Patent
US 9,017,639METHOD FOR MAKING GRAPHENE
XIANG-MING HE
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 9,017,639Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; disposing metal lithium and graphite in the electrolyte solution, wherein the metal lithium and the graphite are in dfree- contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of the graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound.
: The method of claim 1, wherein the electrolyte lithium salt is lithium chlorate, lithium nitrate, lithium chloride, lithium acetate, lithium hexafluorophosphate, lithium bis (oxalato) borate, lithium tetrafluoroborate, lithium trifluoromethanesulfonate or any combination thereof.
: The method of claim 1, wherein the electrolyte lithium salt is dissolvable in the organic solvent and lithium ions of the electrolyte lithium salt is separable in the organic solvent.
: The method of claim 1, wherein a molar concentration of the electrolyte lithium salt Page 2 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. is in a range from about 0.1 mo l/L to about 100 mo l/L.
: The method of claim 1, wherein the graphite is electrographite, natural flake graphite, pyrolysis graphite, or expandable graphite.
: The method of claim 1, wherein the electrolyte solution with the metal lithium and the graphite dissolving therein is further heated in a hydrothermal reactor.
: The method of claim 1, wherein the graphene is peeled off by supersonic dispersing the graphite intercalation compound.
: The method of claim 1, wherein the graphene is separated out by a centrifugal separation method or filtration method after peeling off the graphene.
. canceled
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; Page 3 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. mixing metal lithium powder with graphite powder in the electrolyte solution, wherein the metal lithium powder and the graphite powder are in contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound. Page 4 of
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Lithium chlorate dissolved in propene carbonate (PC) at 1.5 mol/L. Natural flake graphite (1 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 190°C under high pressure for 1 hour to form graphite intercalation compound. Supersonic dispersed at 1500 W for 40 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in tetrahydrofuran (THF) at 0.5 mol/L. Natural flake graphite (8 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 200°C under high pressure in hydrothermal reactor for 1.5 hours to form graphite intercalation compound. Supersonic dispersed at 600 W for 120 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in 1,2-Dimethoxyethane (DME) to form electrolyte solution. Natural flake graphite and metal lithium powder mixed with electrolyte solution, heated in hydrothermal reactor to form graphite intercalation compound, then supersonic dispersed to obtain graphene.
Materials described outside the worked examples.
graphene
electrolyte lithium salt
Measurements and analyses referenced in the patent, with their drawing references.
Scanning electron microscopic (SEM) images of graphene made by Example 1 method, shown in FIGS. 1 and 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.05–1000 µm | — |
Duration | 1800–144000 s |
Patent
Atlas literature
Patent
US 9,017,639Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; disposing metal lithium and graphite in the electrolyte solution, wherein the metal lithium and the graphite are in dfree- contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of the graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound.
: The method of claim 1, wherein the electrolyte lithium salt is lithium chlorate, lithium nitrate, lithium chloride, lithium acetate, lithium hexafluorophosphate, lithium bis (oxalato) borate, lithium tetrafluoroborate, lithium trifluoromethanesulfonate or any combination thereof.
: The method of claim 1, wherein the electrolyte lithium salt is dissolvable in the organic solvent and lithium ions of the electrolyte lithium salt is separable in the organic solvent.
: The method of claim 1, wherein a molar concentration of the electrolyte lithium salt Page 2 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. is in a range from about 0.1 mo l/L to about 100 mo l/L.
: The method of claim 1, wherein the graphite is electrographite, natural flake graphite, pyrolysis graphite, or expandable graphite.
: The method of claim 1, wherein the electrolyte solution with the metal lithium and the graphite dissolving therein is further heated in a hydrothermal reactor.
: The method of claim 1, wherein the graphene is peeled off by supersonic dispersing the graphite intercalation compound.
: The method of claim 1, wherein the graphene is separated out by a centrifugal separation method or filtration method after peeling off the graphene.
. canceled
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; Page 3 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. mixing metal lithium powder with graphite powder in the electrolyte solution, wherein the metal lithium powder and the graphite powder are in contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound. Page 4 of
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Lithium chlorate dissolved in propene carbonate (PC) at 1.5 mol/L. Natural flake graphite (1 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 190°C under high pressure for 1 hour to form graphite intercalation compound. Supersonic dispersed at 1500 W for 40 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in tetrahydrofuran (THF) at 0.5 mol/L. Natural flake graphite (8 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 200°C under high pressure in hydrothermal reactor for 1.5 hours to form graphite intercalation compound. Supersonic dispersed at 600 W for 120 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in 1,2-Dimethoxyethane (DME) to form electrolyte solution. Natural flake graphite and metal lithium powder mixed with electrolyte solution, heated in hydrothermal reactor to form graphite intercalation compound, then supersonic dispersed to obtain graphene.
Materials described outside the worked examples.
graphene
electrolyte lithium salt
Measurements and analyses referenced in the patent, with their drawing references.
Scanning electron microscopic (SEM) images of graphene made by Example 1 method, shown in FIGS. 1 and 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.05–1000 µm | — |
Duration | 1800–144000 s |
Patent
Atlas literature
Patent
US 9,017,639Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; disposing metal lithium and graphite in the electrolyte solution, wherein the metal lithium and the graphite are in dfree- contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of the graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound.
: The method of claim 1, wherein the electrolyte lithium salt is lithium chlorate, lithium nitrate, lithium chloride, lithium acetate, lithium hexafluorophosphate, lithium bis (oxalato) borate, lithium tetrafluoroborate, lithium trifluoromethanesulfonate or any combination thereof.
: The method of claim 1, wherein the electrolyte lithium salt is dissolvable in the organic solvent and lithium ions of the electrolyte lithium salt is separable in the organic solvent.
