Patent
US 10,109,845METHODS FOR MAKING GRAPHENE-SUPPORTED METAL OXIDE MONOLITH
Marcus A. Worsley
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 10,109,845Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 shows a schematic illustration of the synthetic procedures for 3D graphene macroassembly (GMA)/Fe 2 O 3 hybrids. Step 1, three-dimensional GMA was …
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 3 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 0 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 0 3, …
FIG. 4 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 0 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 10 shows electrochemical measurements for titanium oxide graphene material. [0024]
FIG. 11 shows more electrochemical measurements for titanium oxide graphene material (annealed at 600 ° C for 1 hour under N 2 flow). [0025]
FIG. 12. (A) Nitrogen adsorption/desorption isotherms and (B) pore size distribution for graphene/Fe 2 O 3 hybrids. [0026]
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 15.(Differential capacity plots of graphene/(a +y)- Fe₂ O 3 56 wt.% Fe₂ O 3). The convoluted nature of the inset oxidation peaks can be seen. [0029]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 17. A comparison of simulated Li₂ O (cubic) diffraction patterns along < 100 > zone axis with the FFT pattern (inset) from our experiments. A good match is …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 20. Selected area diffraction (SAD) pattern taken from a(graphene/(a +y)- Fe₂ O₃ 40 wt.%) sample after 30 cycles and charged to the delithiated state (3. O …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
FIG. 22. The calculated ratio change (h'/a') after the lithiation, as a function of the initial particle shape defined by h/a (see Spherical-cap model section …
FIG. 23 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 O 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 O 3, …
FIG. 24 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 O 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 25. (a) Schematics of solid-electrolyte-interphase (SEI) formation on graphene surface upon discharge and its effect on suppressing surface reactions that …
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-supported metal oxide monolith, comprising: providing a graphene aerogel monolith; immersing said graphene aerogel monolith in a solution comprising at least one metal salt to form a mixture; curing said mixture to obtain a gel; and heating said gel to obtain a graphene-supported metal oxide monolith that comprises (i) a three-dimensional network of g raphene sheets crosslinked by covalent carbon bonds, and (ii) at least one metal oxide embedded inside said three-dimensional network, wherein the g raphene- supported metal oxide monolith is mesoporous, wherein the g raphene-supported metal oxide monolith has a surface area of at least 500 m 2/g, wherein the metal oxide accounts for 40-80 wt.% of the g raphene-supported metal oxide monolith. Currently amended
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds. Original
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds, and wherein the surfaces of the graphene sheets are substantially free of carbon nanoparticles. Original
The method of claim 1, wherein the solution further comprises at least one organic solvent. Original
The method of claim 1, wherein the solution further comprises at least one initiator. Original
The method of claim 1, wherein the solution further comprises at least one initiator, and wherein the molar ratio of the initiator to the metal salt is tuned to promote nanoparticle nucleation and anchoring on the surface of graphene sheets. Original
The method of claim 1, wherein the metal salt is an iron salt or a titanium salt. Original
The method of claim 1, wherein the metal salt is an iron salt, and the gel is heated under nitrogen at 400 ° C or more. Original
The method of claim 1, wherein the metal salt is a titanium salt, and the gel is heated under air at 250 ° C or more. Original
The method of claim 1, further comprising incorporating the graphene- supported metal oxide monolith into an electrode. Original
The method of claim 1, wherein the graphene aerogel monolith is obtained by: preparing a reaction mixture comprising a graphene oxide (GO) suspension and at least one catalyst; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel; and pyrolyzing the dry gel to produce the graphene aerogel. Original
The method of claim 1, SVG 15340875.05-23-2018.JHJOP02QRXEAPX1.CLM.3.14.388.1642.491.1699.svg Chemistry Black and white wherein the metal oxide copper, zin c, zirconium, tin, silicon, aluminum, thereof. Currently amended 0.19 0.343 comprises manganese, iron, cobalt, nickel, chromium, vanadium, titanium, or combinations
18-19. Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Three-dimensional graphene macroassembly (GMA) fabricated by reduction of graphene oxides using NH₄OH, supercritically dried, and annealed at 1050 °C.
3 materials1 process step
FeOOH nanoparticles anchored inside 3D GMA by a sol-gel method, followed by additional supercritical drying and annealing at 515 °C to yield graphene/Fe₂O₃ hybrids.
