Patent
US 10,717,653GRAPHENE PRODUCTION BY THE THERMAL RELEASE OF INTRINSIC CARBON
Phillip C. Womble
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 10,717,653Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows observed Raman peaks.
Figure 2 shows a comparison of hydrophobic activity.
Figure 3 shows the results of a corrosion test.
Figure 4 shows Raman spectrum from the growth medium.
Figure 5 shows a magnified view of graphene.
Figure 6 shows a close-up view of a graphene domain.
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 fo rm ing graphene, comprising: (a) applying a vacuum to a furnace, the inside of the furnace comprising: A. an oxygen scavenger; and, B. a growth sample, the growth sample, comprising: a carbon-containing metal and a substrate, wherein the carbon-containing metal is in the fo rm of a plurality of seeds that are in contact with the substrate; (b) introducing a hydrogen-containing gas to the furnace; (c) heating the inside of the furnace to a temperature and for a time sufficient to initiate graphene for m ation on the carbon-containing metal; [[]] (d) cooling the furnace; and (e) removing the seeds from the substrate. Currently amended
The method of claim 1, wherein the carbon-containing metal is selected from: Fe and Ni. Previously presented
The method of claim 1, wherein the carbon-containing metal is carbon steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is 1095 steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is grey steel. Previously presented
The method of claim 1, wherein the oxygen scavenger is Ti sponge. Previously presented
The method of claim 1, wherein the vacuum applied is 510 m Torr. Previously presented
The method of claim 1, wherein the vacuum applied is 2 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is introduced until the pressure of the furnace is from 20-150 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is a fo rm ing gas. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % Ar/5% H 2. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % N 2/5 % H 2. Previously presented
The method of claim 1, wherein the furnace is heated to a temperature of from 900- 1100° C for an hour. Previously presented
The method of claim 1, wherein the furnace is maintained at its highest temperature for 30-60 minutes. Previously presented
Canceled
Canceled
The method of claim [[2]] 1, wherein the substrate is selected from: Cu, sapphire, and Ni on sapphire. Currently amended
The method of claim [[2]] !, wherein the substrate is Cu. Currently amended
The method of claim [[2]] 1, wherein the substrate is sapphire. Currently amended
The method of claim [[2]] _, wherein the substrate is Ni on sapphire. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
General procedure for graphene growth on a carbon-containing metal (e.g., Fe with at least 1 wt% C). The sample is placed in the central heating zone of a tube furnace with ~70 cc/L Ti sponge (99.9% pure, top size 19 mm, minimum below 3 mm) as oxygen scavenger in separate crucibles. Vacuum is applied until pressure is below 2 mTorr, then 95% Ar/5% H₂ forming gas is introduced until pressure is 40–100 mTorr. The furnace is ramped at 20°C/min to above 1000°C, held for ~1 hour, then powered off and allowed to cool naturally at ~20°C/min.
1 material1 process step
Pieces of carbon steel were heated at 800–1100°C using the procedure in Example 1. Raman spectra (Renishaw InVia, 532 nm laser) showed graphene D (1350 cm⁻¹), G (1585 cm⁻¹), and 2D (2700 cm⁻¹) peaks when steel was heated above 800°C. The D peak decreased and 2D peak increased with increasing temperature, indicating improved graphene quality. Hydrophobicity (water droplet shape) was also observed to increase with temperature; steel heated to 1050°C showed more spherical water droplets compared to 800°C. Corrosion resistance was tested over 10 days in 5 M saline: three graphene-coated samples (PW-76-1, -6, -10) heated to 1050°C for 1 hour were compared to untreated and degreased-only blades.
Materials described outside the worked examples.
hydrogen-containing gas
Fe
Ni
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Raman D peak | 1350 cm⁻¹ | carbon steel |
Raman G peak |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,717,653Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows observed Raman peaks.
Figure 2 shows a comparison of hydrophobic activity.
Figure 3 shows the results of a corrosion test.
Figure 4 shows Raman spectrum from the growth medium.
Figure 5 shows a magnified view of graphene.
Figure 6 shows a close-up view of a graphene domain.
