Patent
US 9,145,302THE METHOD FOR PRODUCING GRAPHENE BY CHEMICAL EXFOLIATION
Won Kook CHOI
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 9,145,302Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically shows a procedure whereby a layer of graphite oxide is exfoliated from the surface of zinc oxide nanoparticles;
FIG. 2 schematically shows chemical bonding between the functional groups 4 (carboxyl, hydroxyl and epoxy groups) on an exfoliated carbon monolayer and zinc …
FIG. 3 schematically shows a zinc oxide nanoparticle of a quasi metal oxide-graphene core-shell structure wherein graphene surrounds the nanoparticle; 5
FIG. 4 schematically shows graphene obtained by removing zinc oxide from a nanoparticle of a quasi zinc oxide-graphene core-shell structure;
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 7 shows an X-ray diffraction pattern of particles of a quasi zinc oxide-graphene core-shell structure and graphene (top right) prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 10 shows an analysis result of graphene prepared in Example 1 by electron energy loss spectroscopy (EELS);
FIG. 11 shows an energy-dispersive X-ray emission (EDX) spectrum of graphene prepared in
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
FIG. 14 shows an X-ray diffraction pattern of particles of a quasi copper oxide-graphene core-shell structure prepared in Example 2. It should be understood …
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 preparing graphene comprising: mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O 3, In₂₀ 3, Li₂ CO 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to components to form graphene, wherein grap hene com p rises a structure of one- atom-thick p lanar sheet of carbon atoms.
The method for preparing graphene according to claim 1, wherein the solid components comprise a metal oxide-graphene core-shell in which graphene surrounds a core comprising nanoparticles of the metal oxide. previously presented
The method for preparing graphene according to claim 1, further comprising: treating graphite powder into an acid solution comprising sulfuric acid and nitric acid to form graphite oxide; and drying the graphite oxide to form the graphite oxide powder.
The method for preparing graphene according to claim 1, wherein removing the metal oxide away from the solid components to form graphene by using an acid selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid and a mixture thereof. 6-8. (canceled)
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from [[BaC O 3,]] Bi₂ O 3, B203, [[CaC O 3,]] Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, S nO-HfO₄₂ In₂₀ 3, [[Li₂CO3,]] IrO 2, P₂₀-sPO-CaO.1 Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, [[Sn O 2,]] and SrC O3.
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from Y₂ 0 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf O 2,]] IrO2, Nb₂ 05, PbO, and Sb₂ O3.
canceled
canceled
canceled
canceled
Nanoparticles comprising: a core comprising a metal oxide selected from the group consisting of BaC O3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂ 0 3, [[RuO2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O3, In₂₀ 3, IrO 2, P₂ 05, P 0 2, C aO, Sc₂ O 3, Nb₂ O5, PbO, Sb₂ O 3, and SrC O 3[[,]]; and graphene surrounding the core, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms. currently amended
canceled
A method for preparing graphene comprising: Page 3 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930684.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white treating graphite powder mixed with an acid solution consisting essentially of sulfuric acid and nitric acid to form a graphite oxide dispersion; isolating graphite oxide powder from the graphite oxide dispersion; mixing together the graphite oxide powder and a reaction solvent to prepare a graphite oxide dispersion; mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, MeO₀-R2iO₂ PdO, AgO, C dO, [[Hf O 2,]] In₂₀ 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms.
1 2. The method of claim 11, wherein the acid solution for treating graphite powder comprises sulfuric acid at about 18M and nitric acid at about 1 7M mixed together at a respective volume ratio of about 3:1.
The method of claim 11, wherein isolating the graphite oxide Page 5 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930686.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white powder comprises: centrifuging the graphite oxide dispersion u sing-wate; decanting and washing the centrifuged graphite oxide dispersion with ethanol; and drying the decanted and washed the centrifuged graphite oxide dispersion to obtain the graphite oxide powder.
The method of claim 11, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, P₂₀ 5, P 0 2, and C aO.
