Patent
US 9,919,264ENHANCED GRAPHENE OXIDE MEMBRANES AND METHODS FOR MAKING SAME
YONGSOON SHIN, DAVID W. GOTTHOLD, LEONARD S. FIFIELD, WEI LIU
BATTELLE MEMORIAL INSTITUTE·US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 9,919,264Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 3 is a table comparing physical properties of exemplary GO membranes of the present invention against conventional GO membranes. [0011]
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
FIG. 5 is an optical microscope image of a concentrated GO dispersion showing presence of large GO flakes after removal of small flakes used to prepare GO …
FIG. 6 and
FIG. 7 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional GO membranes. [0015]
FIG. 8 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional permeation membranes.
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 for making a graphene oxide membrane, comprising the step of: casting a gel dispersion comprising graphene oxide (GO) flakes having an average diameter greater than or equal to about 100 micrometers at a substantially neutral pH onto a receiving surface.
The method of claim 1, further including the step of air drying the gel dispersion on the receiving surface to form the membrane.
The method of claim 1, wherein the gel dispersion includes a pH selected from about 5 to about 7.5.
The method of claim 1, wherein the graphene oxide (GO) flakes in the gel has a concentration between about 1 % to about 3 % by weight.
The method of Claim 1, wherein the gel dispersion is formed by a process including placing a graphite solid with a particle size greater than about 150 micrometers into a concentrated acid solution without sonicating or stirring the graphite for a time sufficient to form a quantity of graphite oxide.
The method of Claim 1, further comprising using a draw-bar to draw the dispersion down to the selected thickness.
A free-standing graphene oxide membrane having a thickness in the range between 1 micrometer to 10 micrometers, a selectivity for H₂ O in a mixed gas greater than 10 4, and a permeability for H₂ 0 of at least ~10 5 mol/m 2.s.Pa.
The free-standing graphene oxide membrane of claim 11 wherein the membrane has graphene oxide (GO) flakes with an average diameter greater than or equal to about 100 micrometers. 17
Embodiments described in the patent, grouped by the materials and process steps they use.
8 materials5 process steps
An aqueous gel dispersion (1-3 wt%) of graphene oxide (GO) flakes having an average diameter greater than 100 micrometers is cast onto a receiving surface at substantially neutral pH (5-7.5) to form a GO membrane. The dispersion is prepared by placing graphite solid (particle size >150 µm) into a 9:1 H₂SO₄/H₃PO₄ concentrated acid solution without sonicating or stirring for 8-9 minutes to form graphite oxide, followed by addition of excess KMnO₄ powder to exfoliate and fully oxidize to individual GO layers. The GO slurry is then added to 30 wt% H₂O₂/H₂O at 0-4°C to neutralize residual KMnO4, washed with 1 M H₂SO₄ or HCl without stirring to remove metal ions, then iteratively rinsed with DI water (~3-4 times) until pH 6-7.5. The slurry is centrifuged at 4000 rpm for 8-9 minutes to remove flakes <5 µm diameter. The concentrated GO dispersion (1-3 wt%) is cast onto a receiving surface and drawn to selected thickness using a draw bar, then air dried to form a free-standing membrane.
Layer stacks claimed or described, ordered top of device to substrate.
free-standing graphene oxide membrane
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
free-standing GO membrane thickness | 1–10 micrometer | graphene oxide (GO) flakes |
H2O selectivity in mixed gas | ≥ 10000 dimensionless |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,919,264Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 3 is a table comparing physical properties of exemplary GO membranes of the present invention against conventional GO membranes. [0011]
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
FIG. 5 is an optical microscope image of a concentrated GO dispersion showing presence of large GO flakes after removal of small flakes used to prepare GO …
FIG. 6 and
FIG. 7 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional GO membranes. [0015]
FIG. 8 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional permeation membranes.
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 for making a graphene oxide membrane, comprising the step of: casting a gel dispersion comprising graphene oxide (GO) flakes having an average diameter greater than or equal to about 100 micrometers at a substantially neutral pH onto a receiving surface.
The method of claim 1, further including the step of air drying the gel dispersion on the receiving surface to form the membrane.
The method of claim 1, wherein the gel dispersion includes a pH selected from about 5 to about 7.5.
The method of claim 1, wherein the graphene oxide (GO) flakes in the gel has a concentration between about 1 % to about 3 % by weight.
The method of Claim 1, wherein the gel dispersion is formed by a process including placing a graphite solid with a particle size greater than about 150 micrometers into a concentrated acid solution without sonicating or stirring the graphite for a time sufficient to form a quantity of graphite oxide.
The method of Claim 1, further comprising using a draw-bar to draw the dispersion down to the selected thickness.
A free-standing graphene oxide membrane having a thickness in the range between 1 micrometer to 10 micrometers, a selectivity for H₂ O in a mixed gas greater than 10 4, and a permeability for H₂ 0 of at least ~10 5 mol/m 2.s.Pa.
The free-standing graphene oxide membrane of claim 11 wherein the membrane has graphene oxide (GO) flakes with an average diameter greater than or equal to about 100 micrometers. 17
Embodiments described in the patent, grouped by the materials and process steps they use.
