Patent
US 11,447,391METHOD OF GROWING A GRAPHENE COATING OR CARBON NANOTUBES ON A CATALYTIC SUBSTRATE
SAMAN CHOUBAK
US
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Patent
Atlas literature
Patent
US 11,447,391Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Canceled
Canceled
A method of growing a graphene coating on a catalytic substrate by chemical vapor deposition, wherein the catalytic substrate is a copper, copper-metal alloy, or semiconductor Ge catalytic substrate, the method comprising using a low pressure chemical vapor deposition (LP-CVD) system having a manifold capable of ultra-high vacuum (U H V) conditions to perform the steps of: a) heating said catalytic substrate at a growth temperature, b) exposing the catalytic substrate heated at said growth temperature to a gaseous atmosphere of a hydro carbon-containing gas in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1 x 10- 7 s cc m, thereby growing the graphene coating on the catalytic substrate, and c) cooling said catalytic substrate down to a temperature at which etching of the graphene coating by oxidizing species does not occur in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1x 10- 7 s ccm, Pox wherein steps b) and c) are carried out in the gaseous atmosphere in which the ratio P red is about 5x10-6 or less, P ox being the partial pressure of oxidizing species in the gaseous atmosphere and Pre d being the partial pressure of reducing species in the atmosphere, wherein steps b) and c) are carried out in [[an]]the gaseous atmosphere having a reduced content of oxidizing species and comprising about 100 ppb or less of oxidizing species, [[and]] wherein steps b) and c) are purified before use so as to comprise about 100 ppb or less of oxidizing species, and wherein steps a), b) and c) are carried out in a reactor surrounded by heaters, said heaters providing the temperatures required for said steps a), b) and c). Currently amended
The method of claim 3, wherein the ratio Pred is about 5x10-8 or less during steps b) and c). Original
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 10 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein steps b) and c) are carried out under a gaseous atmosphere of a reducing species. Original
The method of claim 3, wherein step a) is carried out under a gaseous atmosphere of a reducing species or a gaseous atmosphere of an inert species. Original
The method of claim 3, wherein step a) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, wherein step c) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, further comprising, before step a), an annealing step comprising heating the catalytic substrate at an annealing temperature and annealing the catalytic substrate at said annealing temperature. Original
The method of claim 3, wherein step b) last about 5 minutes or less. Original
The method of claim 3, wherein the hydro carbon-containing gas is methane. Currently amended
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 1 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein the ratio P red is about 5x10-7 or less during steps b) and c). Previously presented
The method of claim 3, wherein the catalytic Previously presented
The method of claim 3, wherein step b) last
The method of claim 3, wherein step b) last
The method of claim 3, wherein, during step achieved within 10 seconds. Previously presented substrate is copper (Cu) or a Cu-Ni alloy. about 3 minutes or less. Previously presented about 1 minutes or less. Previously presented b), about 90 % or more surface coverage is
Canceled
Canceled
Canceled
Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Graphene growth below 1 minute on catalytic substrate; SEM images showing coverages for effective growth times from 10 s to 60 s; about 90% or more surface coverage achieved within 10 seconds.
Materials described outside the worked examples.
catalytic substrate (copper, copper-metal alloy, or semiconductor Ge)
hydrocarbon-containing gas
methane
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Pressure | 0.04–1 Torr | — |
Pressure |
Patent
Atlas literature
Patent
US 11,447,391Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Canceled
Canceled
A method of growing a graphene coating on a catalytic substrate by chemical vapor deposition, wherein the catalytic substrate is a copper, copper-metal alloy, or semiconductor Ge catalytic substrate, the method comprising using a low pressure chemical vapor deposition (LP-CVD) system having a manifold capable of ultra-high vacuum (U H V) conditions to perform the steps of: a) heating said catalytic substrate at a growth temperature, b) exposing the catalytic substrate heated at said growth temperature to a gaseous atmosphere of a hydro carbon-containing gas in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1 x 10- 7 s cc m, thereby growing the graphene coating on the catalytic substrate, and c) cooling said catalytic substrate down to a temperature at which etching of the graphene coating by oxidizing species does not occur in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1x 10- 7 s ccm, Pox wherein steps b) and c) are carried out in the gaseous atmosphere in which the ratio P red is about 5x10-6 or less, P ox being the partial pressure of oxidizing species in the gaseous atmosphere and Pre d being the partial pressure of reducing species in the atmosphere, wherein steps b) and c) are carried out in [[an]]the gaseous atmosphere having a reduced content of oxidizing species and comprising about 100 ppb or less of oxidizing species, [[and]] wherein steps b) and c) are purified before use so as to comprise about 100 ppb or less of oxidizing species, and wherein steps a), b) and c) are carried out in a reactor surrounded by heaters, said heaters providing the temperatures required for said steps a), b) and c). Currently amended