The method of claim 11, wherein the metal oxide is selected from the group consisting of Ce₀ 2, GeO, Y₂ 0 3, R uO₂-HfOG₂ In₂₀ 3, IrO 2, Sc₂ O 3, Nb₂ 05, Sb₂ O 3, and SrC O3. Page 6 of SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930687.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white
The method of claim 11, wherein the metal oxide comprises Nb₂O5.
The method of claim 11, wherein the metal oxide comprises CeO2.
The method of claim 11, wherein the metal oxide comprises [[Hf 0 2]] S c203 Page 7 of 15
The method of clai 11, A method for prep arin g gra p hene com p risin g: treatin g gra p hite p owder mixed with an acid solution consistin g essentially Page 4 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930685.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white of sulfuric acid and nitric acid to form a gra p hite oxide dis p ersion; isolatin g gra p hite oxide p owder from the gra p hite oxide dis p ersion; mixing together the gra p hite oxide p owder and a reaction solvent to prep are a gra p hite oxide dis p ersion; mixing together a gra p hite oxide dis p ersion and a metal precursor solution to obtain solid com p onents to form metal-oxide- grap hene nano p article, wherein the metal oxide is selected from the group consistin g of BaC O3, Bi₂₀ 3, B₂₀ 3, CaC O3, Ce O2, GeO, Y₂₀ 3, MoO, Ru O2, PdO, AgO, CdO, Hf O2, I n20 3, IrO2, P₂₀ 5, P02 CaO, Sc₂ 03, Nb₂ 05, PbO, Sb₂ 03, and SrC O3; sep aratin g solid com p onents from the reaction solvent; washing the se p arated solid com p onents with a washin g solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein gra p hene com p rises a structure of one-atom-thick p lanar sheet of carbon atoms, wherein treating comprises: sonicating and heating the graphite powder mixed with the acid solution to form a sonicated dispersion; and keeping the sonicated dispersion for about 4 days at room temperature.
The method of claim 13, wherein sonicating and heating is performed at about 45 0 C with 200 W for about 2 hours.
Layer stacks claimed or described, ordered top of device to substrate.
quasi metal oxide-graphene core-shell nanoparticle
Materials described outside the worked examples.
graphene
metal oxide (generic, claimed group)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,145,302Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically shows a procedure whereby a layer of graphite oxide is exfoliated from the surface of zinc oxide nanoparticles;
FIG. 2 schematically shows chemical bonding between the functional groups 4 (carboxyl, hydroxyl and epoxy groups) on an exfoliated carbon monolayer and zinc …
FIG. 3 schematically shows a zinc oxide nanoparticle of a quasi metal oxide-graphene core-shell structure wherein graphene surrounds the nanoparticle; 5
FIG. 4 schematically shows graphene obtained by removing zinc oxide from a nanoparticle of a quasi zinc oxide-graphene core-shell structure;
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 7 shows an X-ray diffraction pattern of particles of a quasi zinc oxide-graphene core-shell structure and graphene (top right) prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 10 shows an analysis result of graphene prepared in Example 1 by electron energy loss spectroscopy (EELS);
FIG. 11 shows an energy-dispersive X-ray emission (EDX) spectrum of graphene prepared in
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
FIG. 14 shows an X-ray diffraction pattern of particles of a quasi copper oxide-graphene core-shell structure prepared in Example 2. It should be understood …
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 preparing graphene comprising: mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O 3, In₂₀ 3, Li₂ CO 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to components to form graphene, wherein grap hene com p rises a structure of one- atom-thick p lanar sheet of carbon atoms.
The method for preparing graphene according to claim 1, wherein the solid components comprise a metal oxide-graphene core-shell in which graphene surrounds a core comprising nanoparticles of the metal oxide. previously presented
The method for preparing graphene according to claim 1, further comprising: treating graphite powder into an acid solution comprising sulfuric acid and nitric acid to form graphite oxide; and drying the graphite oxide to form the graphite oxide powder.