2 materials1 process step
Titanium oxide graphene material prepared and annealed at 600 °C for 1 hour under N₂ flow, yielding anatase phase with grain size ~3 nm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-supported metal oxide monolith
electrode incorporating graphene-supported metal oxide monolith
Materials described outside the worked examples.
metal salt
graphene-supported metal oxide monolith
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET surface area (claimed minimum) | 500 m2/g | graphene-supported metal oxide monolith |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,109,845Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 shows a schematic illustration of the synthetic procedures for 3D graphene macroassembly (GMA)/Fe 2 O 3 hybrids. Step 1, three-dimensional GMA was …
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 3 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 0 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 0 3, …
FIG. 4 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 0 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 10 shows electrochemical measurements for titanium oxide graphene material. [0024]
FIG. 11 shows more electrochemical measurements for titanium oxide graphene material (annealed at 600 ° C for 1 hour under N 2 flow). [0025]
FIG. 12. (A) Nitrogen adsorption/desorption isotherms and (B) pore size distribution for graphene/Fe 2 O 3 hybrids. [0026]
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 15.(Differential capacity plots of graphene/(a +y)- Fe₂ O 3 56 wt.% Fe₂ O 3). The convoluted nature of the inset oxidation peaks can be seen. [0029]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 17. A comparison of simulated Li₂ O (cubic) diffraction patterns along < 100 > zone axis with the FFT pattern (inset) from our experiments. A good match is …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 20. Selected area diffraction (SAD) pattern taken from a(graphene/(a +y)- Fe₂ O₃ 40 wt.%) sample after 30 cycles and charged to the delithiated state (3. O …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
FIG. 22. The calculated ratio change (h'/a') after the lithiation, as a function of the initial particle shape defined by h/a (see Spherical-cap model section …
FIG. 23 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 O 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 O 3, …
FIG. 24 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 O 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 25. (a) Schematics of solid-electrolyte-interphase (SEI) formation on graphene surface upon discharge and its effect on suppressing surface reactions that …
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-supported metal oxide monolith, comprising: providing a graphene aerogel monolith; immersing said graphene aerogel monolith in a solution comprising at least one metal salt to form a mixture; curing said mixture to obtain a gel; and heating said gel to obtain a graphene-supported metal oxide monolith that comprises (i) a three-dimensional network of g raphene sheets crosslinked by covalent carbon bonds, and (ii) at least one metal oxide embedded inside said three-dimensional network, wherein the g raphene- supported metal oxide monolith is mesoporous, wherein the g raphene-supported metal oxide monolith has a surface area of at least 500 m 2/g, wherein the metal oxide accounts for 40-80 wt.% of the g raphene-supported metal oxide monolith. Currently amended
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds. Original
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds, and wherein the surfaces of the graphene sheets are substantially free of carbon nanoparticles. Original
The method of claim 1, wherein the solution further comprises at least one organic solvent. Original
The method of claim 1, wherein the solution further comprises at least one initiator. Original
The method of claim 1, wherein the solution further comprises at least one initiator, and wherein the molar ratio of the initiator to the metal salt is tuned to promote nanoparticle nucleation and anchoring on the surface of graphene sheets. Original
The method of claim 1, wherein the metal salt is an iron salt or a titanium salt. Original
The method of claim 1, wherein the metal salt is an iron salt, and the gel is heated under nitrogen at 400 ° C or more. Original
The method of claim 1, wherein the metal salt is a titanium salt, and the gel is heated under air at 250 ° C or more. Original
The method of claim 1, further comprising incorporating the graphene- supported metal oxide monolith into an electrode. Original
The method of claim 1, wherein the graphene aerogel monolith is obtained by: preparing a reaction mixture comprising a graphene oxide (GO) suspension and at least one catalyst; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel; and pyrolyzing the dry gel to produce the graphene aerogel. Original
The method of claim 1, SVG 15340875.05-23-2018.JHJOP02QRXEAPX1.CLM.3.14.388.1642.491.1699.svg Chemistry Black and white wherein the metal oxide copper, zin c, zirconium, tin, silicon, aluminum, thereof. Currently amended 0.19 0.343 comprises manganese, iron, cobalt, nickel, chromium, vanadium, titanium, or combinations
18-19. Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Three-dimensional graphene macroassembly (GMA) fabricated by reduction of graphene oxides using NH₄OH, supercritically dried, and annealed at 1050 °C.
3 materials1 process step
FeOOH nanoparticles anchored inside 3D GMA by a sol-gel method, followed by additional supercritical drying and annealing at 515 °C to yield graphene/Fe₂O₃ hybrids.
