VAPOR-TRAPPING GROWTH OF SINGLE-CRYSTALLINE GRAPHENE FLOWERS | Matter42 Literature
Patent details
Patent
US 9,627,485
VAPOR-TRAPPING GROWTH OF SINGLE-CRYSTALLINE GRAPHENE FLOWERS
Chongwu Zhou
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 2
FIG. 3
FIG. 4
FIG. 5
FIG. 6
FIG. 7
FIG. 8
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 21 dependent
1
IndependentCCuCH₄H₂
A method comprising: placing a vessel comprising a quartz tube having an open end into a chemical vapor deposition chamber, wherein metal foil is positioned in the vessel, and wherein the open end of the vessel is closer to a first opening of the chemical vapor deposition chamber than a closed end of the vessel is to the first opening; evacuating the chemical vapor deposition chamber; flowing hydrogen gas through the chamber from the first opening of the chamber to a second opening of the chamber to achieve a first pressure less than atmospheric pressure; heating the atmosphere in the chamber to anneal the metal foil; flowing methane and hydrogen through the chamber from the first opening of the chamber to the second opening of the chamber to achieve a second pressure less than atmospheric pressure; and depositing carbon on the metal foil to yield a single-crystalline graphene layer on the metal foil.
2
Dependent← claim 1
The method of claim 1, wherein the methane and hydrogen introduced into the chamber do not flow through the vessel.
4
Dependent← claim 1Cu
The method of claim 1, wherein a local environment between the metal foil and an interior of the vessel is different from an environment inside the chamber, and wherein the metal foil is a copper foil.
6
Dependent← claim 1C
The method of claim 1, wherein the graphene layer is in the shape of a four- lobed flower, a six-lobed flower, or a combination thereof.
7
Dependent← claim 1C
The method of claim 1, wherein a dimension of the graphene layer on the metal foil is up to 100 m.
10
Dependent← claim 1
The method of claim 1, further comprising adjusting a total pressure, a methane to hydrogen flow rate ratio, or both to obtain a desired morphology.
11
Dependent← claim 1
The method of claim 1, wherein a ratio of a flow rate of the methane to a flow rate of the hydrogen is between 1: 10 to 1: 20.
12
Dependent← claim 1
The method of claim 1, wherein a total pressure of methane and hydrogen is less than 200 mTorr.
13
Dependent← claim 1C
The method of claim 1, further comprising removing the graphene layer from the metal foil.
14
Dependent← claim 1C
The method of claim 1, wherein the graphene produces one set of symmetric six-fold electron diffraction pattern oriented in the same direction.
15
Dependent← claim 1C
A single-crystalline graphene layer formed by the method of claim 1. withdrawn
16
Dependent← claim 1Cgraphene field effect transistor on Si/SiO2
A field effect transistor comprising a graphene layer formed by the method of claim 1. withdrawn
17
Dependent← claim 1CSiSiO₂graphene field effect transistor on Si/SiO2
A method of forming a field effect transistor, the method comprising: providing a silicon substrate; providing a thermal oxide on the silicon substrate; transferring the graphene layer formed by the method of claim 1 from the metal foil onto the thermal oxide layer to form a graphene channel; depositing a source electrode at one end of the graphene channel; and depositing a drain electrode at another end of the graphene channel.
21
Dependent← claim 1Ch-BNgraphene Hall-bar device on h-BN
A device comprising the graphene layer formed using the method of claim 1, wherein the graphene layer is transferred onto hexagonal boron nitride (h-BN), and an electron SVG 14214173.09-01-2016.ISKZOIFHRXEAPX0.CLM.3.22.1239.2292.1280.2334.svg 0.14 0.137 Chemistry Black and white mobility in the device is about 20,000 cm 2 V-1. withdrawn
Worked examples
Embodiments described in the patent, grouped by the materials and process steps they use.
