Patent
US 10,336,619AN IMPROVED METHOD FOR THE SYNTHESIS OF GRAPHENE OXIDE
VIRAJ C. JAYAWARDENA
US
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Patent
Atlas literature
Patent
US 10,336,619Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an X-ray Diffraction pattern obtained for a graphene oxide powder according to an example embodiment of the present invention [0014]
FIG. 2 is a Thermogravimetric Analysis spectrum obtained for a graphene oxide according to an example embodiment of the present invention 25 [0015]
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
FIG. 4 are Raman spectra for graphene oxide [0017]
FIG. 5 is a Nuclear Magnetic Resonance (NMR) spectra for graphene oxide [0018]
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
FIG. 8 is an UV/VIS spectrum for highly-oxidized graphene oxide
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Twice Amended) A method of synthesizing graphene oxide with an X-ra y diffraction spectrum having a single dominant peak at a two theta angle below 10 degrees without the use of H 3 P O 4 or a nitrogen-containing compound comprising: a. providing a graphite source; b. reacting the graphite source with H 2 S O 4 in a vessel; c. adding KMn O 4 to the vessel to form a reaction mixture, wherein the H 2 S O 4, graphite source, and KMn O 4 are maintained at a temperature between 0 0 C and 10 0 C from the addition of the H 2 S O 4 through reaction with KMn O 4 for a period of more than 8 hours; d. adding H 2 0 2 and H 2 O to the reaction mixture in order to create a supernatant and a graphene oxide slurry; and e. separating the supernatant in order to obtain the graphene oxide slurry. Currently amended
The method of claim 1 further comprising washing the graphene oxide slurry with one or more washing agents. Original
Canceled
The method of claim 9 wherein the ratio of is between about 1: 2 and about 1:5. Original
Canceled
Canceled
Canceled oxide slurry is dried at room temperature under oxide slurry is exfoliated. Original comprises addition of the graphene oxide slurry to mixture to create a sonicated mixture. Original further comprises transfer of the sonicated mixture graphite source (in grams) to KMn O 4 (in grams) source comprises at least 99 % graphite.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Approximately 1.5 g of natural high purity (>99%) vein graphite from Bogala Graphite (Sri Lanka) was added to 100 ml of H₂SO₄ (95-97%, Sigma-Aldrich) at 0°C. The mixture was maintained at 0-10°C while stirring. About 5.4 g of KMnO₄ (99%, Lions Lab Chemicals, India) was added. After adding KMnO₄ the mixture was stirred for 12 hours at 0-10°C; colour turned dark brown. The reaction was quenched with ~200 g ice, 200 ml H₂O, and 1.5 ml H₂O2. The supernatant was discarded leaving graphene oxide slurry, which was washed with 400 ml deionized water, then 1:2 aqueous HCl solution, then 400 ml ethanol and 400 ml diethyl ether. The brown solid was dried at room temperature under vacuum.
Materials described outside the worked examples.
hydrogen peroxide
H₂O₂
hydrochloric acid
HCl
ethanol
C₂H₅OH
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
single dominant XRD peak below 10 degrees two-theta (claimed) | ≤ 10 deg | graphene oxide |
Temperature | 35–1000 °C |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,336,619Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an X-ray Diffraction pattern obtained for a graphene oxide powder according to an example embodiment of the present invention [0014]
FIG. 2 is a Thermogravimetric Analysis spectrum obtained for a graphene oxide according to an example embodiment of the present invention 25 [0015]
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
FIG. 4 are Raman spectra for graphene oxide [0017]
FIG. 5 is a Nuclear Magnetic Resonance (NMR) spectra for graphene oxide [0018]
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
FIG. 8 is an UV/VIS spectrum for highly-oxidized graphene oxide
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Twice Amended) A method of synthesizing graphene oxide with an X-ra y diffraction spectrum having a single dominant peak at a two theta angle below 10 degrees without the use of H 3 P O 4 or a nitrogen-containing compound comprising: a. providing a graphite source; b. reacting the graphite source with H 2 S O 4 in a vessel; c. adding KMn O 4 to the vessel to form a reaction mixture, wherein the H 2 S O 4, graphite source, and KMn O 4 are maintained at a temperature between 0 0 C and 10 0 C from the addition of the H 2 S O 4 through reaction with KMn O 4 for a period of more than 8 hours; d. adding H 2 0 2 and H 2 O to the reaction mixture in order to create a supernatant and a graphene oxide slurry; and e. separating the supernatant in order to obtain the graphene oxide slurry. Currently amended