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 fo rm ing graphene, comprising: (a) applying a vacuum to a furnace, the inside of the furnace comprising: A. an oxygen scavenger; and, B. a growth sample, the growth sample, comprising: a carbon-containing metal and a substrate, wherein the carbon-containing metal is in the fo rm of a plurality of seeds that are in contact with the substrate; (b) introducing a hydrogen-containing gas to the furnace; (c) heating the inside of the furnace to a temperature and for a time sufficient to initiate graphene for m ation on the carbon-containing metal; [[]] (d) cooling the furnace; and (e) removing the seeds from the substrate. Currently amended
The method of claim 1, wherein the carbon-containing metal is selected from: Fe and Ni. Previously presented
The method of claim 1, wherein the carbon-containing metal is carbon steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is 1095 steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is grey steel. Previously presented
The method of claim 1, wherein the oxygen scavenger is Ti sponge. Previously presented
The method of claim 1, wherein the vacuum applied is 510 m Torr. Previously presented
The method of claim 1, wherein the vacuum applied is 2 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is introduced until the pressure of the furnace is from 20-150 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is a fo rm ing gas. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % Ar/5% H 2. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % N 2/5 % H 2. Previously presented
The method of claim 1, wherein the furnace is heated to a temperature of from 900- 1100° C for an hour. Previously presented
The method of claim 1, wherein the furnace is maintained at its highest temperature for 30-60 minutes. Previously presented
Canceled
Canceled
The method of claim [[2]] 1, wherein the substrate is selected from: Cu, sapphire, and Ni on sapphire. Currently amended
The method of claim [[2]] !, wherein the substrate is Cu. Currently amended
The method of claim [[2]] 1, wherein the substrate is sapphire. Currently amended
The method of claim [[2]] _, wherein the substrate is Ni on sapphire. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
General procedure for graphene growth on a carbon-containing metal (e.g., Fe with at least 1 wt% C). The sample is placed in the central heating zone of a tube furnace with ~70 cc/L Ti sponge (99.9% pure, top size 19 mm, minimum below 3 mm) as oxygen scavenger in separate crucibles. Vacuum is applied until pressure is below 2 mTorr, then 95% Ar/5% H₂ forming gas is introduced until pressure is 40–100 mTorr. The furnace is ramped at 20°C/min to above 1000°C, held for ~1 hour, then powered off and allowed to cool naturally at ~20°C/min.
1 material1 process step
Pieces of carbon steel were heated at 800–1100°C using the procedure in Example 1. Raman spectra (Renishaw InVia, 532 nm laser) showed graphene D (1350 cm⁻¹), G (1585 cm⁻¹), and 2D (2700 cm⁻¹) peaks when steel was heated above 800°C. The D peak decreased and 2D peak increased with increasing temperature, indicating improved graphene quality. Hydrophobicity (water droplet shape) was also observed to increase with temperature; steel heated to 1050°C showed more spherical water droplets compared to 800°C. Corrosion resistance was tested over 10 days in 5 M saline: three graphene-coated samples (PW-76-1, -6, -10) heated to 1050°C for 1 hour were compared to untreated and degreased-only blades.
Materials described outside the worked examples.
hydrogen-containing gas
Fe
Ni
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Raman D peak | 1350 cm⁻¹ | carbon steel |
Raman G peak |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,717,653Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows observed Raman peaks.
Figure 2 shows a comparison of hydrophobic activity.
Figure 3 shows the results of a corrosion test.
Figure 4 shows Raman spectrum from the growth medium.
Figure 5 shows a magnified view of graphene.
Figure 6 shows a close-up view of a graphene domain.
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 fo rm ing graphene, comprising: (a) applying a vacuum to a furnace, the inside of the furnace comprising: A. an oxygen scavenger; and, B. a growth sample, the growth sample, comprising: a carbon-containing metal and a substrate, wherein the carbon-containing metal is in the fo rm of a plurality of seeds that are in contact with the substrate; (b) introducing a hydrogen-containing gas to the furnace; (c) heating the inside of the furnace to a temperature and for a time sufficient to initiate graphene for m ation on the carbon-containing metal; [[]] (d) cooling the furnace; and (e) removing the seeds from the substrate. Currently amended
The method of claim 1, wherein the carbon-containing metal is selected from: Fe and Ni. Previously presented
The method of claim 1, wherein the carbon-containing metal is carbon steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is 1095 steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is grey steel. Previously presented
The method of claim 1, wherein the oxygen scavenger is Ti sponge. Previously presented
The method of claim 1, wherein the vacuum applied is 510 m Torr. Previously presented
The method of claim 1, wherein the vacuum applied is 2 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is introduced until the pressure of the furnace is from 20-150 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is a fo rm ing gas. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % Ar/5% H 2. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % N 2/5 % H 2. Previously presented
The method of claim 1, wherein the furnace is heated to a temperature of from 900- 1100° C for an hour. Previously presented
The method of claim 1, wherein the furnace is maintained at its highest temperature for 30-60 minutes. Previously presented
Canceled
Canceled
The method of claim [[2]] 1, wherein the substrate is selected from: Cu, sapphire, and Ni on sapphire. Currently amended
The method of claim [[2]] !, wherein the substrate is Cu. Currently amended
The method of claim [[2]] 1, wherein the substrate is sapphire. Currently amended
The method of claim [[2]] _, wherein the substrate is Ni on sapphire. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
General procedure for graphene growth on a carbon-containing metal (e.g., Fe with at least 1 wt% C). The sample is placed in the central heating zone of a tube furnace with ~70 cc/L Ti sponge (99.9% pure, top size 19 mm, minimum below 3 mm) as oxygen scavenger in separate crucibles. Vacuum is applied until pressure is below 2 mTorr, then 95% Ar/5% H₂ forming gas is introduced until pressure is 40–100 mTorr. The furnace is ramped at 20°C/min to above 1000°C, held for ~1 hour, then powered off and allowed to cool naturally at ~20°C/min.