Vapor-trapping CVD growth of single-crystalline graphene flowers
description derived process summary
4 materials1 process step
Cu foil placed inside a half-inch quartz tube (single open end) which is placed inside a 2-inch CVD quartz tube. Chamber evacuated, 7 sccm H₂ introduced at 40 mTorr, temperature ramped to 1000 °C in 40 minutes, Cu foils annealed at 1000 °C for 20 minutes. Then 1 sccm CH₄ and 12.5 sccm H₂ introduced, pressure held at 200 mTorr for 30 minutes during growth. Chamber cooled to room temperature while CH₄/H₂ flow continued at 200 mTorr. Single-crystalline graphene flowers (four-lobe and six-lobe) up to 100 μm formed on the inner Cu foil; continuous polycrystalline film with etching formed on outer Cu foil.
Graphene growth without vapor-trapping tube (reduced methane flow rate comparison)
description derived process summary
4 materials1 process step
Graphene grown on Cu foil without quartz tube 140, using 0.5 sccm CH₄ and 25 sccm H₂ at total pressure of 150 mTorr. Other parameters identical to vapor-trapping recipe. Flower shapes were less uniform compared to vapor-trapping approach.
Transfer and FET fabrication on Si/SiO₂
description derived process summary
3 materials1 process step
Graphene flowers transferred from Cu foil onto Si/SiO₂ substrate. Field effect transistors fabricated with source and drain electrodes; fitted device mobility ~4,200 cm2 V-1 s-1 obtained.
Transfer onto h-BN and Hall-bar device
description derived process summary
2 materials
Graphene layer transferred onto hexagonal boron nitride (h-BN) to form a Hall-bar device. Electron mobility ~20,000 cm2 V-1 s-1 obtained.
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
graphene field effect transistor on Si/SiO₂
Cchannel
SiO₂gate dielectric
Sisubstrate
graphene Hall-bar device on h-BN
Cchannel
h-BNsubstrate
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
fitted device mobility on Si/SiO2
4200 cm2 V-1 s-1
C
electron mobility on h-BN Hall-bar device
20000 cm2 V-1 s-1
Why these are connected
Related documents with shared materials, methods, properties, or citations.
VAPOR-TRAPPING GROWTH OF SINGLE-CRYSTALLINE GRAPHENE FLOWERS
Chongwu Zhou
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 2
FIG. 3
FIG. 4
FIG. 5
FIG. 6
FIG. 7
FIG. 8
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 21 dependent
1
IndependentCCuCH₄H₂
A method comprising: placing a vessel comprising a quartz tube having an open end into a chemical vapor deposition chamber, wherein metal foil is positioned in the vessel, and wherein the open end of the vessel is closer to a first opening of the chemical vapor deposition chamber than a closed end of the vessel is to the first opening; evacuating the chemical vapor deposition chamber; flowing hydrogen gas through the chamber from the first opening of the chamber to a second opening of the chamber to achieve a first pressure less than atmospheric pressure; heating the atmosphere in the chamber to anneal the metal foil; flowing methane and hydrogen through the chamber from the first opening of the chamber to the second opening of the chamber to achieve a second pressure less than atmospheric pressure; and depositing carbon on the metal foil to yield a single-crystalline graphene layer on the metal foil.
2
Dependent← claim 1
The method of claim 1, wherein the methane and hydrogen introduced into the chamber do not flow through the vessel.
4
Dependent← claim 1Cu
The method of claim 1, wherein a local environment between the metal foil and an interior of the vessel is different from an environment inside the chamber, and wherein the metal foil is a copper foil.
6
Dependent← claim 1C
The method of claim 1, wherein the graphene layer is in the shape of a four- lobed flower, a six-lobed flower, or a combination thereof.
7
Dependent← claim 1C
The method of claim 1, wherein a dimension of the graphene layer on the metal foil is up to 100 m.
10
Dependent← claim 1
The method of claim 1, further comprising adjusting a total pressure, a methane to hydrogen flow rate ratio, or both to obtain a desired morphology.
