Patent
US 8,691,179METHOD FOR FABRICATING GRAPHENE SHEETS OR GRAPHENE PARTICLES USING SUPERCRITICAL FLUID
Jaehoon KIM
US
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Patent
Atlas literature
Patent
US 8,691,179Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
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 for fabricating graphene comprising: dispersing graphene oxide into an alcohol; heating and pressuring the graphene oxide alcohol dispersion at or above supercritical fluid conditions of the alcohol to reduce the graphene oxide into graphene; and separating the graphene away from the alcohol.
The method of claim 13, further comprising oxidizing graphite into graphene oxide.
The method of claim 13, wherein the alcohol comprises at least one selected from a group consisting of methanol, ethanol, propanol, isopropyl alcohol, butanol, iso-butanol, 2-butanol, tert-butanol, n-pentanol, isopentyl alcohol, 2-methyl- 1 -butanol, neopentyl alcohol, dimethyl carbinol, methyl propyl carbinol, methyl isopropyl carbinol, dimethyl ethyl carbinol, 1-hexanol, 2-hexanol, 3-hexanol, 2-methyl- 1 -pentanol, 3-methyl- 1 -pentanol, 4-methyl- 1 -pentanol, 2- methyl-2-pentanol, 3-methyl-2-pentanol, 4-methyl-2-pentanol, 2-methyl-3- pentanol, 3-methyl-3-pentanol, 2,2-dimethyl- 1 -butanol, 2,3-dimethyl- 1 -butanol, 2,3- dimethyl-2-butanol, 3,3-dimethyl- 1-butanol, 2-ethyl- 1 -butanol, 1 -heptanol, 2- heptanol, 3-heptanol, and 4-heptanol.
The method of claim 13, wherein separating the graphene away from the alcohol comprises centrifuging and/or filtering.
The method of claim 13, wherein heating and pressuring is performed in a continuous supercritical fluid process.
The method of claim 13, wherein heating and pressuring is performed in a batch-type supercritical fluid process. Page 8 of 12
1 7. The method of claim 1 3, wherein the alcohol comprises methanol and/or ethanol.
1 8. The method of claim 1 3, wherein dispersing graphene oxide into the alcohol comprises using supersonic waves.
1 9. The method of claim 1 3, wherein the graphene oxide comprises at least one functional group selected from a group consisting of epoxy group, Page 7 of 12 SVG 13238098.08-15-2013.HKJWTBS₅PXXIFW1.CLM10775022.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white carboxyl group, carbonyl group and hydroxyl group.
Materials described outside the worked examples.
graphene oxide
graphene
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 10–21600 s | — |
Duration |
Table 1
Graphene oxide Reaction C/0 ratio by 0/0 ratio Examples Solvents concentration time
The thusly-obtained results were shown in Table 1.
p. 8
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,691,179Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
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 for fabricating graphene comprising: dispersing graphene oxide into an alcohol; heating and pressuring the graphene oxide alcohol dispersion at or above supercritical fluid conditions of the alcohol to reduce the graphene oxide into graphene; and separating the graphene away from the alcohol.
The method of claim 13, further comprising oxidizing graphite into graphene oxide.
The method of claim 13, wherein the alcohol comprises at least one selected from a group consisting of methanol, ethanol, propanol, isopropyl alcohol, butanol, iso-butanol, 2-butanol, tert-butanol, n-pentanol, isopentyl alcohol, 2-methyl- 1 -butanol, neopentyl alcohol, dimethyl carbinol, methyl propyl carbinol, methyl isopropyl carbinol, dimethyl ethyl carbinol, 1-hexanol, 2-hexanol, 3-hexanol, 2-methyl- 1 -pentanol, 3-methyl- 1 -pentanol, 4-methyl- 1 -pentanol, 2- methyl-2-pentanol, 3-methyl-2-pentanol, 4-methyl-2-pentanol, 2-methyl-3- pentanol, 3-methyl-3-pentanol, 2,2-dimethyl- 1 -butanol, 2,3-dimethyl- 1 -butanol, 2,3- dimethyl-2-butanol, 3,3-dimethyl- 1-butanol, 2-ethyl- 1 -butanol, 1 -heptanol, 2- heptanol, 3-heptanol, and 4-heptanol.