The method for preparing graphene according to claim 1, wherein removing the metal oxide away from the solid components to form graphene by using an acid selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid and a mixture thereof. 6-8. (canceled)
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from [[BaC O 3,]] Bi₂ O 3, B203, [[CaC O 3,]] Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, S nO-HfO₄₂ In₂₀ 3, [[Li₂CO3,]] IrO 2, P₂₀-sPO-CaO.1 Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, [[Sn O 2,]] and SrC O3.
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from Y₂ 0 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf O 2,]] IrO2, Nb₂ 05, PbO, and Sb₂ O3.
canceled
canceled
canceled
canceled
Nanoparticles comprising: a core comprising a metal oxide selected from the group consisting of BaC O3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂ 0 3, [[RuO2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O3, In₂₀ 3, IrO 2, P₂ 05, P 0 2, C aO, Sc₂ O 3, Nb₂ O5, PbO, Sb₂ O 3, and SrC O 3[[,]]; and graphene surrounding the core, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms. currently amended
canceled
A method for preparing graphene comprising: Page 3 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930684.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white treating graphite powder mixed with an acid solution consisting essentially of sulfuric acid and nitric acid to form a graphite oxide dispersion; isolating graphite oxide powder from the graphite oxide dispersion; mixing together the graphite oxide powder and a reaction solvent to prepare a graphite oxide dispersion; mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, MeO₀-R2iO₂ PdO, AgO, C dO, [[Hf O 2,]] In₂₀ 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms.
1 2. The method of claim 11, wherein the acid solution for treating graphite powder comprises sulfuric acid at about 18M and nitric acid at about 1 7M mixed together at a respective volume ratio of about 3:1.
The method of claim 11, wherein isolating the graphite oxide Page 5 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930686.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white powder comprises: centrifuging the graphite oxide dispersion u sing-wate; decanting and washing the centrifuged graphite oxide dispersion with ethanol; and drying the decanted and washed the centrifuged graphite oxide dispersion to obtain the graphite oxide powder.
The method of claim 11, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, P₂₀ 5, P 0 2, and C aO.
The method of claim 11, wherein the metal oxide is selected from the group consisting of Ce₀ 2, GeO, Y₂ 0 3, R uO₂-HfOG₂ In₂₀ 3, IrO 2, Sc₂ O 3, Nb₂ 05, Sb₂ O 3, and SrC O3. Page 6 of SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930687.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white
The method of claim 11, wherein the metal oxide comprises Nb₂O5.
The method of claim 11, wherein the metal oxide comprises CeO2.
The method of claim 11, wherein the metal oxide comprises [[Hf 0 2]] S c203 Page 7 of 15
The method of clai 11, A method for prep arin g gra p hene com p risin g: treatin g gra p hite p owder mixed with an acid solution consistin g essentially Page 4 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930685.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white of sulfuric acid and nitric acid to form a gra p hite oxide dis p ersion; isolatin g gra p hite oxide p owder from the gra p hite oxide dis p ersion; mixing together the gra p hite oxide p owder and a reaction solvent to prep are a gra p hite oxide dis p ersion; mixing together a gra p hite oxide dis p ersion and a metal precursor solution to obtain solid com p onents to form metal-oxide- grap hene nano p article, wherein the metal oxide is selected from the group consistin g of BaC O3, Bi₂₀ 3, B₂₀ 3, CaC O3, Ce O2, GeO, Y₂₀ 3, MoO, Ru O2, PdO, AgO, CdO, Hf O2, I n20 3, IrO2, P₂₀ 5, P02 CaO, Sc₂ 03, Nb₂ 05, PbO, Sb₂ 03, and SrC O3; sep aratin g solid com p onents from the reaction solvent; washing the se p arated solid com p onents with a washin g solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein gra p hene com p rises a structure of one-atom-thick p lanar sheet of carbon atoms, wherein treating comprises: sonicating and heating the graphite powder mixed with the acid solution to form a sonicated dispersion; and keeping the sonicated dispersion for about 4 days at room temperature.
The method of claim 13, wherein sonicating and heating is performed at about 45 0 C with 200 W for about 2 hours.
