Patent
US 9,738,528GRAPHENE, METHOD AND APPARATUS FOR PREPARING GRAPHENE
Jin Seo LEE
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 9,738,528Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 and 2, the apparatus for preparing the graphene according to an exemplary embodiment of the present invention includes a mixing bath 100 forming a …
FIG. 2 exemplarily shows an apparatus for preparing a graphene according to an exemplary embodiment of the present invention.
FIG. 3 shows an infrared spectroscopy spectrum of graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 4 shows Raman spectrum of graphenes obtained by Example 1 25 and Comparative Example 1 of the present invention. 5
FIG. 5 shows scanning electron microscope (SEM) images of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. Referring to
FIG. 6, it could be confirmed that weight loss was shown around 200 0C in Comparative Example 1 The weight loss is caused by pyrolysis of impurities such as …
FIG. 7 shows XRD spectrum of a graphite oxide obtained by Preparation Example 1, the graphenes obtained by Example 1 and Comparative Example 1 of the present …
FIG. 8 shows transmission electron microscope (TEM) images of the 10 graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 9 shows graph showing electrical conductivity of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. 15 [Description …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
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A method for preparing a graphene comprising: forming a mixed solution including a graphite oxide, a solvent, a first oxidizing agent; and a sulfur compound or a nitrogen compound; forming the graphene by reacting the mixed solution under a subcritical condition or a supercritical condition of the solvent; and recovering the graphene -.; wherein the sulfur compound is represented by the following Chemical Formula 1, and the nitrogen compound is represented by the following Chemical Formula 2: [Chemical Formula 1 HO A 1-SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.17.655.1854.867.1909.svg 0.183 0.707 Chemistry Black and white -OH in Chemical Formula 1, Al and A₂ are each independently linear or branched C₁-C₁₀ alkylene group or C₆-C₂₀ arylene group, and Q is a sulfur atom (-S-) or a sulfone group(-(O=S=0)-), and [Chemical Formula 2. R 2 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.22.394.2333.545.2529.svg 0.653 0.503 Chemistry Black and white R 4 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.24.450.2532.510.2585.svg 0.177 0.20 Chemistry Black and white in Chemical Formula 2, at least one of R₁ to R₄ is a nitro group (- NO₂), and the remainder is hydrogen, linear or branched C₁-C₇ alkyl group or C₆-C₂₀ aryl group.
Page 2 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of 9. The method of claim 7, wherein the solvent includes water, carbon dioxide, or mixtures thereof. original
The method of claim 7, wherein the graphite oxide is formed by treating a graphite oxide precursor with an acid and a second oxidizing agent.
1 2. The method of claim 7, wherein the first oxidizing agent is at least one kind selected from the group consisiting of oxygen, ozone, and hydrogen peroxide.
The method of claim 7, wherein the graphite oxide is included in an amount of 0.0001 to parts by weight based on 100 parts by weight of the solvent.
The method of claim 7, wherein the nitrogen compound or the sulfur compound is included at 0.0001 to 1 molar ratio (M) with respect to the mixed solution.
1 5. The method of claim 7, wherein the subcritical condition or the supercritical condition has a temperature of 50 to 600 C.
1 6. The method of claim 7, wherein the subcritical condition or the supercritical condition has a pressure of 30 to 500 atm. Page 3 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of
The method of claim 7, wherein in the forming of the graphene, the mixed solution further including a reducing adjuvant is reacted under the subcritical condition or the supercritical condition.
1 9. The method of claim 7, further comprising, after the forming of the mixed solution and before the forming of the graphene, pre-heating the mixed solution to 50 to 500 C.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, high-pressure-filtering the graphene.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, washing the formed graphene.