11
Dependent← claim 1
The method of claim 1, wherein a ratio of a flow rate of the methane to a flow rate of the hydrogen is between 1: 10 to 1: 20.
12
Dependent← claim 1
The method of claim 1, wherein a total pressure of methane and hydrogen is less than 200 mTorr.
13
Dependent← claim 1C
The method of claim 1, further comprising removing the graphene layer from the metal foil.
14
Dependent← claim 1C
The method of claim 1, wherein the graphene produces one set of symmetric six-fold electron diffraction pattern oriented in the same direction.
15
Dependent← claim 1C
A single-crystalline graphene layer formed by the method of claim 1. withdrawn
16
Dependent← claim 1Cgraphene field effect transistor on Si/SiO2
A field effect transistor comprising a graphene layer formed by the method of claim 1. withdrawn
17
Dependent← claim 1CSiSiO₂graphene field effect transistor on Si/SiO2
A method of forming a field effect transistor, the method comprising: providing a silicon substrate; providing a thermal oxide on the silicon substrate; transferring the graphene layer formed by the method of claim 1 from the metal foil onto the thermal oxide layer to form a graphene channel; depositing a source electrode at one end of the graphene channel; and depositing a drain electrode at another end of the graphene channel.
21
Dependent← claim 1Ch-BNgraphene Hall-bar device on h-BN
A device comprising the graphene layer formed using the method of claim 1, wherein the graphene layer is transferred onto hexagonal boron nitride (h-BN), and an electron SVG 14214173.09-01-2016.ISKZOIFHRXEAPX0.CLM.3.22.1239.2292.1280.2334.svg 0.14 0.137 Chemistry Black and white mobility in the device is about 20,000 cm 2 V-1. withdrawn
Worked examples
Embodiments described in the patent, grouped by the materials and process steps they use.
Vapor-trapping CVD growth of single-crystalline graphene flowers
description derived process summary
4 materials1 process step
Cu foil placed inside a half-inch quartz tube (single open end) which is placed inside a 2-inch CVD quartz tube. Chamber evacuated, 7 sccm H₂ introduced at 40 mTorr, temperature ramped to 1000 °C in 40 minutes, Cu foils annealed at 1000 °C for 20 minutes. Then 1 sccm CH₄ and 12.5 sccm H₂ introduced, pressure held at 200 mTorr for 30 minutes during growth. Chamber cooled to room temperature while CH₄/H₂ flow continued at 200 mTorr. Single-crystalline graphene flowers (four-lobe and six-lobe) up to 100 μm formed on the inner Cu foil; continuous polycrystalline film with etching formed on outer Cu foil.
Graphene growth without vapor-trapping tube (reduced methane flow rate comparison)
description derived process summary
4 materials1 process step
Graphene grown on Cu foil without quartz tube 140, using 0.5 sccm CH₄ and 25 sccm H₂ at total pressure of 150 mTorr. Other parameters identical to vapor-trapping recipe. Flower shapes were less uniform compared to vapor-trapping approach.
Transfer and FET fabrication on Si/SiO₂
description derived process summary
3 materials1 process step
Graphene flowers transferred from Cu foil onto Si/SiO₂ substrate. Field effect transistors fabricated with source and drain electrodes; fitted device mobility ~4,200 cm2 V-1 s-1 obtained.
Transfer onto h-BN and Hall-bar device
description derived process summary
2 materials
Graphene layer transferred onto hexagonal boron nitride (h-BN) to form a Hall-bar device. Electron mobility ~20,000 cm2 V-1 s-1 obtained.
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
graphene field effect transistor on Si/SiO₂
Cchannel
SiO₂gate dielectric
Sisubstrate
graphene Hall-bar device on h-BN
Cchannel
h-BNsubstrate
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
fitted device mobility on Si/SiO2
4200 cm2 V-1 s-1
C
electron mobility on h-BN Hall-bar device
20000 cm2 V-1 s-1
Why these are connected
Related documents with shared materials, methods, properties, or citations.