The method of claim 13, wherein separating the graphene away from the alcohol comprises centrifuging and/or filtering.
The method of claim 13, wherein heating and pressuring is performed in a continuous supercritical fluid process.
The method of claim 13, wherein heating and pressuring is performed in a batch-type supercritical fluid process. Page 8 of 12
1 7. The method of claim 1 3, wherein the alcohol comprises methanol and/or ethanol.
1 8. The method of claim 1 3, wherein dispersing graphene oxide into the alcohol comprises using supersonic waves.
1 9. The method of claim 1 3, wherein the graphene oxide comprises at least one functional group selected from a group consisting of epoxy group, Page 7 of 12 SVG 13238098.08-15-2013.HKJWTBS₅PXXIFW1.CLM10775022.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white carboxyl group, carbonyl group and hydroxyl group.
Materials described outside the worked examples.
graphene oxide
graphene
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 10–21600 s | — |
Duration |
Table 1
Graphene oxide Reaction C/0 ratio by 0/0 ratio Examples Solvents concentration time
The thusly-obtained results were shown in Table 1.
p. 8
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,691,179Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
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 for fabricating graphene comprising: dispersing graphene oxide into an alcohol; heating and pressuring the graphene oxide alcohol dispersion at or above supercritical fluid conditions of the alcohol to reduce the graphene oxide into graphene; and separating the graphene away from the alcohol.
The method of claim 13, further comprising oxidizing graphite into graphene oxide.
The method of claim 13, wherein the alcohol comprises at least one selected from a group consisting of methanol, ethanol, propanol, isopropyl alcohol, butanol, iso-butanol, 2-butanol, tert-butanol, n-pentanol, isopentyl alcohol, 2-methyl- 1 -butanol, neopentyl alcohol, dimethyl carbinol, methyl propyl carbinol, methyl isopropyl carbinol, dimethyl ethyl carbinol, 1-hexanol, 2-hexanol, 3-hexanol, 2-methyl- 1 -pentanol, 3-methyl- 1 -pentanol, 4-methyl- 1 -pentanol, 2- methyl-2-pentanol, 3-methyl-2-pentanol, 4-methyl-2-pentanol, 2-methyl-3- pentanol, 3-methyl-3-pentanol, 2,2-dimethyl- 1 -butanol, 2,3-dimethyl- 1 -butanol, 2,3- dimethyl-2-butanol, 3,3-dimethyl- 1-butanol, 2-ethyl- 1 -butanol, 1 -heptanol, 2- heptanol, 3-heptanol, and 4-heptanol.
The method of claim 13, wherein separating the graphene away from the alcohol comprises centrifuging and/or filtering.
The method of claim 13, wherein heating and pressuring is performed in a continuous supercritical fluid process.
The method of claim 13, wherein heating and pressuring is performed in a batch-type supercritical fluid process. Page 8 of 12
1 7. The method of claim 1 3, wherein the alcohol comprises methanol and/or ethanol.
1 8. The method of claim 1 3, wherein dispersing graphene oxide into the alcohol comprises using supersonic waves.
1 9. The method of claim 1 3, wherein the graphene oxide comprises at least one functional group selected from a group consisting of epoxy group, Page 7 of 12 SVG 13238098.08-15-2013.HKJWTBS₅PXXIFW1.CLM10775022.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white carboxyl group, carbonyl group and hydroxyl group.
Materials described outside the worked examples.
graphene oxide
graphene
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 10–21600 s | — |
Duration |
Table 1
Graphene oxide Reaction C/0 ratio by 0/0 ratio Examples Solvents concentration time
The thusly-obtained results were shown in Table 1.
p. 8
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,691,179Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
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 for fabricating graphene comprising: dispersing graphene oxide into an alcohol; heating and pressuring the graphene oxide alcohol dispersion at or above supercritical fluid conditions of the alcohol to reduce the graphene oxide into graphene; and separating the graphene away from the alcohol.
The method of claim 13, further comprising oxidizing graphite into graphene oxide.
