas in step (2) is 40 to 90 ml/min.
The process for preparing graphene according to claim 10, characterized in that the electron beam deposition in step (3) is carried out under the following conditions: the distance between the SiC substrate and the target being 50 cm, the chamber pressure being 5 x 10- 4 Pa, the beam current being 40mA, and the evaporation time being 10 to 20 minutes.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas during annealing in step (4) is 20-1 00ml/min.
The process for preparing graphene according to claim 10, characterized in that the SiC substrate is in a crystal form of 4H-SiC or 6H-SiC. 3 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 9130001
The process for preparing graphene according to claim 10, characterized in that the CC l 4 vapor in step (2) is obtained by heating CCl₄ liquid to a temperature of 60 to 90°C.
The process for preparing graphene according to claim 10, characterized in that the metal film is a Ni film.
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Materials described outside the worked examples.
double-layered graphene
SiC substrate
SiC
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 20–100 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,691,612Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic view of the device used to prepare graphene in accordance with the present invention.
Figure 2 is a flow diagram schematically representing the process for preparing graphene in accordance with the present invention.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-9. canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled
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A process for preparing graphene on a SiC substrate, based on metal film- assisted annealing, comprising the following steps: (1) subjecting a SiC substrate to a standard cleaning process so as to remove contaminants from the surface of the SiC substrate; (2) placing the cleaned SiC substrate into a quartz tube and heating the quartz tube up to a temperature of 750 to 1150 ° C; and introducing CC 1 4 vapor into the quartz tube to react with SiC for a period of 20 to 100 minutes so as to generate a double-layered carbon film, wherein the CC 4 vapor is carried by Ar gas; (3) forming a metal film with a thickness of 350 to 600 nm on a Si substrate by electron beam deposition, wherein the metal film is capable of catalyzing carbon to reconstitute into graphene; (4) placing the obtained double-layered carbon film sample onto the metal film, and subsequently annealing them in an Ar atmosphere at a temperature of 900 to 1100 C for 10-30 minutes so as to reconstitute the double-layered carbon film into double-layered graphene; and (5) removing the metal film from the double-layered graphene, and thereby obtaining double-layered graphene. 2 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 913-0001
The process for preparing graphene according to claim 10, characterized in that step (1) subjecting a SiC substrate to a standard cleaning process is carried out by: (l a) immersing the SiC substrate in a medium of NH 4 0H+H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove organic residues from the surface of the SiC substrate; and (l b) immersing the SiC substrate in a medium of HC l +H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove ionic contaminants.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas in step (2) is 40 to 90 ml/min.
The process for preparing graphene according to claim 10, characterized in that the electron beam deposition in step (3) is carried out under the following conditions: the distance between the SiC substrate and the target being 50 cm, the chamber pressure being 5 x 10- 4 Pa, the beam current being 40mA, and the evaporation time being 10 to 20 minutes.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas during annealing in step (4) is 20-1 00ml/min.
The process for preparing graphene according to claim 10, characterized in that the SiC substrate is in a crystal form of 4H-SiC or 6H-SiC. 3 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 9130001
The process for preparing graphene according to claim 10, characterized in that the CC l 4 vapor in step (2) is obtained by heating CCl₄ liquid to a temperature of 60 to 90°C.
The process for preparing graphene according to claim 10, characterized in that the metal film is a Ni film.
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canceled
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Materials described outside the worked examples.
double-layered graphene
SiC substrate
SiC
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 20–100 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,691,612Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic view of the device used to prepare graphene in accordance with the present invention.