Layer stacks claimed or described, ordered top of device to substrate.
quasi metal oxide-graphene core-shell nanoparticle
Materials described outside the worked examples.
graphene
metal oxide (generic, claimed group)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,145,302Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically shows a procedure whereby a layer of graphite oxide is exfoliated from the surface of zinc oxide nanoparticles;
FIG. 2 schematically shows chemical bonding between the functional groups 4 (carboxyl, hydroxyl and epoxy groups) on an exfoliated carbon monolayer and zinc …
FIG. 3 schematically shows a zinc oxide nanoparticle of a quasi metal oxide-graphene core-shell structure wherein graphene surrounds the nanoparticle; 5
FIG. 4 schematically shows graphene obtained by removing zinc oxide from a nanoparticle of a quasi zinc oxide-graphene core-shell structure;
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 7 shows an X-ray diffraction pattern of particles of a quasi zinc oxide-graphene core-shell structure and graphene (top right) prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 10 shows an analysis result of graphene prepared in Example 1 by electron energy loss spectroscopy (EELS);
FIG. 11 shows an energy-dispersive X-ray emission (EDX) spectrum of graphene prepared in
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
FIG. 14 shows an X-ray diffraction pattern of particles of a quasi copper oxide-graphene core-shell structure prepared in Example 2. It should be understood …
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 preparing graphene comprising: mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O 3, In₂₀ 3, Li₂ CO 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to components to form graphene, wherein grap hene com p rises a structure of one- atom-thick p lanar sheet of carbon atoms.
The method for preparing graphene according to claim 1, wherein the solid components comprise a metal oxide-graphene core-shell in which graphene surrounds a core comprising nanoparticles of the metal oxide. previously presented
The method for preparing graphene according to claim 1, further comprising: treating graphite powder into an acid solution comprising sulfuric acid and nitric acid to form graphite oxide; and drying the graphite oxide to form the graphite oxide powder.
The method for preparing graphene according to claim 1, wherein removing the metal oxide away from the solid components to form graphene by using an acid selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid and a mixture thereof. 6-8. (canceled)
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from [[BaC O 3,]] Bi₂ O 3, B203, [[CaC O 3,]] Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, S nO-HfO₄₂ In₂₀ 3, [[Li₂CO3,]] IrO 2, P₂₀-sPO-CaO.1 Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, [[Sn O 2,]] and SrC O3.
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from Y₂ 0 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf O 2,]] IrO2, Nb₂ 05, PbO, and Sb₂ O3.
canceled
canceled
canceled
canceled
Nanoparticles comprising: a core comprising a metal oxide selected from the group consisting of BaC O3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂ 0 3, [[RuO2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O3, In₂₀ 3, IrO 2, P₂ 05, P 0 2, C aO, Sc₂ O 3, Nb₂ O5, PbO, Sb₂ O 3, and SrC O 3[[,]]; and graphene surrounding the core, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms. currently amended
canceled
A method for preparing graphene comprising: Page 3 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930684.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white treating graphite powder mixed with an acid solution consisting essentially of sulfuric acid and nitric acid to form a graphite oxide dispersion; isolating graphite oxide powder from the graphite oxide dispersion; mixing together the graphite oxide powder and a reaction solvent to prepare a graphite oxide dispersion; mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, MeO₀-R2iO₂ PdO, AgO, C dO, [[Hf O 2,]] In₂₀ 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms.
1 2. The method of claim 11, wherein the acid solution for treating graphite powder comprises sulfuric acid at about 18M and nitric acid at about 1 7M mixed together at a respective volume ratio of about 3:1.
The method of claim 11, wherein isolating the graphite oxide Page 5 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930686.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white powder comprises: centrifuging the graphite oxide dispersion u sing-wate; decanting and washing the centrifuged graphite oxide dispersion with ethanol; and drying the decanted and washed the centrifuged graphite oxide dispersion to obtain the graphite oxide powder.
The method of claim 11, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, P₂₀ 5, P 0 2, and C aO.