The method of claim 13, wherein the alcohol comprises at least one selected from a group consisting of methanol, ethanol, propanol, isopropyl alcohol, butanol, iso-butanol, 2-butanol, tert-butanol, n-pentanol, isopentyl alcohol, 2-methyl- 1 -butanol, neopentyl alcohol, dimethyl carbinol, methyl propyl carbinol, methyl isopropyl carbinol, dimethyl ethyl carbinol, 1-hexanol, 2-hexanol, 3-hexanol, 2-methyl- 1 -pentanol, 3-methyl- 1 -pentanol, 4-methyl- 1 -pentanol, 2- methyl-2-pentanol, 3-methyl-2-pentanol, 4-methyl-2-pentanol, 2-methyl-3- pentanol, 3-methyl-3-pentanol, 2,2-dimethyl- 1 -butanol, 2,3-dimethyl- 1 -butanol, 2,3- dimethyl-2-butanol, 3,3-dimethyl- 1-butanol, 2-ethyl- 1 -butanol, 1 -heptanol, 2- heptanol, 3-heptanol, and 4-heptanol.
The method of claim 13, wherein separating the graphene away from the alcohol comprises centrifuging and/or filtering.
The method of claim 13, wherein heating and pressuring is performed in a continuous supercritical fluid process.
The method of claim 13, wherein heating and pressuring is performed in a batch-type supercritical fluid process. Page 8 of 12
1 7. The method of claim 1 3, wherein the alcohol comprises methanol and/or ethanol.
1 8. The method of claim 1 3, wherein dispersing graphene oxide into the alcohol comprises using supersonic waves.
1 9. The method of claim 1 3, wherein the graphene oxide comprises at least one functional group selected from a group consisting of epoxy group, Page 7 of 12 SVG 13238098.08-15-2013.HKJWTBS₅PXXIFW1.CLM10775022.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white carboxyl group, carbonyl group and hydroxyl group.
Materials described outside the worked examples.
graphene oxide
graphene
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 10–21600 s | — |
Duration |
Table 1
Graphene oxide Reaction C/0 ratio by 0/0 ratio Examples Solvents concentration time
The thusly-obtained results were shown in Table 1.
p. 8
Related documents with shared materials, methods, properties, or citations.
alcohol
graphite
sulfuric acid
H₂SO₄
potassium persulfate
K₂S₂O₈
phosphorous pentoxide
P₂O₅
potassium permanganate
KMnO₄
hydrogen peroxide
H₂O₂
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
| — |
Duration | 300–7200 s | — |
Pressure | 20–600 bar | — |
Pressure | 100–500 bar | — |
Duration | ≥ 6 hours | — |
alcohol
graphite
sulfuric acid
H₂SO₄
potassium persulfate
K₂S₂O₈
phosphorous pentoxide
P₂O₅
potassium permanganate
KMnO₄
hydrogen peroxide
H₂O₂
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
| — |
Duration | 300–7200 s | — |
Pressure | 20–600 bar | — |
Pressure | 100–500 bar | — |
Duration | ≥ 6 hours | — |
alcohol
graphite
sulfuric acid
H₂SO₄
potassium persulfate
K₂S₂O₈
phosphorous pentoxide
P₂O₅
potassium permanganate
KMnO₄
hydrogen peroxide
H₂O₂
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
| — |
Duration | 300–7200 s | — |
Pressure | 20–600 bar | — |
Pressure | 100–500 bar | — |
Duration | ≥ 6 hours | — |
alcohol
graphite
sulfuric acid
H₂SO₄
potassium persulfate
K₂S₂O₈
phosphorous pentoxide
P₂O₅
potassium permanganate
KMnO₄
hydrogen peroxide
H₂O₂
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 1 is a graph showing FT-IR measurement results of graphene Is fabricated within a supercritical methanol through a batch-type supercritical fluid process …
FIG. 2, it can be exhibited that little oxygen is present in the XPS spectrum of the graphite powders whereas the graphene oxide contains 5 much oxygen in view …
FIG. 3 is a graph showing TGA measurement results of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid …
FIG. 4 is a TEM image of the graphene fabricated within the supercritical methanol through the batch-type supercritical fluid process of Example 1; 25
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 5 is a graph showing XPS measurement results of graphene 7 fabricated within a supercritical methanol through a continuous supercritical fluid process of …
FIG. 6 is a TEM image of the graphene fabricated within the supercritical methanol through the continuous supercritical fluid process of Example 10.
| — |
Duration | 300–7200 s | — |
Pressure | 20–600 bar | — |
Pressure | 100–500 bar | — |
Duration | ≥ 6 hours | — |