Patent
US 11,701,621 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 revealing the Raman spectrum of the 50 sample, two strong peaks centered at 1590 cm⁻¹ (G band) and 2684 cm⁻¹ (2D band), the typical characteristic peaks …
FIG. 2: The SEM image of graphene membrane obtained from Example 1. 20
FIG. 3: The SEM image of graphene membrane obtained from Example 2.
FIG. 4: The SEM image of graphene membrane obtained from Example 5. DETAILED DESCRIPTION Some examples are given to further illustrate the detail preparation …
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 direct growth of porous graphene sepa-ration membrane on a metal foil, comprising: (1) directly coating mixture of an etching agent, an organic solvent A and a polymer on a metal foil, and calcining the mixture and the metal foil at high tem-perature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to the organic solvent A is 1:0.5-50:100-1000, alternatively, coating a dispersion or solution of the etching agent on a metal foil, on which a polymer film is overlaid; calcining the obtained metal foil at high temperature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to a solvent B or a dispersion B is 1:0.5-50:100-1000; the calcination is performed at 400-1200° C. for 0.17-4 hours; wherein the solvent B or the dispersion B is used for dissolution or dispersion of the etching agent, B₂ wherein the etching agent is polyoxometalate, metal nitrates, metal oxide, or a mixture of thereof, and a mass concentration of the etching agent solution or dispersion is 0.1%-20%, wherein the polymer is polyvinyl butyral or/and polym-ethylmethacrylate, wherein the organic solvent A is methanol, ethanol, isopropyl alcohol, acetone, chloroform, or a mixture thereof, the solvent B or the dispersion B is ethanol or/and water, wherein the metal foil is copper foil or nickel foil, and wherein the oxygen-free condition is inert gas protec-tion or vacuum, (2) removing the metal foil and reaction products to obtain the porous graphene separation membranes; wherein the porous graphene separation membranes consist of single-layered, double-layered or multi-lay-ered graphene. ∗ ∗ ∗ ∗ ∗
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
PMMA and Cu(NO₃)2·3H₂O dissolved in acetone (mass ratio Cu(NO₃)2:PMMA:acetone = 1:5:200); 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 100 Pa, then at 1000°C for 30 min in 400 sccm Ar/10 sccm H₂ at 100 Pa. Sample floated on 2.5 M FeCl₃/0.5 M HCl to remove Cu foil and reaction products. Porous graphene membrane obtained with average pore size ~20 nm and water flux 48000 L m−2 h−1 bar−1. Raman spectrum shows G band at 1590 cm⁻¹ and 2D band at 2684 cm⁻¹.
4 materials1 process step
Cu(NO₃)2:PMMA:acetone mass ratio = 1:2.5:100; 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at ambient pressure. Sample floated on 2.5 M FeCl₃/0.5 M HCl. Porous graphene membrane obtained with average pore size ~35 nm and water flux 105000 L m−2 h−1 bar−1.
3 materials1 process step
0.1 g Fe(NO₃)3·9H₂O and 2.5 g PVB dissolved in 100 g ethanol (mass ratio Fe(NO₃)3:PVB:ethanol = 1:25:1000); 20 µL spin-coated at 1000 r/min on 2 cm×2 cm Ni foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 50 Pa, then at 800°C for 30 min in 400 sccm Ar/10 sccm H₂ at 50 Pa. Sample floated on 2 wt% (NH₄)2S₂O₈ to remove metal foil and reaction products. Porous graphene membrane transferred to substrates for filtration.
Layer stacks claimed or described, ordered top of device to substrate.
porous graphene separation membrane
Materials described outside the worked examples.
polyoxometalate etching agent
metal nitrates etching agent
metal oxide etching agent
polyvinyl butyral or polymethylmethacrylate
copper foil or nickel foil
porous graphene separation membrane
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
G band | 1590 cm⁻¹ | porous graphene separation membrane |
2D band | 2684 cm⁻¹ | porous graphene separation membrane |
water flux Example 1 | 48000 L m-2 h-1 bar-1 | porous graphene separation membrane |
water flux Example 2 | 105000 L m-2 h-1 bar-1 | porous graphene separation membrane |
Temperature | 400–1200 °C | — |
Duration | 0.17–4 hours | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 revealing the Raman spectrum of the 50 sample, two strong peaks centered at 1590 cm⁻¹ (G band) and 2684 cm⁻¹ (2D band), the typical characteristic peaks …
FIG. 2: The SEM image of graphene membrane obtained from Example 1. 20
FIG. 3: The SEM image of graphene membrane obtained from Example 2.