An apparatus for preparing a graphene comprising: a mixing bath forming a pre-mixed solution by mixing a graphite oxide, a solvent, and a sulfur compound or a nitrogen compound; a first oxidizing agent feeding pump supplying a first oxidizing agent; a pre-heater pre-heating the pre-mixed solution and the first oxidizing agent supplied from the mixing bath and the first oxidizing g egnt feeding pump, respectively; Page 4 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of a reactor connected to a rear end of the pre-heater, and generating a reaction of a mixed solution including the pre-mixed solution and the first oxidizing agent under a subcritical condition or a supercritical condition of the solvent; a cooler connected to a rear end of the reactor and cooling a product of the reaction; and recovering baths connected to a rear end of the cooler and recovering the graphene from the product;and a reducing adjuvant feeding pump connected to the middle of the reactor and injecting a reducing adjuvant into the reactor;;; wherein the reducing adjuvant feeding pump is connected to a point of 1/6 to 1/2 from an entrance of the reactor.
The apparatus of claim 22, further comprising a circulating pump connected to the mixing bath, and circulating and mixing the graphite oxide, nitrogen compound to form the pre-mixed solution.
The apparatus of claim 22, further comprising bath and the pre-heater, and connected to the rear cooler.
The apparatus of claim 22, further comprising between the cooler and the recovering bath, and
The apparatus of claim 22, wherein the recovering product delivered from the cooler. Page 5 of 9 the solvent, and the sulfur compound or the a heat exchanger provided between the mixing end of the reactor and a front end of the a cooling and pressure-releasing bath provided cooling and pressure-releasing the product. bath further includes filters filtering the
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Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of graphite oxide from a graphite oxide precursor using acid treatment and an oxidizing agent, referenced as starting material for subsequent examples.
5 materials1 process step
Preparation of graphene via subcritical or supercritical reaction of graphite oxide with a sulfur compound or nitrogen compound and a first oxidizing agent in a solvent. Product characterized by IR, Raman, SEM, TGA, XRD, TEM, and electrical conductivity measurements.
2 materials1 process step
Preparation of graphene without the sulfur or nitrogen compound additive under subcritical or supercritical conditions, used as comparison against Example 1.
Layer stacks claimed or described, ordered top of device to substrate.
apparatus for preparing graphene
No layer stack recorded.
Materials described outside the worked examples.
solvent
graphite oxide precursor
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Oxygen Content Wt Percent | ≤ 20 wt% | graphene |
Carbon Oxygen Weight Ratio | ≥ 5 |
Related documents with shared materials, methods, properties, or citations.
METHOD FOR MANUFACTURING STACK OF GRAPHENE AND CARBON NANOTUBE, ELECTRODE MATERIAL INCLUDING STACK OF GRAPHENE AND CARBON NANOTUBE, AND ELECTRIC DOUBLE-LAYER CAPACITOR USING THE SAME
METHOD OF PRODUCING NANO-SIZE GRAPHENE-BASED MATERIAL AND AN EQUIPMENT FOR PRODUCING THE SAME
Patent
Atlas literature
Patent
US 9,738,528Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 and 2, the apparatus for preparing the graphene according to an exemplary embodiment of the present invention includes a mixing bath 100 forming a …
FIG. 2 exemplarily shows an apparatus for preparing a graphene according to an exemplary embodiment of the present invention.