1 material1 process step
Pieces of carbon steel were heated at 800–1100°C using the procedure in Example 1. Raman spectra (Renishaw InVia, 532 nm laser) showed graphene D (1350 cm⁻¹), G (1585 cm⁻¹), and 2D (2700 cm⁻¹) peaks when steel was heated above 800°C. The D peak decreased and 2D peak increased with increasing temperature, indicating improved graphene quality. Hydrophobicity (water droplet shape) was also observed to increase with temperature; steel heated to 1050°C showed more spherical water droplets compared to 800°C. Corrosion resistance was tested over 10 days in 5 M saline: three graphene-coated samples (PW-76-1, -6, -10) heated to 1050°C for 1 hour were compared to untreated and degreased-only blades.
Materials described outside the worked examples.
hydrogen-containing gas
Fe
Ni
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Raman D peak | 1350 cm⁻¹ | carbon steel |
Raman G peak |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,717,653Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows observed Raman peaks.
Figure 2 shows a comparison of hydrophobic activity.
Figure 3 shows the results of a corrosion test.
Figure 4 shows Raman spectrum from the growth medium.
Figure 5 shows a magnified view of graphene.
Figure 6 shows a close-up view of a graphene domain.
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 fo rm ing graphene, comprising: (a) applying a vacuum to a furnace, the inside of the furnace comprising: A. an oxygen scavenger; and, B. a growth sample, the growth sample, comprising: a carbon-containing metal and a substrate, wherein the carbon-containing metal is in the fo rm of a plurality of seeds that are in contact with the substrate; (b) introducing a hydrogen-containing gas to the furnace; (c) heating the inside of the furnace to a temperature and for a time sufficient to initiate graphene for m ation on the carbon-containing metal; [[]] (d) cooling the furnace; and (e) removing the seeds from the substrate. Currently amended
The method of claim 1, wherein the carbon-containing metal is selected from: Fe and Ni. Previously presented
The method of claim 1, wherein the carbon-containing metal is carbon steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is 1095 steel. Previously presented
The method of claim 1, wherein the carbon-containing metal is grey steel. Previously presented
The method of claim 1, wherein the oxygen scavenger is Ti sponge. Previously presented
The method of claim 1, wherein the vacuum applied is 510 m Torr. Previously presented
The method of claim 1, wherein the vacuum applied is 2 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is introduced until the pressure of the furnace is from 20-150 m Torr. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is a fo rm ing gas. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % Ar/5% H 2. Previously presented
The method of claim 1, wherein the hydrogen-containing gas is 95 % N 2/5 % H 2. Previously presented
The method of claim 1, wherein the furnace is heated to a temperature of from 900- 1100° C for an hour. Previously presented
The method of claim 1, wherein the furnace is maintained at its highest temperature for 30-60 minutes. Previously presented
Canceled
Canceled
The method of claim [[2]] 1, wherein the substrate is selected from: Cu, sapphire, and Ni on sapphire. Currently amended
The method of claim [[2]] !, wherein the substrate is Cu. Currently amended
The method of claim [[2]] 1, wherein the substrate is sapphire. Currently amended
The method of claim [[2]] _, wherein the substrate is Ni on sapphire. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
General procedure for graphene growth on a carbon-containing metal (e.g., Fe with at least 1 wt% C). The sample is placed in the central heating zone of a tube furnace with ~70 cc/L Ti sponge (99.9% pure, top size 19 mm, minimum below 3 mm) as oxygen scavenger in separate crucibles. Vacuum is applied until pressure is below 2 mTorr, then 95% Ar/5% H₂ forming gas is introduced until pressure is 40–100 mTorr. The furnace is ramped at 20°C/min to above 1000°C, held for ~1 hour, then powered off and allowed to cool naturally at ~20°C/min.