8 materials5 process steps
An aqueous gel dispersion (1-3 wt%) of graphene oxide (GO) flakes having an average diameter greater than 100 micrometers is cast onto a receiving surface at substantially neutral pH (5-7.5) to form a GO membrane. The dispersion is prepared by placing graphite solid (particle size >150 µm) into a 9:1 H₂SO₄/H₃PO₄ concentrated acid solution without sonicating or stirring for 8-9 minutes to form graphite oxide, followed by addition of excess KMnO₄ powder to exfoliate and fully oxidize to individual GO layers. The GO slurry is then added to 30 wt% H₂O₂/H₂O at 0-4°C to neutralize residual KMnO4, washed with 1 M H₂SO₄ or HCl without stirring to remove metal ions, then iteratively rinsed with DI water (~3-4 times) until pH 6-7.5. The slurry is centrifuged at 4000 rpm for 8-9 minutes to remove flakes <5 µm diameter. The concentrated GO dispersion (1-3 wt%) is cast onto a receiving surface and drawn to selected thickness using a draw bar, then air dried to form a free-standing membrane.
Layer stacks claimed or described, ordered top of device to substrate.
free-standing graphene oxide membrane
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
free-standing GO membrane thickness | 1–10 micrometer | graphene oxide (GO) flakes |
H2O selectivity in mixed gas | ≥ 10000 dimensionless |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,919,264Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 3 is a table comparing physical properties of exemplary GO membranes of the present invention against conventional GO membranes. [0011]
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
FIG. 5 is an optical microscope image of a concentrated GO dispersion showing presence of large GO flakes after removal of small flakes used to prepare GO …
FIG. 6 and
FIG. 7 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional GO membranes. [0015]
FIG. 8 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional permeation membranes.
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 for making a graphene oxide membrane, comprising the step of: casting a gel dispersion comprising graphene oxide (GO) flakes having an average diameter greater than or equal to about 100 micrometers at a substantially neutral pH onto a receiving surface.
The method of claim 1, further including the step of air drying the gel dispersion on the receiving surface to form the membrane.
The method of claim 1, wherein the gel dispersion includes a pH selected from about 5 to about 7.5.
The method of claim 1, wherein the graphene oxide (GO) flakes in the gel has a concentration between about 1 % to about 3 % by weight.
The method of Claim 1, wherein the gel dispersion is formed by a process including placing a graphite solid with a particle size greater than about 150 micrometers into a concentrated acid solution without sonicating or stirring the graphite for a time sufficient to form a quantity of graphite oxide.
The method of Claim 1, further comprising using a draw-bar to draw the dispersion down to the selected thickness.
A free-standing graphene oxide membrane having a thickness in the range between 1 micrometer to 10 micrometers, a selectivity for H₂ O in a mixed gas greater than 10 4, and a permeability for H₂ 0 of at least ~10 5 mol/m 2.s.Pa.
The free-standing graphene oxide membrane of claim 11 wherein the membrane has graphene oxide (GO) flakes with an average diameter greater than or equal to about 100 micrometers. 17
Embodiments described in the patent, grouped by the materials and process steps they use.
8 materials5 process steps
An aqueous gel dispersion (1-3 wt%) of graphene oxide (GO) flakes having an average diameter greater than 100 micrometers is cast onto a receiving surface at substantially neutral pH (5-7.5) to form a GO membrane. The dispersion is prepared by placing graphite solid (particle size >150 µm) into a 9:1 H₂SO₄/H₃PO₄ concentrated acid solution without sonicating or stirring for 8-9 minutes to form graphite oxide, followed by addition of excess KMnO₄ powder to exfoliate and fully oxidize to individual GO layers. The GO slurry is then added to 30 wt% H₂O₂/H₂O at 0-4°C to neutralize residual KMnO4, washed with 1 M H₂SO₄ or HCl without stirring to remove metal ions, then iteratively rinsed with DI water (~3-4 times) until pH 6-7.5. The slurry is centrifuged at 4000 rpm for 8-9 minutes to remove flakes <5 µm diameter. The concentrated GO dispersion (1-3 wt%) is cast onto a receiving surface and drawn to selected thickness using a draw bar, then air dried to form a free-standing membrane.
Layer stacks claimed or described, ordered top of device to substrate.
free-standing graphene oxide membrane
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
free-standing GO membrane thickness | 1–10 micrometer | graphene oxide (GO) flakes |
H2O selectivity in mixed gas | ≥ 10000 dimensionless |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,919,264Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 3 is a table comparing physical properties of exemplary GO membranes of the present invention against conventional GO membranes. [0011]
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
FIG. 5 is an optical microscope image of a concentrated GO dispersion showing presence of large GO flakes after removal of small flakes used to prepare GO …
FIG. 6 and
FIG. 7 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional GO membranes. [0015]
FIG. 8 is a table comparing permeability test results for exemplary GO membranes of the present invention against conventional permeation membranes.
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 for making a graphene oxide membrane, comprising the step of: casting a gel dispersion comprising graphene oxide (GO) flakes having an average diameter greater than or equal to about 100 micrometers at a substantially neutral pH onto a receiving surface.