FIG. 3 shows an infrared spectroscopy spectrum of graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 4 shows Raman spectrum of graphenes obtained by Example 1 25 and Comparative Example 1 of the present invention. 5
FIG. 5 shows scanning electron microscope (SEM) images of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. Referring to
FIG. 6, it could be confirmed that weight loss was shown around 200 0C in Comparative Example 1 The weight loss is caused by pyrolysis of impurities such as …
FIG. 7 shows XRD spectrum of a graphite oxide obtained by Preparation Example 1, the graphenes obtained by Example 1 and Comparative Example 1 of the present …
FIG. 8 shows transmission electron microscope (TEM) images of the 10 graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 9 shows graph showing electrical conductivity of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. 15 [Description …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
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A method for preparing a graphene comprising: forming a mixed solution including a graphite oxide, a solvent, a first oxidizing agent; and a sulfur compound or a nitrogen compound; forming the graphene by reacting the mixed solution under a subcritical condition or a supercritical condition of the solvent; and recovering the graphene -.; wherein the sulfur compound is represented by the following Chemical Formula 1, and the nitrogen compound is represented by the following Chemical Formula 2: [Chemical Formula 1 HO A 1-SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.17.655.1854.867.1909.svg 0.183 0.707 Chemistry Black and white -OH in Chemical Formula 1, Al and A₂ are each independently linear or branched C₁-C₁₀ alkylene group or C₆-C₂₀ arylene group, and Q is a sulfur atom (-S-) or a sulfone group(-(O=S=0)-), and [Chemical Formula 2. R 2 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.22.394.2333.545.2529.svg 0.653 0.503 Chemistry Black and white R 4 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.24.450.2532.510.2585.svg 0.177 0.20 Chemistry Black and white in Chemical Formula 2, at least one of R₁ to R₄ is a nitro group (- NO₂), and the remainder is hydrogen, linear or branched C₁-C₇ alkyl group or C₆-C₂₀ aryl group.
Page 2 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of 9. The method of claim 7, wherein the solvent includes water, carbon dioxide, or mixtures thereof. original
The method of claim 7, wherein the graphite oxide is formed by treating a graphite oxide precursor with an acid and a second oxidizing agent.
1 2. The method of claim 7, wherein the first oxidizing agent is at least one kind selected from the group consisiting of oxygen, ozone, and hydrogen peroxide.
The method of claim 7, wherein the graphite oxide is included in an amount of 0.0001 to parts by weight based on 100 parts by weight of the solvent.
The method of claim 7, wherein the nitrogen compound or the sulfur compound is included at 0.0001 to 1 molar ratio (M) with respect to the mixed solution.
1 5. The method of claim 7, wherein the subcritical condition or the supercritical condition has a temperature of 50 to 600 C.
1 6. The method of claim 7, wherein the subcritical condition or the supercritical condition has a pressure of 30 to 500 atm. Page 3 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of
The method of claim 7, wherein in the forming of the graphene, the mixed solution further including a reducing adjuvant is reacted under the subcritical condition or the supercritical condition.
1 9. The method of claim 7, further comprising, after the forming of the mixed solution and before the forming of the graphene, pre-heating the mixed solution to 50 to 500 C.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, high-pressure-filtering the graphene.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, washing the formed graphene.
An apparatus for preparing a graphene comprising: a mixing bath forming a pre-mixed solution by mixing a graphite oxide, a solvent, and a sulfur compound or a nitrogen compound; a first oxidizing agent feeding pump supplying a first oxidizing agent; a pre-heater pre-heating the pre-mixed solution and the first oxidizing agent supplied from the mixing bath and the first oxidizing g egnt feeding pump, respectively; Page 4 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of a reactor connected to a rear end of the pre-heater, and generating a reaction of a mixed solution including the pre-mixed solution and the first oxidizing agent under a subcritical condition or a supercritical condition of the solvent; a cooler connected to a rear end of the reactor and cooling a product of the reaction; and recovering baths connected to a rear end of the cooler and recovering the graphene from the product;and a reducing adjuvant feeding pump connected to the middle of the reactor and injecting a reducing adjuvant into the reactor;;; wherein the reducing adjuvant feeding pump is connected to a point of 1/6 to 1/2 from an entrance of the reactor.
The apparatus of claim 22, further comprising a circulating pump connected to the mixing bath, and circulating and mixing the graphite oxide, nitrogen compound to form the pre-mixed solution.
The apparatus of claim 22, further comprising bath and the pre-heater, and connected to the rear cooler.
The apparatus of claim 22, further comprising between the cooler and the recovering bath, and
The apparatus of claim 22, wherein the recovering product delivered from the cooler. Page 5 of 9 the solvent, and the sulfur compound or the a heat exchanger provided between the mixing end of the reactor and a front end of the a cooling and pressure-releasing bath provided cooling and pressure-releasing the product. bath further includes filters filtering the
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Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of graphite oxide from a graphite oxide precursor using acid treatment and an oxidizing agent, referenced as starting material for subsequent examples.