FIG. 4: The SEM image of graphene membrane obtained from Example 5. DETAILED DESCRIPTION Some examples are given to further illustrate the detail preparation …
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 direct growth of porous graphene sepa-ration membrane on a metal foil, comprising: (1) directly coating mixture of an etching agent, an organic solvent A and a polymer on a metal foil, and calcining the mixture and the metal foil at high tem-perature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to the organic solvent A is 1:0.5-50:100-1000, alternatively, coating a dispersion or solution of the etching agent on a metal foil, on which a polymer film is overlaid; calcining the obtained metal foil at high temperature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to a solvent B or a dispersion B is 1:0.5-50:100-1000; the calcination is performed at 400-1200° C. for 0.17-4 hours; wherein the solvent B or the dispersion B is used for dissolution or dispersion of the etching agent, B₂ wherein the etching agent is polyoxometalate, metal nitrates, metal oxide, or a mixture of thereof, and a mass concentration of the etching agent solution or dispersion is 0.1%-20%, wherein the polymer is polyvinyl butyral or/and polym-ethylmethacrylate, wherein the organic solvent A is methanol, ethanol, isopropyl alcohol, acetone, chloroform, or a mixture thereof, the solvent B or the dispersion B is ethanol or/and water, wherein the metal foil is copper foil or nickel foil, and wherein the oxygen-free condition is inert gas protec-tion or vacuum, (2) removing the metal foil and reaction products to obtain the porous graphene separation membranes; wherein the porous graphene separation membranes consist of single-layered, double-layered or multi-lay-ered graphene. ∗ ∗ ∗ ∗ ∗
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
PMMA and Cu(NO₃)2·3H₂O dissolved in acetone (mass ratio Cu(NO₃)2:PMMA:acetone = 1:5:200); 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 100 Pa, then at 1000°C for 30 min in 400 sccm Ar/10 sccm H₂ at 100 Pa. Sample floated on 2.5 M FeCl₃/0.5 M HCl to remove Cu foil and reaction products. Porous graphene membrane obtained with average pore size ~20 nm and water flux 48000 L m−2 h−1 bar−1. Raman spectrum shows G band at 1590 cm⁻¹ and 2D band at 2684 cm⁻¹.
4 materials1 process step
Cu(NO₃)2:PMMA:acetone mass ratio = 1:2.5:100; 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at ambient pressure. Sample floated on 2.5 M FeCl₃/0.5 M HCl. Porous graphene membrane obtained with average pore size ~35 nm and water flux 105000 L m−2 h−1 bar−1.
3 materials1 process step
0.1 g Fe(NO₃)3·9H₂O and 2.5 g PVB dissolved in 100 g ethanol (mass ratio Fe(NO₃)3:PVB:ethanol = 1:25:1000); 20 µL spin-coated at 1000 r/min on 2 cm×2 cm Ni foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 50 Pa, then at 800°C for 30 min in 400 sccm Ar/10 sccm H₂ at 50 Pa. Sample floated on 2 wt% (NH₄)2S₂O₈ to remove metal foil and reaction products. Porous graphene membrane transferred to substrates for filtration.
Layer stacks claimed or described, ordered top of device to substrate.
porous graphene separation membrane
Materials described outside the worked examples.
polyoxometalate etching agent
metal nitrates etching agent
metal oxide etching agent
polyvinyl butyral or polymethylmethacrylate
copper foil or nickel foil
porous graphene separation membrane
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
G band | 1590 cm⁻¹ | porous graphene separation membrane |
2D band | 2684 cm⁻¹ | porous graphene separation membrane |
water flux Example 1 | 48000 L m-2 h-1 bar-1 | porous graphene separation membrane |
water flux Example 2 | 105000 L m-2 h-1 bar-1 | porous graphene separation membrane |
Temperature | 400–1200 °C | — |
Duration | 0.17–4 hours | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 revealing the Raman spectrum of the 50 sample, two strong peaks centered at 1590 cm⁻¹ (G band) and 2684 cm⁻¹ (2D band), the typical characteristic peaks …
FIG. 2: The SEM image of graphene membrane obtained from Example 1. 20
FIG. 3: The SEM image of graphene membrane obtained from Example 2.