The method of claim 11, wherein the metal oxide is selected from the group consisting of Ce₀ 2, GeO, Y₂ 0 3, R uO₂-HfOG₂ In₂₀ 3, IrO 2, Sc₂ O 3, Nb₂ 05, Sb₂ O 3, and SrC O3. Page 6 of SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930687.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white
The method of claim 11, wherein the metal oxide comprises Nb₂O5.
The method of claim 11, wherein the metal oxide comprises CeO2.
The method of claim 11, wherein the metal oxide comprises [[Hf 0 2]] S c203 Page 7 of 15
The method of clai 11, A method for prep arin g gra p hene com p risin g: treatin g gra p hite p owder mixed with an acid solution consistin g essentially Page 4 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930685.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white of sulfuric acid and nitric acid to form a gra p hite oxide dis p ersion; isolatin g gra p hite oxide p owder from the gra p hite oxide dis p ersion; mixing together the gra p hite oxide p owder and a reaction solvent to prep are a gra p hite oxide dis p ersion; mixing together a gra p hite oxide dis p ersion and a metal precursor solution to obtain solid com p onents to form metal-oxide- grap hene nano p article, wherein the metal oxide is selected from the group consistin g of BaC O3, Bi₂₀ 3, B₂₀ 3, CaC O3, Ce O2, GeO, Y₂₀ 3, MoO, Ru O2, PdO, AgO, CdO, Hf O2, I n20 3, IrO2, P₂₀ 5, P02 CaO, Sc₂ 03, Nb₂ 05, PbO, Sb₂ 03, and SrC O3; sep aratin g solid com p onents from the reaction solvent; washing the se p arated solid com p onents with a washin g solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein gra p hene com p rises a structure of one-atom-thick p lanar sheet of carbon atoms, wherein treating comprises: sonicating and heating the graphite powder mixed with the acid solution to form a sonicated dispersion; and keeping the sonicated dispersion for about 4 days at room temperature.
The method of claim 13, wherein sonicating and heating is performed at about 45 0 C with 200 W for about 2 hours.
Layer stacks claimed or described, ordered top of device to substrate.
quasi metal oxide-graphene core-shell nanoparticle
Materials described outside the worked examples.
graphene
metal oxide (generic, claimed group)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,145,302Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 schematically shows a procedure whereby a layer of graphite oxide is exfoliated from the surface of zinc oxide nanoparticles;
FIG. 2 schematically shows chemical bonding between the functional groups 4 (carboxyl, hydroxyl and epoxy groups) on an exfoliated carbon monolayer and zinc …
FIG. 3 schematically shows a zinc oxide nanoparticle of a quasi metal oxide-graphene core-shell structure wherein graphene surrounds the nanoparticle; 5
FIG. 4 schematically shows graphene obtained by removing zinc oxide from a nanoparticle of a quasi zinc oxide-graphene core-shell structure;
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 7 shows an X-ray diffraction pattern of particles of a quasi zinc oxide-graphene core-shell structure and graphene (top right) prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 10 shows an analysis result of graphene prepared in Example 1 by electron energy loss spectroscopy (EELS);
FIG. 11 shows an energy-dispersive X-ray emission (EDX) spectrum of graphene prepared in
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
FIG. 14 shows an X-ray diffraction pattern of particles of a quasi copper oxide-graphene core-shell structure prepared in Example 2. It should be understood …
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A method for preparing graphene comprising: mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O 3, In₂₀ 3, Li₂ CO 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to components to form graphene, wherein grap hene com p rises a structure of one- atom-thick p lanar sheet of carbon atoms.
The method for preparing graphene according to claim 1, wherein the solid components comprise a metal oxide-graphene core-shell in which graphene surrounds a core comprising nanoparticles of the metal oxide. previously presented
The method for preparing graphene according to claim 1, further comprising: treating graphite powder into an acid solution comprising sulfuric acid and nitric acid to form graphite oxide; and drying the graphite oxide to form the graphite oxide powder.