5 materials1 process step
Preparation of graphene via subcritical or supercritical reaction of graphite oxide with a sulfur compound or nitrogen compound and a first oxidizing agent in a solvent. Product characterized by IR, Raman, SEM, TGA, XRD, TEM, and electrical conductivity measurements.
2 materials1 process step
Preparation of graphene without the sulfur or nitrogen compound additive under subcritical or supercritical conditions, used as comparison against Example 1.
Layer stacks claimed or described, ordered top of device to substrate.
apparatus for preparing graphene
No layer stack recorded.
Materials described outside the worked examples.
solvent
graphite oxide precursor
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Oxygen Content Wt Percent | ≤ 20 wt% | graphene |
Carbon Oxygen Weight Ratio | ≥ 5 |
Related documents with shared materials, methods, properties, or citations.
METHOD FOR MANUFACTURING STACK OF GRAPHENE AND CARBON NANOTUBE, ELECTRODE MATERIAL INCLUDING STACK OF GRAPHENE AND CARBON NANOTUBE, AND ELECTRIC DOUBLE-LAYER CAPACITOR USING THE SAME
METHOD OF PRODUCING NANO-SIZE GRAPHENE-BASED MATERIAL AND AN EQUIPMENT FOR PRODUCING THE SAME
Patent
Atlas literature
Patent
US 9,738,528Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 and 2, the apparatus for preparing the graphene according to an exemplary embodiment of the present invention includes a mixing bath 100 forming a …
FIG. 2 exemplarily shows an apparatus for preparing a graphene according to an exemplary embodiment of the present invention.
FIG. 3 shows an infrared spectroscopy spectrum of graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 4 shows Raman spectrum of graphenes obtained by Example 1 25 and Comparative Example 1 of the present invention. 5
FIG. 5 shows scanning electron microscope (SEM) images of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. Referring to
FIG. 6, it could be confirmed that weight loss was shown around 200 0C in Comparative Example 1 The weight loss is caused by pyrolysis of impurities such as …
FIG. 7 shows XRD spectrum of a graphite oxide obtained by Preparation Example 1, the graphenes obtained by Example 1 and Comparative Example 1 of the present …
FIG. 8 shows transmission electron microscope (TEM) images of the 10 graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 9 shows graph showing electrical conductivity of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. 15 [Description …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
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A method for preparing a graphene comprising: forming a mixed solution including a graphite oxide, a solvent, a first oxidizing agent; and a sulfur compound or a nitrogen compound; forming the graphene by reacting the mixed solution under a subcritical condition or a supercritical condition of the solvent; and recovering the graphene -.; wherein the sulfur compound is represented by the following Chemical Formula 1, and the nitrogen compound is represented by the following Chemical Formula 2: [Chemical Formula 1 HO A 1-SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.17.655.1854.867.1909.svg 0.183 0.707 Chemistry Black and white -OH in Chemical Formula 1, Al and A₂ are each independently linear or branched C₁-C₁₀ alkylene group or C₆-C₂₀ arylene group, and Q is a sulfur atom (-S-) or a sulfone group(-(O=S=0)-), and [Chemical Formula 2. R 2 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.22.394.2333.545.2529.svg 0.653 0.503 Chemistry Black and white R 4 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.24.450.2532.510.2585.svg 0.177 0.20 Chemistry Black and white in Chemical Formula 2, at least one of R₁ to R₄ is a nitro group (- NO₂), and the remainder is hydrogen, linear or branched C₁-C₇ alkyl group or C₆-C₂₀ aryl group.
Page 2 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of 9. The method of claim 7, wherein the solvent includes water, carbon dioxide, or mixtures thereof. original
The method of claim 7, wherein the graphite oxide is formed by treating a graphite oxide precursor with an acid and a second oxidizing agent.