2 materials1 process step
Titanium oxide graphene material prepared and annealed at 600 °C for 1 hour under N₂ flow, yielding anatase phase with grain size ~3 nm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-supported metal oxide monolith
electrode incorporating graphene-supported metal oxide monolith
Materials described outside the worked examples.
metal salt
graphene-supported metal oxide monolith
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET surface area (claimed minimum) | 500 m2/g | graphene-supported metal oxide monolith |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,109,845Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 shows a schematic illustration of the synthetic procedures for 3D graphene macroassembly (GMA)/Fe 2 O 3 hybrids. Step 1, three-dimensional GMA was …
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 3 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 0 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 0 3, …
FIG. 4 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 0 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 10 shows electrochemical measurements for titanium oxide graphene material. [0024]
FIG. 11 shows more electrochemical measurements for titanium oxide graphene material (annealed at 600 ° C for 1 hour under N 2 flow). [0025]
FIG. 12. (A) Nitrogen adsorption/desorption isotherms and (B) pore size distribution for graphene/Fe 2 O 3 hybrids. [0026]
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 15.(Differential capacity plots of graphene/(a +y)- Fe₂ O 3 56 wt.% Fe₂ O 3). The convoluted nature of the inset oxidation peaks can be seen. [0029]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 17. A comparison of simulated Li₂ O (cubic) diffraction patterns along < 100 > zone axis with the FFT pattern (inset) from our experiments. A good match is …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 20. Selected area diffraction (SAD) pattern taken from a(graphene/(a +y)- Fe₂ O₃ 40 wt.%) sample after 30 cycles and charged to the delithiated state (3. O …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
FIG. 22. The calculated ratio change (h'/a') after the lithiation, as a function of the initial particle shape defined by h/a (see Spherical-cap model section …
FIG. 23 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 O 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 O 3, …
FIG. 24 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 O 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 25. (a) Schematics of solid-electrolyte-interphase (SEI) formation on graphene surface upon discharge and its effect on suppressing surface reactions that …
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-supported metal oxide monolith, comprising: providing a graphene aerogel monolith; immersing said graphene aerogel monolith in a solution comprising at least one metal salt to form a mixture; curing said mixture to obtain a gel; and heating said gel to obtain a graphene-supported metal oxide monolith that comprises (i) a three-dimensional network of g raphene sheets crosslinked by covalent carbon bonds, and (ii) at least one metal oxide embedded inside said three-dimensional network, wherein the g raphene- supported metal oxide monolith is mesoporous, wherein the g raphene-supported metal oxide monolith has a surface area of at least 500 m 2/g, wherein the metal oxide accounts for 40-80 wt.% of the g raphene-supported metal oxide monolith. Currently amended
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds. Original
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds, and wherein the surfaces of the graphene sheets are substantially free of carbon nanoparticles. Original
The method of claim 1, wherein the solution further comprises at least one organic solvent. Original
The method of claim 1, wherein the solution further comprises at least one initiator. Original
The method of claim 1, wherein the solution further comprises at least one initiator, and wherein the molar ratio of the initiator to the metal salt is tuned to promote nanoparticle nucleation and anchoring on the surface of graphene sheets. Original
The method of claim 1, wherein the metal salt is an iron salt or a titanium salt. Original
The method of claim 1, wherein the metal salt is an iron salt, and the gel is heated under nitrogen at 400 ° C or more. Original
The method of claim 1, wherein the metal salt is a titanium salt, and the gel is heated under air at 250 ° C or more. Original
The method of claim 1, further comprising incorporating the graphene- supported metal oxide monolith into an electrode. Original
The method of claim 1, wherein the graphene aerogel monolith is obtained by: preparing a reaction mixture comprising a graphene oxide (GO) suspension and at least one catalyst; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel; and pyrolyzing the dry gel to produce the graphene aerogel. Original
The method of claim 1, SVG 15340875.05-23-2018.JHJOP02QRXEAPX1.CLM.3.14.388.1642.491.1699.svg Chemistry Black and white wherein the metal oxide copper, zin c, zirconium, tin, silicon, aluminum, thereof. Currently amended 0.19 0.343 comprises manganese, iron, cobalt, nickel, chromium, vanadium, titanium, or combinations
18-19. Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Three-dimensional graphene macroassembly (GMA) fabricated by reduction of graphene oxides using NH₄OH, supercritically dried, and annealed at 1050 °C.
3 materials1 process step
FeOOH nanoparticles anchored inside 3D GMA by a sol-gel method, followed by additional supercritical drying and annealing at 515 °C to yield graphene/Fe₂O₃ hybrids.