The method for preparing graphene according to claim 1, wherein removing the metal oxide away from the solid components to form graphene by using an acid selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid and a mixture thereof. 6-8. (canceled)
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from [[BaC O 3,]] Bi₂ O 3, B203, [[CaC O 3,]] Ce₀ 2, GeO, Y₂₀ 3, [[Ru O 2,]] PdO, AgO, C dO, S nO-HfO₄₂ In₂₀ 3, [[Li₂CO3,]] IrO 2, P₂₀-sPO-CaO.1 Sc₂ O 3, Nb₂ 05, PbO, Sb₂ O 3, [[Sn O 2,]] and SrC O3.
The method for preparing graphene according to claim 1, wherein the metal oxide is selected from Y₂ 0 3, [[Ru O 2,]] PdO, AgO, C dO, [[Hf O 2,]] IrO2, Nb₂ 05, PbO, and Sb₂ O3.
canceled
canceled
canceled
canceled
Nanoparticles comprising: a core comprising a metal oxide selected from the group consisting of BaC O3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂ 0 3, [[RuO2,]] PdO, AgO, C dO, [[Hf 0 2,]] Ga₂ O3, In₂₀ 3, IrO 2, P₂ 05, P 0 2, C aO, Sc₂ O 3, Nb₂ O5, PbO, Sb₂ O 3, and SrC O 3[[,]]; and graphene surrounding the core, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms. currently amended
canceled
A method for preparing graphene comprising: Page 3 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930684.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white treating graphite powder mixed with an acid solution consisting essentially of sulfuric acid and nitric acid to form a graphite oxide dispersion; isolating graphite oxide powder from the graphite oxide dispersion; mixing together the graphite oxide powder and a reaction solvent to prepare a graphite oxide dispersion; mixing together a graphite oxide dispersion and a metal precursor solution to obtain solid components to form metal-oxide-graphene nanoparticle, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, Ce₀ 2, GeO, Y₂₀ 3, MeO₀-R2iO₂ PdO, AgO, C dO, [[Hf O 2,]] In₂₀ 3, IrO 2, P₂₀ 5, P 0 2, C aO, Sc₂ O3, Nb₂ 05, PbO, Sb₂ O 3, and SrC O3; separating solid components from the reaction solvent; washing the separated solid components with a washing solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein grap hene com p rises a structure of one-atom-thick pl anar sheet of carbon atoms.
1 2. The method of claim 11, wherein the acid solution for treating graphite powder comprises sulfuric acid at about 18M and nitric acid at about 1 7M mixed together at a respective volume ratio of about 3:1.
The method of claim 11, wherein isolating the graphite oxide Page 5 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930686.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white powder comprises: centrifuging the graphite oxide dispersion u sing-wate; decanting and washing the centrifuged graphite oxide dispersion with ethanol; and drying the decanted and washed the centrifuged graphite oxide dispersion to obtain the graphite oxide powder.
The method of claim 11, wherein the metal oxide is selected from the group consisting of BaC O 3, Bi₂ O 3, B203, CaC03, P₂₀ 5, P 0 2, and C aO.
The method of claim 11, wherein the metal oxide is selected from the group consisting of Ce₀ 2, GeO, Y₂ 0 3, R uO₂-HfOG₂ In₂₀ 3, IrO 2, Sc₂ O 3, Nb₂ 05, Sb₂ O 3, and SrC O3. Page 6 of SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930687.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white
The method of claim 11, wherein the metal oxide comprises Nb₂O5.
The method of claim 11, wherein the metal oxide comprises CeO2.