: The method of claim 1, wherein a molar concentration of the electrolyte lithium salt Page 2 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. is in a range from about 0.1 mo l/L to about 100 mo l/L.
: The method of claim 1, wherein the graphite is electrographite, natural flake graphite, pyrolysis graphite, or expandable graphite.
: The method of claim 1, wherein the electrolyte solution with the metal lithium and the graphite dissolving therein is further heated in a hydrothermal reactor.
: The method of claim 1, wherein the graphene is peeled off by supersonic dispersing the graphite intercalation compound.
: The method of claim 1, wherein the graphene is separated out by a centrifugal separation method or filtration method after peeling off the graphene.
. canceled
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; Page 3 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. mixing metal lithium powder with graphite powder in the electrolyte solution, wherein the metal lithium powder and the graphite powder are in contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound. Page 4 of
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Lithium chlorate dissolved in propene carbonate (PC) at 1.5 mol/L. Natural flake graphite (1 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 190°C under high pressure for 1 hour to form graphite intercalation compound. Supersonic dispersed at 1500 W for 40 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in tetrahydrofuran (THF) at 0.5 mol/L. Natural flake graphite (8 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 200°C under high pressure in hydrothermal reactor for 1.5 hours to form graphite intercalation compound. Supersonic dispersed at 600 W for 120 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in 1,2-Dimethoxyethane (DME) to form electrolyte solution. Natural flake graphite and metal lithium powder mixed with electrolyte solution, heated in hydrothermal reactor to form graphite intercalation compound, then supersonic dispersed to obtain graphene.
Materials described outside the worked examples.
graphene
electrolyte lithium salt
Measurements and analyses referenced in the patent, with their drawing references.
Scanning electron microscopic (SEM) images of graphene made by Example 1 method, shown in FIGS. 1 and 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.05–1000 µm | — |
Duration | 1800–144000 s |
Patent
Atlas literature
Patent
US 9,017,639Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; disposing metal lithium and graphite in the electrolyte solution, wherein the metal lithium and the graphite are in dfree- contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of the graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound.
: The method of claim 1, wherein the electrolyte lithium salt is lithium chlorate, lithium nitrate, lithium chloride, lithium acetate, lithium hexafluorophosphate, lithium bis (oxalato) borate, lithium tetrafluoroborate, lithium trifluoromethanesulfonate or any combination thereof.
: The method of claim 1, wherein the electrolyte lithium salt is dissolvable in the organic solvent and lithium ions of the electrolyte lithium salt is separable in the organic solvent.
: The method of claim 1, wherein a molar concentration of the electrolyte lithium salt Page 2 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. is in a range from about 0.1 mo l/L to about 100 mo l/L.
: The method of claim 1, wherein the graphite is electrographite, natural flake graphite, pyrolysis graphite, or expandable graphite.
: The method of claim 1, wherein the electrolyte solution with the metal lithium and the graphite dissolving therein is further heated in a hydrothermal reactor.
: The method of claim 1, wherein the graphene is peeled off by supersonic dispersing the graphite intercalation compound.
: The method of claim 1, wherein the graphene is separated out by a centrifugal separation method or filtration method after peeling off the graphene.
. canceled
: A method for making graphene, the method comprising: forming an electrolyte solution by dissolving an electrolyte lithium salt in an organic solvent, wherein lithium ions are separated out from the electrolyte lithium salt in the electrolyte solution; Page 3 of 10 App l. No. 13/554,127 Reply to Office Action of Attorney Docket No. mixing metal lithium powder with graphite powder in the electrolyte solution, wherein the metal lithium powder and the graphite powder are in contact with each other, thereby the lithium ions and organic solvent molecules from the organic solvent jointly gather between adjacent layers of graphite to form a graphite intercalation compound; and peeling off graphene from the graphite intercalation compound. Page 4 of
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Lithium chlorate dissolved in propene carbonate (PC) at 1.5 mol/L. Natural flake graphite (1 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 190°C under high pressure for 1 hour to form graphite intercalation compound. Supersonic dispersed at 1500 W for 40 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in tetrahydrofuran (THF) at 0.5 mol/L. Natural flake graphite (8 micron particle diameter) and metal lithium powder mixed with electrolyte solution. Heated to 200°C under high pressure in hydrothermal reactor for 1.5 hours to form graphite intercalation compound. Supersonic dispersed at 600 W for 120 minutes to form graphene suspension. Graphene separated by centrifugal separation and dried by natural drying.
4 materials1 process step
Lithium chlorate dissolved in 1,2-Dimethoxyethane (DME) to form electrolyte solution. Natural flake graphite and metal lithium powder mixed with electrolyte solution, heated in hydrothermal reactor to form graphite intercalation compound, then supersonic dispersed to obtain graphene.
Materials described outside the worked examples.
graphene
electrolyte lithium salt
Measurements and analyses referenced in the patent, with their drawing references.
Scanning electron microscopic (SEM) images of graphene made by Example 1 method, shown in FIGS. 1 and 2.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.05–1000 µm | — |
Duration | 1800–144000 s |
organic solvent
graphite
graphite intercalation compound
| — |
Duration | 5–400 minutes | — |
Temperature | 150–300 °C | — |
organic solvent
graphite
graphite intercalation compound
| — |
Duration | 5–400 minutes | — |
Temperature | 150–300 °C | — |
organic solvent
graphite
graphite intercalation compound
| — |
Duration | 5–400 minutes | — |
Temperature | 150–300 °C | — |
organic solvent
graphite
graphite intercalation compound
| — |
Duration | 5–400 minutes | — |
Temperature | 150–300 °C | — |