2 materials1 process step
Titanium oxide graphene material prepared and annealed at 600 °C for 1 hour under N₂ flow, yielding anatase phase with grain size ~3 nm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-supported metal oxide monolith
electrode incorporating graphene-supported metal oxide monolith
Materials described outside the worked examples.
metal salt
graphene-supported metal oxide monolith
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET surface area (claimed minimum) | 500 m2/g | graphene-supported metal oxide monolith |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,109,845Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 shows a schematic illustration of the synthetic procedures for 3D graphene macroassembly (GMA)/Fe 2 O 3 hybrids. Step 1, three-dimensional GMA was …
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 3 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 0 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 0 3, …
FIG. 4 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 0 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 10 shows electrochemical measurements for titanium oxide graphene material. [0024]
FIG. 11 shows more electrochemical measurements for titanium oxide graphene material (annealed at 600 ° C for 1 hour under N 2 flow). [0025]
FIG. 12. (A) Nitrogen adsorption/desorption isotherms and (B) pore size distribution for graphene/Fe 2 O 3 hybrids. [0026]
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 15.(Differential capacity plots of graphene/(a +y)- Fe₂ O 3 56 wt.% Fe₂ O 3). The convoluted nature of the inset oxidation peaks can be seen. [0029]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 17. A comparison of simulated Li₂ O (cubic) diffraction patterns along < 100 > zone axis with the FFT pattern (inset) from our experiments. A good match is …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 20. Selected area diffraction (SAD) pattern taken from a(graphene/(a +y)- Fe₂ O₃ 40 wt.%) sample after 30 cycles and charged to the delithiated state (3. O …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
FIG. 22. The calculated ratio change (h'/a') after the lithiation, as a function of the initial particle shape defined by h/a (see Spherical-cap model section …
FIG. 23 shows specific capacity, rate performance, and cycle stability of graphene/Fe 2 O 3 hybrids. The observed specific capacities of (A) graphene/Fe 2 O 3, …
FIG. 24 shows selected discharge/charge cycles for (A) pure GMA and (C) graphene/Fe 2 O 3, and their corresponding differential capacity curves, (B) and (D), …
FIG. 25. (a) Schematics of solid-electrolyte-interphase (SEI) formation on graphene surface upon discharge and its effect on suppressing surface reactions that …
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-supported metal oxide monolith, comprising: providing a graphene aerogel monolith; immersing said graphene aerogel monolith in a solution comprising at least one metal salt to form a mixture; curing said mixture to obtain a gel; and heating said gel to obtain a graphene-supported metal oxide monolith that comprises (i) a three-dimensional network of g raphene sheets crosslinked by covalent carbon bonds, and (ii) at least one metal oxide embedded inside said three-dimensional network, wherein the g raphene- supported metal oxide monolith is mesoporous, wherein the g raphene-supported metal oxide monolith has a surface area of at least 500 m 2/g, wherein the metal oxide accounts for 40-80 wt.% of the g raphene-supported metal oxide monolith. Currently amended
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds. Original
The method of claim 1, wherein the graphene aerogel monolith comprises a three-dimensional network of graphene sheets crosslinked by covalent carbon bonds, and wherein the surfaces of the graphene sheets are substantially free of carbon nanoparticles. Original
The method of claim 1, wherein the solution further comprises at least one organic solvent. Original
The method of claim 1, wherein the solution further comprises at least one initiator. Original
The method of claim 1, wherein the solution further comprises at least one initiator, and wherein the molar ratio of the initiator to the metal salt is tuned to promote nanoparticle nucleation and anchoring on the surface of graphene sheets. Original
The method of claim 1, wherein the metal salt is an iron salt or a titanium salt. Original
The method of claim 1, wherein the metal salt is an iron salt, and the gel is heated under nitrogen at 400 ° C or more. Original
The method of claim 1, wherein the metal salt is a titanium salt, and the gel is heated under air at 250 ° C or more. Original
The method of claim 1, further comprising incorporating the graphene- supported metal oxide monolith into an electrode. Original
The method of claim 1, wherein the graphene aerogel monolith is obtained by: preparing a reaction mixture comprising a graphene oxide (GO) suspension and at least one catalyst; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel; and pyrolyzing the dry gel to produce the graphene aerogel. Original
The method of claim 1, SVG 15340875.05-23-2018.JHJOP02QRXEAPX1.CLM.3.14.388.1642.491.1699.svg Chemistry Black and white wherein the metal oxide copper, zin c, zirconium, tin, silicon, aluminum, thereof. Currently amended 0.19 0.343 comprises manganese, iron, cobalt, nickel, chromium, vanadium, titanium, or combinations
18-19. Canceled
Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Three-dimensional graphene macroassembly (GMA) fabricated by reduction of graphene oxides using NH₄OH, supercritically dried, and annealed at 1050 °C.