The method of claim 1, further including the step of air drying the gel dispersion on the receiving surface to form the membrane.
The method of claim 1, wherein the gel dispersion includes a pH selected from about 5 to about 7.5.
The method of claim 1, wherein the graphene oxide (GO) flakes in the gel has a concentration between about 1 % to about 3 % by weight.
The method of Claim 1, wherein the gel dispersion is formed by a process including placing a graphite solid with a particle size greater than about 150 micrometers into a concentrated acid solution without sonicating or stirring the graphite for a time sufficient to form a quantity of graphite oxide.
The method of Claim 1, further comprising using a draw-bar to draw the dispersion down to the selected thickness.
A free-standing graphene oxide membrane having a thickness in the range between 1 micrometer to 10 micrometers, a selectivity for H₂ O in a mixed gas greater than 10 4, and a permeability for H₂ 0 of at least ~10 5 mol/m 2.s.Pa.
The free-standing graphene oxide membrane of claim 11 wherein the membrane has graphene oxide (GO) flakes with an average diameter greater than or equal to about 100 micrometers. 17
Embodiments described in the patent, grouped by the materials and process steps they use.
8 materials5 process steps
An aqueous gel dispersion (1-3 wt%) of graphene oxide (GO) flakes having an average diameter greater than 100 micrometers is cast onto a receiving surface at substantially neutral pH (5-7.5) to form a GO membrane. The dispersion is prepared by placing graphite solid (particle size >150 µm) into a 9:1 H₂SO₄/H₃PO₄ concentrated acid solution without sonicating or stirring for 8-9 minutes to form graphite oxide, followed by addition of excess KMnO₄ powder to exfoliate and fully oxidize to individual GO layers. The GO slurry is then added to 30 wt% H₂O₂/H₂O at 0-4°C to neutralize residual KMnO4, washed with 1 M H₂SO₄ or HCl without stirring to remove metal ions, then iteratively rinsed with DI water (~3-4 times) until pH 6-7.5. The slurry is centrifuged at 4000 rpm for 8-9 minutes to remove flakes <5 µm diameter. The concentrated GO dispersion (1-3 wt%) is cast onto a receiving surface and drawn to selected thickness using a draw bar, then air dried to form a free-standing membrane.
Layer stacks claimed or described, ordered top of device to substrate.
free-standing graphene oxide membrane
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 presents an exemplary method for making graphene oxide membranes in accordance with the present invention. [0009] FIG s. 2A-2D are photographic images …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
free-standing GO membrane thickness | 1–10 micrometer | graphene oxide (GO) flakes |
H2O selectivity in mixed gas | ≥ 10000 dimensionless |
Related documents with shared materials, methods, properties, or citations.
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
H2O permeability | ≥ 0.00001 mol/m2.s.Pa | graphene oxide (GO) flakes |
GO flake average diameter in membrane | ≥ 100 micrometer | graphene oxide (GO) flakes |
Thickness | 2–10 µm | — |
Thickness | 1–30 µm | — |
Duration | 8–9 minutes | — |
Duration | 8–10 minutes | — |
Thickness | ≤ 5 µm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 150 µm | — |
Thickness | ≥ 5 µm | — |
Thickness | 1–10 µm | — |
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
H2O permeability | ≥ 0.00001 mol/m2.s.Pa | graphene oxide (GO) flakes |
GO flake average diameter in membrane | ≥ 100 micrometer | graphene oxide (GO) flakes |
Thickness | 2–10 µm | — |
Thickness | 1–30 µm | — |
Duration | 8–9 minutes | — |
Duration | 8–10 minutes | — |
Thickness | ≤ 5 µm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 150 µm | — |
Thickness | ≥ 5 µm | — |
Thickness | 1–10 µm | — |
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
H2O permeability | ≥ 0.00001 mol/m2.s.Pa | graphene oxide (GO) flakes |
GO flake average diameter in membrane | ≥ 100 micrometer | graphene oxide (GO) flakes |
Thickness | 2–10 µm | — |
Thickness | 1–30 µm | — |
Duration | 8–9 minutes | — |
Duration | 8–10 minutes | — |
Thickness | ≤ 5 µm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 150 µm | — |
Thickness | ≥ 5 µm | — |
Thickness | 1–10 µm | — |
FIG. 2D shows an exemplary free- standing GO membrane with a thickness of 1 micrometer that is translucent, yet retains its structural integrity. In some …
FIG. 4 is an SEM image of a GO dispersion prior to removing small GO flakes that shows presence of large GO flakes used to prepare GO membranes in accordance …
H2O permeability | ≥ 0.00001 mol/m2.s.Pa | graphene oxide (GO) flakes |
GO flake average diameter in membrane | ≥ 100 micrometer | graphene oxide (GO) flakes |
Thickness | 2–10 µm | — |
Thickness | 1–30 µm | — |
Duration | 8–9 minutes | — |
Duration | 8–10 minutes | — |
Thickness | ≤ 5 µm | — |
Thickness | ≥ 1 µm | — |
Thickness | ≥ 150 µm | — |
Thickness | ≥ 5 µm | — |
Thickness | 1–10 µm | — |