1 2. The method of claim 7, wherein the first oxidizing agent is at least one kind selected from the group consisiting of oxygen, ozone, and hydrogen peroxide.
The method of claim 7, wherein the graphite oxide is included in an amount of 0.0001 to parts by weight based on 100 parts by weight of the solvent.
The method of claim 7, wherein the nitrogen compound or the sulfur compound is included at 0.0001 to 1 molar ratio (M) with respect to the mixed solution.
1 5. The method of claim 7, wherein the subcritical condition or the supercritical condition has a temperature of 50 to 600 C.
1 6. The method of claim 7, wherein the subcritical condition or the supercritical condition has a pressure of 30 to 500 atm. Page 3 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of
The method of claim 7, wherein in the forming of the graphene, the mixed solution further including a reducing adjuvant is reacted under the subcritical condition or the supercritical condition.
1 9. The method of claim 7, further comprising, after the forming of the mixed solution and before the forming of the graphene, pre-heating the mixed solution to 50 to 500 C.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, high-pressure-filtering the graphene.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, washing the formed graphene.
An apparatus for preparing a graphene comprising: a mixing bath forming a pre-mixed solution by mixing a graphite oxide, a solvent, and a sulfur compound or a nitrogen compound; a first oxidizing agent feeding pump supplying a first oxidizing agent; a pre-heater pre-heating the pre-mixed solution and the first oxidizing agent supplied from the mixing bath and the first oxidizing g egnt feeding pump, respectively; Page 4 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of a reactor connected to a rear end of the pre-heater, and generating a reaction of a mixed solution including the pre-mixed solution and the first oxidizing agent under a subcritical condition or a supercritical condition of the solvent; a cooler connected to a rear end of the reactor and cooling a product of the reaction; and recovering baths connected to a rear end of the cooler and recovering the graphene from the product;and a reducing adjuvant feeding pump connected to the middle of the reactor and injecting a reducing adjuvant into the reactor;;; wherein the reducing adjuvant feeding pump is connected to a point of 1/6 to 1/2 from an entrance of the reactor.
The apparatus of claim 22, further comprising a circulating pump connected to the mixing bath, and circulating and mixing the graphite oxide, nitrogen compound to form the pre-mixed solution.
The apparatus of claim 22, further comprising bath and the pre-heater, and connected to the rear cooler.
The apparatus of claim 22, further comprising between the cooler and the recovering bath, and
The apparatus of claim 22, wherein the recovering product delivered from the cooler. Page 5 of 9 the solvent, and the sulfur compound or the a heat exchanger provided between the mixing end of the reactor and a front end of the a cooling and pressure-releasing bath provided cooling and pressure-releasing the product. bath further includes filters filtering the
canceled
canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of graphite oxide from a graphite oxide precursor using acid treatment and an oxidizing agent, referenced as starting material for subsequent examples.
5 materials1 process step
Preparation of graphene via subcritical or supercritical reaction of graphite oxide with a sulfur compound or nitrogen compound and a first oxidizing agent in a solvent. Product characterized by IR, Raman, SEM, TGA, XRD, TEM, and electrical conductivity measurements.
2 materials1 process step
Preparation of graphene without the sulfur or nitrogen compound additive under subcritical or supercritical conditions, used as comparison against Example 1.
Layer stacks claimed or described, ordered top of device to substrate.
apparatus for preparing graphene
No layer stack recorded.
Materials described outside the worked examples.
solvent
graphite oxide precursor
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Oxygen Content Wt Percent | ≤ 20 wt% | graphene |
Carbon Oxygen Weight Ratio | ≥ 5 |
Related documents with shared materials, methods, properties, or citations.