VAPOR-TRAPPING GROWTH OF SINGLE-CRYSTALLINE GRAPHENE FLOWERS
Chongwu Zhou
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 2
FIG. 3
FIG. 4
FIG. 5
FIG. 6
FIG. 7
FIG. 8
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 21 dependent
1
IndependentCCuCH₄H₂
A method comprising: placing a vessel comprising a quartz tube having an open end into a chemical vapor deposition chamber, wherein metal foil is positioned in the vessel, and wherein the open end of the vessel is closer to a first opening of the chemical vapor deposition chamber than a closed end of the vessel is to the first opening; evacuating the chemical vapor deposition chamber; flowing hydrogen gas through the chamber from the first opening of the chamber to a second opening of the chamber to achieve a first pressure less than atmospheric pressure; heating the atmosphere in the chamber to anneal the metal foil; flowing methane and hydrogen through the chamber from the first opening of the chamber to the second opening of the chamber to achieve a second pressure less than atmospheric pressure; and depositing carbon on the metal foil to yield a single-crystalline graphene layer on the metal foil.
2
Dependent← claim 1
The method of claim 1, wherein the methane and hydrogen introduced into the chamber do not flow through the vessel.
4
Dependent← claim 1Cu
The method of claim 1, wherein a local environment between the metal foil and an interior of the vessel is different from an environment inside the chamber, and wherein the metal foil is a copper foil.
6
Dependent← claim 1C
The method of claim 1, wherein the graphene layer is in the shape of a four- lobed flower, a six-lobed flower, or a combination thereof.
7
Dependent← claim 1C
The method of claim 1, wherein a dimension of the graphene layer on the metal foil is up to 100 m.
10
Dependent← claim 1
The method of claim 1, further comprising adjusting a total pressure, a methane to hydrogen flow rate ratio, or both to obtain a desired morphology.
11
Dependent← claim 1
The method of claim 1, wherein a ratio of a flow rate of the methane to a flow rate of the hydrogen is between 1: 10 to 1: 20.
12
Dependent← claim 1
The method of claim 1, wherein a total pressure of methane and hydrogen is less than 200 mTorr.
13
Dependent← claim 1C
The method of claim 1, further comprising removing the graphene layer from the metal foil.
14
Dependent← claim 1C
The method of claim 1, wherein the graphene produces one set of symmetric six-fold electron diffraction pattern oriented in the same direction.
15
Dependent← claim 1C
A single-crystalline graphene layer formed by the method of claim 1. withdrawn
16
Dependent← claim 1Cgraphene field effect transistor on Si/SiO2
A field effect transistor comprising a graphene layer formed by the method of claim 1. withdrawn
17
Dependent← claim 1CSiSiO₂graphene field effect transistor on Si/SiO2
A method of forming a field effect transistor, the method comprising: providing a silicon substrate; providing a thermal oxide on the silicon substrate; transferring the graphene layer formed by the method of claim 1 from the metal foil onto the thermal oxide layer to form a graphene channel; depositing a source electrode at one end of the graphene channel; and depositing a drain electrode at another end of the graphene channel.
21
Dependent← claim 1Ch-BNgraphene Hall-bar device on h-BN
A device comprising the graphene layer formed using the method of claim 1, wherein the graphene layer is transferred onto hexagonal boron nitride (h-BN), and an electron SVG 14214173.09-01-2016.ISKZOIFHRXEAPX0.CLM.3.22.1239.2292.1280.2334.svg 0.14 0.137 Chemistry Black and white mobility in the device is about 20,000 cm 2 V-1. withdrawn
Worked examples
Embodiments described in the patent, grouped by the materials and process steps they use.