1 material1 process step
Pieces of carbon steel were heated at 800–1100°C using the procedure in Example 1. Raman spectra (Renishaw InVia, 532 nm laser) showed graphene D (1350 cm⁻¹), G (1585 cm⁻¹), and 2D (2700 cm⁻¹) peaks when steel was heated above 800°C. The D peak decreased and 2D peak increased with increasing temperature, indicating improved graphene quality. Hydrophobicity (water droplet shape) was also observed to increase with temperature; steel heated to 1050°C showed more spherical water droplets compared to 800°C. Corrosion resistance was tested over 10 days in 5 M saline: three graphene-coated samples (PW-76-1, -6, -10) heated to 1050°C for 1 hour were compared to untreated and degreased-only blades.
Materials described outside the worked examples.
hydrogen-containing gas
Fe
Ni
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Raman D peak | 1350 cm⁻¹ | carbon steel |
Raman G peak |
Related documents with shared materials, methods, properties, or citations.
1095 steel
grey steel
Cu
sapphire
Al₂O₃
Ni on sapphire
95% N₂/5% H₂ forming gas
| 1585 cm⁻¹ |
carbon steel |
Raman 2D peak | 2700 cm⁻¹ | carbon steel |
Pressure | 40–100 mTorr | — |
Temperature | 800–1100 °C | — |
Pressure | 20–150 mTorr | — |
Pressure | 30–120 mTorr | — |
Pressure | ≤ 10 mTorr | — |
Thickness | ≤ 3 mm | — |
Pressure | ≤ 2 mTorr | — |
Temperature | ≥ 1 °C | — |
Temperature | 900–1100 °C | — |
Duration | 30–60 minutes | — |
SYSTEMS AND METHODS FOR TRANSFERRING GRAPHENE
1095 steel
grey steel
Cu
sapphire
Al₂O₃
Ni on sapphire
95% N₂/5% H₂ forming gas
| 1585 cm⁻¹ |
carbon steel |
Raman 2D peak | 2700 cm⁻¹ | carbon steel |
Pressure | 40–100 mTorr | — |
Temperature | 800–1100 °C | — |
Pressure | 20–150 mTorr | — |
Pressure | 30–120 mTorr | — |
Pressure | ≤ 10 mTorr | — |
Thickness | ≤ 3 mm | — |
Pressure | ≤ 2 mTorr | — |
Temperature | ≥ 1 °C | — |
Temperature | 900–1100 °C | — |
Duration | 30–60 minutes | — |
SYSTEMS AND METHODS FOR TRANSFERRING GRAPHENE
1095 steel
grey steel
Cu
sapphire
Al₂O₃
Ni on sapphire
95% N₂/5% H₂ forming gas
| 1585 cm⁻¹ |
carbon steel |
Raman 2D peak | 2700 cm⁻¹ | carbon steel |
Pressure | 40–100 mTorr | — |
Temperature | 800–1100 °C | — |
Pressure | 20–150 mTorr | — |
Pressure | 30–120 mTorr | — |
Pressure | ≤ 10 mTorr | — |
Thickness | ≤ 3 mm | — |
Pressure | ≤ 2 mTorr | — |
Temperature | ≥ 1 °C | — |
Temperature | 900–1100 °C | — |
Duration | 30–60 minutes | — |
SYSTEMS AND METHODS FOR TRANSFERRING GRAPHENE
1095 steel
grey steel
Cu
sapphire
Al₂O₃
Ni on sapphire
95% N₂/5% H₂ forming gas
| 1585 cm⁻¹ |
carbon steel |
Raman 2D peak | 2700 cm⁻¹ | carbon steel |
Pressure | 40–100 mTorr | — |
Temperature | 800–1100 °C | — |
Pressure | 20–150 mTorr | — |
Pressure | 30–120 mTorr | — |
Pressure | ≤ 10 mTorr | — |
Thickness | ≤ 3 mm | — |
Pressure | ≤ 2 mTorr | — |
Temperature | ≥ 1 °C | — |
Temperature | 900–1100 °C | — |
Duration | 30–60 minutes | — |
SYSTEMS AND METHODS FOR TRANSFERRING GRAPHENE