METHOD FOR MANUFACTURING STACK OF GRAPHENE AND CARBON NANOTUBE, ELECTRODE MATERIAL INCLUDING STACK OF GRAPHENE AND CARBON NANOTUBE, AND ELECTRIC DOUBLE-LAYER CAPACITOR USING THE SAME
METHOD OF PRODUCING NANO-SIZE GRAPHENE-BASED MATERIAL AND AN EQUIPMENT FOR PRODUCING THE SAME
Patent
Atlas literature
Patent
US 9,738,528Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 and 2, the apparatus for preparing the graphene according to an exemplary embodiment of the present invention includes a mixing bath 100 forming a …
FIG. 2 exemplarily shows an apparatus for preparing a graphene according to an exemplary embodiment of the present invention.
FIG. 3 shows an infrared spectroscopy spectrum of graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 4 shows Raman spectrum of graphenes obtained by Example 1 25 and Comparative Example 1 of the present invention. 5
FIG. 5 shows scanning electron microscope (SEM) images of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. Referring to
FIG. 6, it could be confirmed that weight loss was shown around 200 0C in Comparative Example 1 The weight loss is caused by pyrolysis of impurities such as …
FIG. 7 shows XRD spectrum of a graphite oxide obtained by Preparation Example 1, the graphenes obtained by Example 1 and Comparative Example 1 of the present …
FIG. 8 shows transmission electron microscope (TEM) images of the 10 graphenes obtained by Example 1 and Comparative Example 1 of the present invention.
FIG. 9 shows graph showing electrical conductivity of the graphenes obtained by Example 1 and Comparative Example 1 of the present invention. 15 [Description …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
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A method for preparing a graphene comprising: forming a mixed solution including a graphite oxide, a solvent, a first oxidizing agent; and a sulfur compound or a nitrogen compound; forming the graphene by reacting the mixed solution under a subcritical condition or a supercritical condition of the solvent; and recovering the graphene -.; wherein the sulfur compound is represented by the following Chemical Formula 1, and the nitrogen compound is represented by the following Chemical Formula 2: [Chemical Formula 1 HO A 1-SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.17.655.1854.867.1909.svg 0.183 0.707 Chemistry Black and white -OH in Chemical Formula 1, Al and A₂ are each independently linear or branched C₁-C₁₀ alkylene group or C₆-C₂₀ arylene group, and Q is a sulfur atom (-S-) or a sulfone group(-(O=S=0)-), and [Chemical Formula 2. R 2 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.22.394.2333.545.2529.svg 0.653 0.503 Chemistry Black and white R 4 SVG 14907858.05-23-2017.J₃₄BHYG₁PXXIFW2.CLM.1.24.450.2532.510.2585.svg 0.177 0.20 Chemistry Black and white in Chemical Formula 2, at least one of R₁ to R₄ is a nitro group (- NO₂), and the remainder is hydrogen, linear or branched C₁-C₇ alkyl group or C₆-C₂₀ aryl group.
Page 2 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of 9. The method of claim 7, wherein the solvent includes water, carbon dioxide, or mixtures thereof. original
The method of claim 7, wherein the graphite oxide is formed by treating a graphite oxide precursor with an acid and a second oxidizing agent.
1 2. The method of claim 7, wherein the first oxidizing agent is at least one kind selected from the group consisiting of oxygen, ozone, and hydrogen peroxide.
The method of claim 7, wherein the graphite oxide is included in an amount of 0.0001 to parts by weight based on 100 parts by weight of the solvent.
The method of claim 7, wherein the nitrogen compound or the sulfur compound is included at 0.0001 to 1 molar ratio (M) with respect to the mixed solution.
1 5. The method of claim 7, wherein the subcritical condition or the supercritical condition has a temperature of 50 to 600 C.
1 6. The method of claim 7, wherein the subcritical condition or the supercritical condition has a pressure of 30 to 500 atm. Page 3 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of
The method of claim 7, wherein in the forming of the graphene, the mixed solution further including a reducing adjuvant is reacted under the subcritical condition or the supercritical condition.