Vapor-trapping CVD growth of single-crystalline graphene flowers
description derived process summary
4 materials1 process step
Cu foil placed inside a half-inch quartz tube (single open end) which is placed inside a 2-inch CVD quartz tube. Chamber evacuated, 7 sccm H₂ introduced at 40 mTorr, temperature ramped to 1000 °C in 40 minutes, Cu foils annealed at 1000 °C for 20 minutes. Then 1 sccm CH₄ and 12.5 sccm H₂ introduced, pressure held at 200 mTorr for 30 minutes during growth. Chamber cooled to room temperature while CH₄/H₂ flow continued at 200 mTorr. Single-crystalline graphene flowers (four-lobe and six-lobe) up to 100 μm formed on the inner Cu foil; continuous polycrystalline film with etching formed on outer Cu foil.
Graphene growth without vapor-trapping tube (reduced methane flow rate comparison)
description derived process summary
4 materials1 process step
Graphene grown on Cu foil without quartz tube 140, using 0.5 sccm CH₄ and 25 sccm H₂ at total pressure of 150 mTorr. Other parameters identical to vapor-trapping recipe. Flower shapes were less uniform compared to vapor-trapping approach.
Transfer and FET fabrication on Si/SiO₂
description derived process summary
3 materials1 process step
Graphene flowers transferred from Cu foil onto Si/SiO₂ substrate. Field effect transistors fabricated with source and drain electrodes; fitted device mobility ~4,200 cm2 V-1 s-1 obtained.
Transfer onto h-BN and Hall-bar device
description derived process summary
2 materials
Graphene layer transferred onto hexagonal boron nitride (h-BN) to form a Hall-bar device. Electron mobility ~20,000 cm2 V-1 s-1 obtained.
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
graphene field effect transistor on Si/SiO₂
Cchannel
SiO₂gate dielectric
Sisubstrate
graphene Hall-bar device on h-BN
Cchannel
h-BNsubstrate
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
fitted device mobility on Si/SiO2
4200 cm2 V-1 s-1
C
electron mobility on h-BN Hall-bar device
20000 cm2 V-1 s-1
Why these are connected
Related documents with shared materials, methods, properties, or citations.
VAPOR-TRAPPING GROWTH OF SINGLE-CRYSTALLINE GRAPHENE FLOWERS
Chongwu Zhou
US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 2
FIG. 3
FIG. 4
FIG. 5
FIG. 6
FIG. 7
FIG. 8
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1 independent · 21 dependent
1
IndependentCCuCH₄H₂
A method comprising: placing a vessel comprising a quartz tube having an open end into a chemical vapor deposition chamber, wherein metal foil is positioned in the vessel, and wherein the open end of the vessel is closer to a first opening of the chemical vapor deposition chamber than a closed end of the vessel is to the first opening; evacuating the chemical vapor deposition chamber; flowing hydrogen gas through the chamber from the first opening of the chamber to a second opening of the chamber to achieve a first pressure less than atmospheric pressure; heating the atmosphere in the chamber to anneal the metal foil; flowing methane and hydrogen through the chamber from the first opening of the chamber to the second opening of the chamber to achieve a second pressure less than atmospheric pressure; and depositing carbon on the metal foil to yield a single-crystalline graphene layer on the metal foil.
2
Dependent← claim 1
The method of claim 1, wherein the methane and hydrogen introduced into the chamber do not flow through the vessel.
4
Dependent← claim 1Cu
The method of claim 1, wherein a local environment between the metal foil and an interior of the vessel is different from an environment inside the chamber, and wherein the metal foil is a copper foil.
6
Dependent← claim 1C
The method of claim 1, wherein the graphene layer is in the shape of a four- lobed flower, a six-lobed flower, or a combination thereof.
7
Dependent← claim 1C
The method of claim 1, wherein a dimension of the graphene layer on the metal foil is up to 100 m.
10
Dependent← claim 1
The method of claim 1, further comprising adjusting a total pressure, a methane to hydrogen flow rate ratio, or both to obtain a desired morphology.
11
Dependent← claim 1
The method of claim 1, wherein a ratio of a flow rate of the methane to a flow rate of the hydrogen is between 1: 10 to 1: 20.