The method of claim 3, wherein the ratio Pred is about 5x10-8 or less during steps b) and c). Original
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 10 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein steps b) and c) are carried out under a gaseous atmosphere of a reducing species. Original
The method of claim 3, wherein step a) is carried out under a gaseous atmosphere of a reducing species or a gaseous atmosphere of an inert species. Original
The method of claim 3, wherein step a) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, wherein step c) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, further comprising, before step a), an annealing step comprising heating the catalytic substrate at an annealing temperature and annealing the catalytic substrate at said annealing temperature. Original
The method of claim 3, wherein step b) last about 5 minutes or less. Original
The method of claim 3, wherein the hydro carbon-containing gas is methane. Currently amended
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 1 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein the ratio P red is about 5x10-7 or less during steps b) and c). Previously presented
The method of claim 3, wherein the catalytic Previously presented
The method of claim 3, wherein step b) last
The method of claim 3, wherein step b) last
The method of claim 3, wherein, during step achieved within 10 seconds. Previously presented substrate is copper (Cu) or a Cu-Ni alloy. about 3 minutes or less. Previously presented about 1 minutes or less. Previously presented b), about 90 % or more surface coverage is
Canceled
Canceled
Canceled
Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Graphene growth below 1 minute on catalytic substrate; SEM images showing coverages for effective growth times from 10 s to 60 s; about 90% or more surface coverage achieved within 10 seconds.
Materials described outside the worked examples.
catalytic substrate (copper, copper-metal alloy, or semiconductor Ge)
hydrocarbon-containing gas
methane
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Pressure | 0.04–1 Torr | — |
Pressure |
Patent
Atlas literature
Patent
US 11,447,391Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Canceled
Canceled
A method of growing a graphene coating on a catalytic substrate by chemical vapor deposition, wherein the catalytic substrate is a copper, copper-metal alloy, or semiconductor Ge catalytic substrate, the method comprising using a low pressure chemical vapor deposition (LP-CVD) system having a manifold capable of ultra-high vacuum (U H V) conditions to perform the steps of: a) heating said catalytic substrate at a growth temperature, b) exposing the catalytic substrate heated at said growth temperature to a gaseous atmosphere of a hydro carbon-containing gas in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1 x 10- 7 s cc m, thereby growing the graphene coating on the catalytic substrate, and c) cooling said catalytic substrate down to a temperature at which etching of the graphene coating by oxidizing species does not occur in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1x 10- 7 s ccm, Pox wherein steps b) and c) are carried out in the gaseous atmosphere in which the ratio P red is about 5x10-6 or less, P ox being the partial pressure of oxidizing species in the gaseous atmosphere and Pre d being the partial pressure of reducing species in the atmosphere, wherein steps b) and c) are carried out in [[an]]the gaseous atmosphere having a reduced content of oxidizing species and comprising about 100 ppb or less of oxidizing species, [[and]] wherein steps b) and c) are purified before use so as to comprise about 100 ppb or less of oxidizing species, and wherein steps a), b) and c) are carried out in a reactor surrounded by heaters, said heaters providing the temperatures required for said steps a), b) and c). Currently amended
The method of claim 3, wherein the ratio Pred is about 5x10-8 or less during steps b) and c). Original
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 10 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein steps b) and c) are carried out under a gaseous atmosphere of a reducing species. Original
The method of claim 3, wherein step a) is carried out under a gaseous atmosphere of a reducing species or a gaseous atmosphere of an inert species. Original
The method of claim 3, wherein step a) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, wherein step c) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, further comprising, before step a), an annealing step comprising heating the catalytic substrate at an annealing temperature and annealing the catalytic substrate at said annealing temperature. Original
The method of claim 3, wherein step b) last about 5 minutes or less. Original
The method of claim 3, wherein the hydro carbon-containing gas is methane. Currently amended
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 1 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein the ratio P red is about 5x10-7 or less during steps b) and c). Previously presented
The method of claim 3, wherein the catalytic Previously presented
The method of claim 3, wherein step b) last
The method of claim 3, wherein step b) last
The method of claim 3, wherein, during step achieved within 10 seconds. Previously presented substrate is copper (Cu) or a Cu-Ni alloy. about 3 minutes or less. Previously presented about 1 minutes or less. Previously presented b), about 90 % or more surface coverage is
Canceled
Canceled
Canceled
Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Graphene growth below 1 minute on catalytic substrate; SEM images showing coverages for effective growth times from 10 s to 60 s; about 90% or more surface coverage achieved within 10 seconds.