1 9. The method of claim 7, further comprising, after the forming of the mixed solution and before the forming of the graphene, pre-heating the mixed solution to 50 to 500 C.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, high-pressure-filtering the graphene.
The method of claim 7, further comprising, after the forming of the graphene and before the recovering of the graphene, washing the formed graphene.
An apparatus for preparing a graphene comprising: a mixing bath forming a pre-mixed solution by mixing a graphite oxide, a solvent, and a sulfur compound or a nitrogen compound; a first oxidizing agent feeding pump supplying a first oxidizing agent; a pre-heater pre-heating the pre-mixed solution and the first oxidizing agent supplied from the mixing bath and the first oxidizing g egnt feeding pump, respectively; Page 4 of 9 Application Number 14/907,858 Attorney Docket LPP₂₀₁₆₀₁₀₆US Amendment Filed Reply to Office Action of a reactor connected to a rear end of the pre-heater, and generating a reaction of a mixed solution including the pre-mixed solution and the first oxidizing agent under a subcritical condition or a supercritical condition of the solvent; a cooler connected to a rear end of the reactor and cooling a product of the reaction; and recovering baths connected to a rear end of the cooler and recovering the graphene from the product;and a reducing adjuvant feeding pump connected to the middle of the reactor and injecting a reducing adjuvant into the reactor;;; wherein the reducing adjuvant feeding pump is connected to a point of 1/6 to 1/2 from an entrance of the reactor.
The apparatus of claim 22, further comprising a circulating pump connected to the mixing bath, and circulating and mixing the graphite oxide, nitrogen compound to form the pre-mixed solution.
The apparatus of claim 22, further comprising bath and the pre-heater, and connected to the rear cooler.
The apparatus of claim 22, further comprising between the cooler and the recovering bath, and
The apparatus of claim 22, wherein the recovering product delivered from the cooler. Page 5 of 9 the solvent, and the sulfur compound or the a heat exchanger provided between the mixing end of the reactor and a front end of the a cooling and pressure-releasing bath provided cooling and pressure-releasing the product. bath further includes filters filtering the
canceled
canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material1 process step
Preparation of graphite oxide from a graphite oxide precursor using acid treatment and an oxidizing agent, referenced as starting material for subsequent examples.
5 materials1 process step
Preparation of graphene via subcritical or supercritical reaction of graphite oxide with a sulfur compound or nitrogen compound and a first oxidizing agent in a solvent. Product characterized by IR, Raman, SEM, TGA, XRD, TEM, and electrical conductivity measurements.
2 materials1 process step
Preparation of graphene without the sulfur or nitrogen compound additive under subcritical or supercritical conditions, used as comparison against Example 1.
Layer stacks claimed or described, ordered top of device to substrate.
apparatus for preparing graphene
No layer stack recorded.
Materials described outside the worked examples.
solvent
graphite oxide precursor
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Oxygen Content Wt Percent | ≤ 20 wt% | graphene |
Carbon Oxygen Weight Ratio | ≥ 5 |
Related documents with shared materials, methods, properties, or citations.
METHOD FOR MANUFACTURING STACK OF GRAPHENE AND CARBON NANOTUBE, ELECTRODE MATERIAL INCLUDING STACK OF GRAPHENE AND CARBON NANOTUBE, AND ELECTRIC DOUBLE-LAYER CAPACITOR USING THE SAME
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reducing adjuvant
Thickness | 2600–2800 cm | — |
Pressure | 0.0001–30 pa | — |
Pressure | 30–500 atm | — |
reducing adjuvant
Thickness | 2600–2800 cm | — |
Pressure | 0.0001–30 pa | — |
Pressure | 30–500 atm | — |
reducing adjuvant
Thickness | 2600–2800 cm | — |
Pressure | 0.0001–30 pa | — |
Pressure | 30–500 atm | — |
reducing adjuvant
Thickness | 2600–2800 cm | — |
Pressure | 0.0001–30 pa | — |
Pressure | 30–500 atm | — |