Figure 2 is a flow diagram schematically representing the process for preparing graphene in accordance with the present invention.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-9. canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled
canceled
A process for preparing graphene on a SiC substrate, based on metal film- assisted annealing, comprising the following steps: (1) subjecting a SiC substrate to a standard cleaning process so as to remove contaminants from the surface of the SiC substrate; (2) placing the cleaned SiC substrate into a quartz tube and heating the quartz tube up to a temperature of 750 to 1150 ° C; and introducing CC 1 4 vapor into the quartz tube to react with SiC for a period of 20 to 100 minutes so as to generate a double-layered carbon film, wherein the CC 4 vapor is carried by Ar gas; (3) forming a metal film with a thickness of 350 to 600 nm on a Si substrate by electron beam deposition, wherein the metal film is capable of catalyzing carbon to reconstitute into graphene; (4) placing the obtained double-layered carbon film sample onto the metal film, and subsequently annealing them in an Ar atmosphere at a temperature of 900 to 1100 C for 10-30 minutes so as to reconstitute the double-layered carbon film into double-layered graphene; and (5) removing the metal film from the double-layered graphene, and thereby obtaining double-layered graphene. 2 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 913-0001
The process for preparing graphene according to claim 10, characterized in that step (1) subjecting a SiC substrate to a standard cleaning process is carried out by: (l a) immersing the SiC substrate in a medium of NH 4 0H+H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove organic residues from the surface of the SiC substrate; and (l b) immersing the SiC substrate in a medium of HC l +H 2 O 2 for 10 minutes, taking the SiC substrate out and drying it so as to remove ionic contaminants.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas in step (2) is 40 to 90 ml/min.
The process for preparing graphene according to claim 10, characterized in that the electron beam deposition in step (3) is carried out under the following conditions: the distance between the SiC substrate and the target being 50 cm, the chamber pressure being 5 x 10- 4 Pa, the beam current being 40mA, and the evaporation time being 10 to 20 minutes.
The process for preparing graphene according to claim 10, characterized in that the flow rate of Ar gas during annealing in step (4) is 20-1 00ml/min.
The process for preparing graphene according to claim 10, characterized in that the SiC substrate is in a crystal form of 4H-SiC or 6H-SiC. 3 MCDONNELL BOEHNEN HULBERT & BERGHOFF LLP 300 SOUTH WACKER DRIVE CHICAGO, ILLINOIS 60606 TELEPHONE (312) 9130001
The process for preparing graphene according to claim 10, characterized in that the CC l 4 vapor in step (2) is obtained by heating CCl₄ liquid to a temperature of 60 to 90°C.
The process for preparing graphene according to claim 10, characterized in that the metal film is a Ni film.
18-25. canceled
canceled
canceled
canceled
canceled
canceled
Materials described outside the worked examples.
double-layered graphene
SiC substrate
SiC
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 3 is a SEM photograph of the graphene in accordance with the present invention.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 20–100 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
metal film
Ni film
Ni
CCl₄
Ar gas
Ar
double-layered carbon film
Si substrate
Si
| — |
Thickness | 350–600 nm | — |
Duration | 10–20 minutes | — |
Temperature | 900–1100 °C | — |
Duration | 10–30 minutes | — |
Pressure | 0.0001 Pa | — |
Duration | ≤ 20 minutes | — |
Duration | ≥ 1 minutes | — |
Temperature | 750–1150 °C | — |
Temperature | 60–90 °C | — |
metal film
Ni film
Ni
CCl₄
Ar gas
Ar
double-layered carbon film
Si substrate
Si
| — |
Thickness | 350–600 nm | — |
Duration | 10–20 minutes | — |
Temperature | 900–1100 °C | — |
Duration | 10–30 minutes | — |
Pressure | 0.0001 Pa | — |
Duration | ≤ 20 minutes | — |
Duration | ≥ 1 minutes | — |
Temperature | 750–1150 °C | — |
Temperature | 60–90 °C | — |
metal film
Ni film
Ni
CCl₄
Ar gas
Ar
double-layered carbon film
Si substrate
Si
| — |
Thickness | 350–600 nm | — |
Duration | 10–20 minutes | — |
Temperature | 900–1100 °C | — |
Duration | 10–30 minutes | — |
Pressure | 0.0001 Pa | — |
Duration | ≤ 20 minutes | — |
Duration | ≥ 1 minutes | — |
Temperature | 750–1150 °C | — |
Temperature | 60–90 °C | — |
metal film
Ni film
Ni
CCl₄
Ar gas
Ar
double-layered carbon film
Si substrate
Si
| — |
Thickness | 350–600 nm | — |
Duration | 10–20 minutes | — |
Temperature | 900–1100 °C | — |
Duration | 10–30 minutes | — |
Pressure | 0.0001 Pa | — |
Duration | ≤ 20 minutes | — |
Duration | ≥ 1 minutes | — |
Temperature | 750–1150 °C | — |
Temperature | 60–90 °C | — |