FIG. 4: The SEM image of graphene membrane obtained from Example 5. DETAILED DESCRIPTION Some examples are given to further illustrate the detail preparation …
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 direct growth of porous graphene sepa-ration membrane on a metal foil, comprising: (1) directly coating mixture of an etching agent, an organic solvent A and a polymer on a metal foil, and calcining the mixture and the metal foil at high tem-perature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to the organic solvent A is 1:0.5-50:100-1000, alternatively, coating a dispersion or solution of the etching agent on a metal foil, on which a polymer film is overlaid; calcining the obtained metal foil at high temperature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to a solvent B or a dispersion B is 1:0.5-50:100-1000; the calcination is performed at 400-1200° C. for 0.17-4 hours; wherein the solvent B or the dispersion B is used for dissolution or dispersion of the etching agent, B₂ wherein the etching agent is polyoxometalate, metal nitrates, metal oxide, or a mixture of thereof, and a mass concentration of the etching agent solution or dispersion is 0.1%-20%, wherein the polymer is polyvinyl butyral or/and polym-ethylmethacrylate, wherein the organic solvent A is methanol, ethanol, isopropyl alcohol, acetone, chloroform, or a mixture thereof, the solvent B or the dispersion B is ethanol or/and water, wherein the metal foil is copper foil or nickel foil, and wherein the oxygen-free condition is inert gas protec-tion or vacuum, (2) removing the metal foil and reaction products to obtain the porous graphene separation membranes; wherein the porous graphene separation membranes consist of single-layered, double-layered or multi-lay-ered graphene. ∗ ∗ ∗ ∗ ∗
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
PMMA and Cu(NO₃)2·3H₂O dissolved in acetone (mass ratio Cu(NO₃)2:PMMA:acetone = 1:5:200); 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 100 Pa, then at 1000°C for 30 min in 400 sccm Ar/10 sccm H₂ at 100 Pa. Sample floated on 2.5 M FeCl₃/0.5 M HCl to remove Cu foil and reaction products. Porous graphene membrane obtained with average pore size ~20 nm and water flux 48000 L m−2 h−1 bar−1. Raman spectrum shows G band at 1590 cm⁻¹ and 2D band at 2684 cm⁻¹.
4 materials1 process step
Cu(NO₃)2:PMMA:acetone mass ratio = 1:2.5:100; 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at ambient pressure. Sample floated on 2.5 M FeCl₃/0.5 M HCl. Porous graphene membrane obtained with average pore size ~35 nm and water flux 105000 L m−2 h−1 bar−1.
3 materials1 process step
0.1 g Fe(NO₃)3·9H₂O and 2.5 g PVB dissolved in 100 g ethanol (mass ratio Fe(NO₃)3:PVB:ethanol = 1:25:1000); 20 µL spin-coated at 1000 r/min on 2 cm×2 cm Ni foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 50 Pa, then at 800°C for 30 min in 400 sccm Ar/10 sccm H₂ at 50 Pa. Sample floated on 2 wt% (NH₄)2S₂O₈ to remove metal foil and reaction products. Porous graphene membrane transferred to substrates for filtration.
Layer stacks claimed or described, ordered top of device to substrate.
porous graphene separation membrane
Materials described outside the worked examples.
polyoxometalate etching agent
metal nitrates etching agent
metal oxide etching agent
polyvinyl butyral or polymethylmethacrylate
copper foil or nickel foil
porous graphene separation membrane
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
G band | 1590 cm⁻¹ | porous graphene separation membrane |
2D band | 2684 cm⁻¹ | porous graphene separation membrane |
water flux Example 1 | 48000 L m-2 h-1 bar-1 | porous graphene separation membrane |
water flux Example 2 | 105000 L m-2 h-1 bar-1 | porous graphene separation membrane |
Temperature | 400–1200 °C | — |
Duration | 0.17–4 hours | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 revealing the Raman spectrum of the 50 sample, two strong peaks centered at 1590 cm⁻¹ (G band) and 2684 cm⁻¹ (2D band), the typical characteristic peaks …
FIG. 2: The SEM image of graphene membrane obtained from Example 1. 20
FIG. 3: The SEM image of graphene membrane obtained from Example 2.