12
Dependent← claim 1
The method of claim 1, wherein a total pressure of methane and hydrogen is less than 200 mTorr.
13
Dependent← claim 1C
The method of claim 1, further comprising removing the graphene layer from the metal foil.
14
Dependent← claim 1C
The method of claim 1, wherein the graphene produces one set of symmetric six-fold electron diffraction pattern oriented in the same direction.
15
Dependent← claim 1C
A single-crystalline graphene layer formed by the method of claim 1. withdrawn
16
Dependent← claim 1Cgraphene field effect transistor on Si/SiO2
A field effect transistor comprising a graphene layer formed by the method of claim 1. withdrawn
17
Dependent← claim 1CSiSiO₂graphene field effect transistor on Si/SiO2
A method of forming a field effect transistor, the method comprising: providing a silicon substrate; providing a thermal oxide on the silicon substrate; transferring the graphene layer formed by the method of claim 1 from the metal foil onto the thermal oxide layer to form a graphene channel; depositing a source electrode at one end of the graphene channel; and depositing a drain electrode at another end of the graphene channel.
21
Dependent← claim 1Ch-BNgraphene Hall-bar device on h-BN
A device comprising the graphene layer formed using the method of claim 1, wherein the graphene layer is transferred onto hexagonal boron nitride (h-BN), and an electron SVG 14214173.09-01-2016.ISKZOIFHRXEAPX0.CLM.3.22.1239.2292.1280.2334.svg 0.14 0.137 Chemistry Black and white mobility in the device is about 20,000 cm 2 V-1. withdrawn
Worked examples
Embodiments described in the patent, grouped by the materials and process steps they use.
Vapor-trapping CVD growth of single-crystalline graphene flowers
description derived process summary
4 materials1 process step
Cu foil placed inside a half-inch quartz tube (single open end) which is placed inside a 2-inch CVD quartz tube. Chamber evacuated, 7 sccm H₂ introduced at 40 mTorr, temperature ramped to 1000 °C in 40 minutes, Cu foils annealed at 1000 °C for 20 minutes. Then 1 sccm CH₄ and 12.5 sccm H₂ introduced, pressure held at 200 mTorr for 30 minutes during growth. Chamber cooled to room temperature while CH₄/H₂ flow continued at 200 mTorr. Single-crystalline graphene flowers (four-lobe and six-lobe) up to 100 μm formed on the inner Cu foil; continuous polycrystalline film with etching formed on outer Cu foil.
Graphene growth without vapor-trapping tube (reduced methane flow rate comparison)
description derived process summary
4 materials1 process step
Graphene grown on Cu foil without quartz tube 140, using 0.5 sccm CH₄ and 25 sccm H₂ at total pressure of 150 mTorr. Other parameters identical to vapor-trapping recipe. Flower shapes were less uniform compared to vapor-trapping approach.
Transfer and FET fabrication on Si/SiO₂
description derived process summary
3 materials1 process step
Graphene flowers transferred from Cu foil onto Si/SiO₂ substrate. Field effect transistors fabricated with source and drain electrodes; fitted device mobility ~4,200 cm2 V-1 s-1 obtained.
Transfer onto h-BN and Hall-bar device
description derived process summary
2 materials
Graphene layer transferred onto hexagonal boron nitride (h-BN) to form a Hall-bar device. Electron mobility ~20,000 cm2 V-1 s-1 obtained.
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
graphene field effect transistor on Si/SiO₂
Cchannel
SiO₂gate dielectric
Sisubstrate
graphene Hall-bar device on h-BN
Cchannel
h-BNsubstrate
Reported properties
Performance values and ranges asserted in the specification or claims.
Property
Value
Material
fitted device mobility on Si/SiO2
4200 cm2 V-1 s-1
C
electron mobility on h-BN Hall-bar device
20000 cm2 V-1 s-1
Why these are connected
Related documents with shared materials, methods, properties, or citations.