3 materials1 process step
FeOOH nanoparticles anchored inside 3D GMA by a sol-gel method, followed by additional supercritical drying and annealing at 515 °C to yield graphene/Fe₂O₃ hybrids.
2 materials1 process step
Titanium oxide graphene material prepared and annealed at 600 °C for 1 hour under N₂ flow, yielding anatase phase with grain size ~3 nm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-supported metal oxide monolith
electrode incorporating graphene-supported metal oxide monolith
Materials described outside the worked examples.
metal salt
graphene-supported metal oxide monolith
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
BET surface area (claimed minimum) | 500 m2/g | graphene-supported metal oxide monolith |
Related documents with shared materials, methods, properties, or citations.
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
metal oxide weight fraction in monolith |
| 40–80 wt.% |
graphene-supported metal oxide monolith |
anatase TiO2 grain size after annealing at 600 °C 1 h N2 | 3 nm | TiO₂ |
Thickness | ≤ 50 nm | — |
Voltage | ≤ 0.5 V | — |
Thickness | ≥ 250 nm | — |
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
metal oxide weight fraction in monolith |
| 40–80 wt.% |
graphene-supported metal oxide monolith |
anatase TiO2 grain size after annealing at 600 °C 1 h N2 | 3 nm | TiO₂ |
Thickness | ≤ 50 nm | — |
Voltage | ≤ 0.5 V | — |
Thickness | ≥ 250 nm | — |
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
metal oxide weight fraction in monolith |
| 40–80 wt.% |
graphene-supported metal oxide monolith |
anatase TiO2 grain size after annealing at 600 °C 1 h N2 | 3 nm | TiO₂ |
Thickness | ≤ 50 nm | — |
Voltage | ≤ 0.5 V | — |
Thickness | ≥ 250 nm | — |
FIG. 2 shows microstructures of the as-synthesized graphene macroassembly (GMA) and graphene/Fe 2 O 3 hybrids. (A) A TEM image of GMA. (B) and (C), SEM and TEM …
FIG. 5 shows surface morphologies of GMA and graphene/Fe₂ 0 3 after 30 cycles of electrochemical testing. (A) and (B), cross-section SEM images of GMA, and (C) …
FIG. 6 shows microstructures of graphene/Fe₂ 0 3 after 30 cycles and in the lithiation state. (A) A low-magnification TEM image of graphene/Fe 2 0 3. Some …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIG. 7. (A) A summary of theoretical specific capacities (C), electrical conductivities (a), and densities (p) of different transition metal oxides as anode …
FIGS. 8- 11 show x-ray, Raman, and electrochemical characterization. [0116] After annealing, amorphous TiO 2 transit into anatase phase with grain size of~ …
FIG. 9 shows Raman spectra for titanium oxide graphene material. Raman peaks for titania became stronger after annealing at 600 ° C for 1 hour under N 2 flow. …
FIG. 13. Raman spectra of the 3D graphene and a graphene/Fe 2 O 3 hybrid sample (containing both a- and y-Fe 2 O 3). [0027]
FIG. 14. XRD patterns of two representative graphene/Fe 2 O 3 samples. One contains a- and y- Fe 2 O 3 phases, and the other has 100 % y- Fe 2 O 3. [0028]
FIG. 16.(Additional TEM image of graphene/(a +y)- Fe₂ O 3 40 wt.%), indicating the faceted nature of as-grown particles as manifested by the rather straight …
FIG. 18. A bright-field TEM image of the(lithiated graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles, showing a partially lithiated particle. [0032]
FIG. 19.(Microstructures of graphene/(a +y)- Fe₂ O 3 40 wt.%) after 30 cycles. The final state of the sample is charged to 3V (i.e., delithiated). (A) A TEM …
FIG. 21.(Bright-field TEM images of graphene/y- Fe₂ O 3 56 wt.%) in (A) the as- synthesized state, and (B) the lithiated state after 5 cycles. The particle …
metal oxide weight fraction in monolith |
| 40–80 wt.% |
graphene-supported metal oxide monolith |
anatase TiO2 grain size after annealing at 600 °C 1 h N2 | 3 nm | TiO₂ |
Thickness | ≤ 50 nm | — |
Voltage | ≤ 0.5 V | — |
Thickness | ≥ 250 nm | — |