The method of claim 11, wherein the metal oxide comprises [[Hf 0 2]] S c203 Page 7 of 15
The method of clai 11, A method for prep arin g gra p hene com p risin g: treatin g gra p hite p owder mixed with an acid solution consistin g essentially Page 4 of 15 SVG 13193777.03-24-2015.I₇P₀BUQMPXXIFW1.CLM12930685.1.301.160.2248.264.svg 0.347 6.49 Graph Black and white of sulfuric acid and nitric acid to form a gra p hite oxide dis p ersion; isolatin g gra p hite oxide p owder from the gra p hite oxide dis p ersion; mixing together the gra p hite oxide p owder and a reaction solvent to prep are a gra p hite oxide dis p ersion; mixing together a gra p hite oxide dis p ersion and a metal precursor solution to obtain solid com p onents to form metal-oxide- grap hene nano p article, wherein the metal oxide is selected from the group consistin g of BaC O3, Bi₂₀ 3, B₂₀ 3, CaC O3, Ce O2, GeO, Y₂₀ 3, MoO, Ru O2, PdO, AgO, CdO, Hf O2, I n20 3, IrO2, P₂₀ 5, P02 CaO, Sc₂ 03, Nb₂ 05, PbO, Sb₂ 03, and SrC O3; sep aratin g solid com p onents from the reaction solvent; washing the se p arated solid com p onents with a washin g solvent; and removing the metal oxide with acid away from the solid components to form graphene, wherein gra p hene com p rises a structure of one-atom-thick p lanar sheet of carbon atoms, wherein treating comprises: sonicating and heating the graphite powder mixed with the acid solution to form a sonicated dispersion; and keeping the sonicated dispersion for about 4 days at room temperature.
The method of claim 13, wherein sonicating and heating is performed at about 45 0 C with 200 W for about 2 hours.
Layer stacks claimed or described, ordered top of device to substrate.
quasi metal oxide-graphene core-shell nanoparticle
Materials described outside the worked examples.
graphene
metal oxide (generic, claimed group)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 5 shows a transmission electron microscopic image of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1;
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Related documents with shared materials, methods, properties, or citations.
graphite oxide
sulfuric acid
H₂SO₄
nitric acid
HNO₃
graphite powder
acid for metal oxide removal (HCl, HNO3, H₂SO₄ or mixture)
niobium pentoxide
Nb₂O₅
cerium dioxide
CeO₂
scandium oxide
Sc₂O₃
metal oxide nanoparticles (description, broader list including ZnO, CuO, etc.)
N,N-dimethylformamide
DMF
N,N-diethylformamide
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
graphite oxide
sulfuric acid
H₂SO₄
nitric acid
HNO₃
graphite powder
acid for metal oxide removal (HCl, HNO3, H₂SO₄ or mixture)
niobium pentoxide
Nb₂O₅
cerium dioxide
CeO₂
scandium oxide
Sc₂O₃
metal oxide nanoparticles (description, broader list including ZnO, CuO, etc.)
N,N-dimethylformamide
DMF
N,N-diethylformamide
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
graphite oxide
sulfuric acid
H₂SO₄
nitric acid
HNO₃
graphite powder
acid for metal oxide removal (HCl, HNO3, H₂SO₄ or mixture)
niobium pentoxide
Nb₂O₅
cerium dioxide
CeO₂
scandium oxide
Sc₂O₃
metal oxide nanoparticles (description, broader list including ZnO, CuO, etc.)
N,N-dimethylformamide
DMF
N,N-diethylformamide
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.
graphite oxide
sulfuric acid
H₂SO₄
nitric acid
HNO₃
graphite powder
acid for metal oxide removal (HCl, HNO3, H₂SO₄ or mixture)
niobium pentoxide
Nb₂O₅
cerium dioxide
CeO₂
scandium oxide
Sc₂O₃
metal oxide nanoparticles (description, broader list including ZnO, CuO, etc.)
N,N-dimethylformamide
DMF
N,N-diethylformamide
FIG. 6 shows a transmission electron microscopic image and a scanning 10 electron microscopic image of graphene prepared in Example 1;
FIG. 8 shows a Raman spectrum of particles of a quasi zinc oxide-graphene core-shell structure prepared in Example 1; 15
FIG. 9 shows a Raman spectrum of graphene prepared in Example 1;
FIG. 12 shows an X-ray photoelectron spectroscopy (XPS) spectrum of graphene prepared in Example 1;
FIG. 13 shows a high-resolution transmission electron microscopic image of thus prepared particles of a quasi copper oxide-graphene core-shell structure.