FIG. 4: The SEM image of graphene membrane obtained from Example 5. DETAILED DESCRIPTION Some examples are given to further illustrate the detail preparation …
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 direct growth of porous graphene sepa-ration membrane on a metal foil, comprising: (1) directly coating mixture of an etching agent, an organic solvent A and a polymer on a metal foil, and calcining the mixture and the metal foil at high tem-perature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to the organic solvent A is 1:0.5-50:100-1000, alternatively, coating a dispersion or solution of the etching agent on a metal foil, on which a polymer film is overlaid; calcining the obtained metal foil at high temperature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to a solvent B or a dispersion B is 1:0.5-50:100-1000; the calcination is performed at 400-1200° C. for 0.17-4 hours; wherein the solvent B or the dispersion B is used for dissolution or dispersion of the etching agent, B₂ wherein the etching agent is polyoxometalate, metal nitrates, metal oxide, or a mixture of thereof, and a mass concentration of the etching agent solution or dispersion is 0.1%-20%, wherein the polymer is polyvinyl butyral or/and polym-ethylmethacrylate, wherein the organic solvent A is methanol, ethanol, isopropyl alcohol, acetone, chloroform, or a mixture thereof, the solvent B or the dispersion B is ethanol or/and water, wherein the metal foil is copper foil or nickel foil, and wherein the oxygen-free condition is inert gas protec-tion or vacuum, (2) removing the metal foil and reaction products to obtain the porous graphene separation membranes; wherein the porous graphene separation membranes consist of single-layered, double-layered or multi-lay-ered graphene. ∗ ∗ ∗ ∗ ∗
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
PMMA and Cu(NO₃)2·3H₂O dissolved in acetone (mass ratio Cu(NO₃)2:PMMA:acetone = 1:5:200); 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 100 Pa, then at 1000°C for 30 min in 400 sccm Ar/10 sccm H₂ at 100 Pa. Sample floated on 2.5 M FeCl₃/0.5 M HCl to remove Cu foil and reaction products. Porous graphene membrane obtained with average pore size ~20 nm and water flux 48000 L m−2 h−1 bar−1. Raman spectrum shows G band at 1590 cm⁻¹ and 2D band at 2684 cm⁻¹.
4 materials1 process step
Cu(NO₃)2:PMMA:acetone mass ratio = 1:2.5:100; 10 µL spin-coated at 1500 r/min on 1 cm×1 cm Cu foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at ambient pressure. Sample floated on 2.5 M FeCl₃/0.5 M HCl. Porous graphene membrane obtained with average pore size ~35 nm and water flux 105000 L m−2 h−1 bar−1.
3 materials1 process step
0.1 g Fe(NO₃)3·9H₂O and 2.5 g PVB dissolved in 100 g ethanol (mass ratio Fe(NO₃)3:PVB:ethanol = 1:25:1000); 20 µL spin-coated at 1000 r/min on 2 cm×2 cm Ni foil, naturally dried. Calcined at 800°C for 1 h in 400 sccm Ar at 50 Pa, then at 800°C for 30 min in 400 sccm Ar/10 sccm H₂ at 50 Pa. Sample floated on 2 wt% (NH₄)2S₂O₈ to remove metal foil and reaction products. Porous graphene membrane transferred to substrates for filtration.
Layer stacks claimed or described, ordered top of device to substrate.
porous graphene separation membrane
Materials described outside the worked examples.
polyoxometalate etching agent
metal nitrates etching agent
metal oxide etching agent
polyvinyl butyral or polymethylmethacrylate
copper foil or nickel foil
porous graphene separation membrane
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
G band | 1590 cm⁻¹ | porous graphene separation membrane |
2D band | 2684 cm⁻¹ | porous graphene separation membrane |
water flux Example 1 | 48000 L m-2 h-1 bar-1 | porous graphene separation membrane |
water flux Example 2 | 105000 L m-2 h-1 bar-1 | porous graphene separation membrane |
Temperature | 400–1200 °C | — |
Duration | 0.17–4 hours | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 4
Cited non-patent literature · 3