Materials described outside the worked examples.
catalytic substrate (copper, copper-metal alloy, or semiconductor Ge)
hydrocarbon-containing gas
methane
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Pressure | 0.04–1 Torr | — |
Pressure |
Patent
Atlas literature
Patent
US 11,447,391Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Canceled
Canceled
A method of growing a graphene coating on a catalytic substrate by chemical vapor deposition, wherein the catalytic substrate is a copper, copper-metal alloy, or semiconductor Ge catalytic substrate, the method comprising using a low pressure chemical vapor deposition (LP-CVD) system having a manifold capable of ultra-high vacuum (U H V) conditions to perform the steps of: a) heating said catalytic substrate at a growth temperature, b) exposing the catalytic substrate heated at said growth temperature to a gaseous atmosphere of a hydro carbon-containing gas in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1 x 10- 7 s cc m, thereby growing the graphene coating on the catalytic substrate, and c) cooling said catalytic substrate down to a temperature at which etching of the graphene coating by oxidizing species does not occur in said LP-CVD system, wherein the system is sealed to have an air leak rate of <1x 10- 7 s ccm, Pox wherein steps b) and c) are carried out in the gaseous atmosphere in which the ratio P red is about 5x10-6 or less, P ox being the partial pressure of oxidizing species in the gaseous atmosphere and Pre d being the partial pressure of reducing species in the atmosphere, wherein steps b) and c) are carried out in [[an]]the gaseous atmosphere having a reduced content of oxidizing species and comprising about 100 ppb or less of oxidizing species, [[and]] wherein steps b) and c) are purified before use so as to comprise about 100 ppb or less of oxidizing species, and wherein steps a), b) and c) are carried out in a reactor surrounded by heaters, said heaters providing the temperatures required for said steps a), b) and c). Currently amended
The method of claim 3, wherein the ratio Pred is about 5x10-8 or less during steps b) and c). Original
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 10 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein steps b) and c) are carried out under a gaseous atmosphere of a reducing species. Original
The method of claim 3, wherein step a) is carried out under a gaseous atmosphere of a reducing species or a gaseous atmosphere of an inert species. Original
The method of claim 3, wherein step a) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, wherein step c) is carried out in the absence of the hydro carbon-containing gas. Currently amended
The method of claim 3, further comprising, before step a), an annealing step comprising heating the catalytic substrate at an annealing temperature and annealing the catalytic substrate at said annealing temperature. Original
The method of claim 3, wherein step b) last about 5 minutes or less. Original
The method of claim 3, wherein the hydro carbon-containing gas is methane. Currently amended
The method of claim 3, wherein all gases used during steps b) and c) are purified before use so as to comprise about 1 ppb or less of oxidizing species. Previously presented
The method of claim 3, wherein the ratio P red is about 5x10-7 or less during steps b) and c). Previously presented
The method of claim 3, wherein the catalytic Previously presented
The method of claim 3, wherein step b) last
The method of claim 3, wherein step b) last
The method of claim 3, wherein, during step achieved within 10 seconds. Previously presented substrate is copper (Cu) or a Cu-Ni alloy. about 3 minutes or less. Previously presented about 1 minutes or less. Previously presented b), about 90 % or more surface coverage is
Canceled
Canceled
Canceled
Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Graphene growth below 1 minute on catalytic substrate; SEM images showing coverages for effective growth times from 10 s to 60 s; about 90% or more surface coverage achieved within 10 seconds.
Materials described outside the worked examples.
catalytic substrate (copper, copper-metal alloy, or semiconductor Ge)
hydrocarbon-containing gas
methane
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Pressure | 0.04–1 Torr | — |
Pressure |
CH₄
carbon nanotubes
copper (Cu) or Cu-Ni alloy substrate
| 0.000001 Torr |
| — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 4 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 2 minutes | — |
Pressure | ≥ 1.5 Torr | — |
Pressure | ≥ 40 mTorr | — |
CH₄
carbon nanotubes
copper (Cu) or Cu-Ni alloy substrate
| 0.000001 Torr |
| — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 4 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 2 minutes | — |
Pressure | ≥ 1.5 Torr | — |
Pressure | ≥ 40 mTorr | — |
CH₄
carbon nanotubes
copper (Cu) or Cu-Ni alloy substrate
| 0.000001 Torr |
| — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 4 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 2 minutes | — |
Pressure | ≥ 1.5 Torr | — |
Pressure | ≥ 40 mTorr | — |
CH₄
carbon nanotubes
copper (Cu) or Cu-Ni alloy substrate
| 0.000001 Torr |
| — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 4 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 2 minutes | — |
Pressure | ≥ 1.5 Torr | — |
Pressure | ≥ 40 mTorr | — |