The method of claim 1 further comprising washing the graphene oxide slurry with one or more washing agents. Original
Canceled
The method of claim 9 wherein the ratio of is between about 1: 2 and about 1:5. Original
Canceled
Canceled
Canceled oxide slurry is dried at room temperature under oxide slurry is exfoliated. Original comprises addition of the graphene oxide slurry to mixture to create a sonicated mixture. Original further comprises transfer of the sonicated mixture graphite source (in grams) to KMn O 4 (in grams) source comprises at least 99 % graphite.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Approximately 1.5 g of natural high purity (>99%) vein graphite from Bogala Graphite (Sri Lanka) was added to 100 ml of H₂SO₄ (95-97%, Sigma-Aldrich) at 0°C. The mixture was maintained at 0-10°C while stirring. About 5.4 g of KMnO₄ (99%, Lions Lab Chemicals, India) was added. After adding KMnO₄ the mixture was stirred for 12 hours at 0-10°C; colour turned dark brown. The reaction was quenched with ~200 g ice, 200 ml H₂O, and 1.5 ml H₂O2. The supernatant was discarded leaving graphene oxide slurry, which was washed with 400 ml deionized water, then 1:2 aqueous HCl solution, then 400 ml ethanol and 400 ml diethyl ether. The brown solid was dried at room temperature under vacuum.
Materials described outside the worked examples.
hydrogen peroxide
H₂O₂
hydrochloric acid
HCl
ethanol
C₂H₅OH
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
single dominant XRD peak below 10 degrees two-theta (claimed) | ≤ 10 deg | graphene oxide |
Temperature | 35–1000 °C |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,336,619Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an X-ray Diffraction pattern obtained for a graphene oxide powder according to an example embodiment of the present invention [0014]
FIG. 2 is a Thermogravimetric Analysis spectrum obtained for a graphene oxide according to an example embodiment of the present invention 25 [0015]
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
FIG. 4 are Raman spectra for graphene oxide [0017]
FIG. 5 is a Nuclear Magnetic Resonance (NMR) spectra for graphene oxide [0018]
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
FIG. 8 is an UV/VIS spectrum for highly-oxidized graphene oxide
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Twice Amended) A method of synthesizing graphene oxide with an X-ra y diffraction spectrum having a single dominant peak at a two theta angle below 10 degrees without the use of H 3 P O 4 or a nitrogen-containing compound comprising: a. providing a graphite source; b. reacting the graphite source with H 2 S O 4 in a vessel; c. adding KMn O 4 to the vessel to form a reaction mixture, wherein the H 2 S O 4, graphite source, and KMn O 4 are maintained at a temperature between 0 0 C and 10 0 C from the addition of the H 2 S O 4 through reaction with KMn O 4 for a period of more than 8 hours; d. adding H 2 0 2 and H 2 O to the reaction mixture in order to create a supernatant and a graphene oxide slurry; and e. separating the supernatant in order to obtain the graphene oxide slurry. Currently amended
The method of claim 1 further comprising washing the graphene oxide slurry with one or more washing agents. Original
Canceled
The method of claim 9 wherein the ratio of is between about 1: 2 and about 1:5. Original
Canceled
Canceled
Canceled oxide slurry is dried at room temperature under oxide slurry is exfoliated. Original comprises addition of the graphene oxide slurry to mixture to create a sonicated mixture. Original further comprises transfer of the sonicated mixture graphite source (in grams) to KMn O 4 (in grams) source comprises at least 99 % graphite.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Approximately 1.5 g of natural high purity (>99%) vein graphite from Bogala Graphite (Sri Lanka) was added to 100 ml of H₂SO₄ (95-97%, Sigma-Aldrich) at 0°C. The mixture was maintained at 0-10°C while stirring. About 5.4 g of KMnO₄ (99%, Lions Lab Chemicals, India) was added. After adding KMnO₄ the mixture was stirred for 12 hours at 0-10°C; colour turned dark brown. The reaction was quenched with ~200 g ice, 200 ml H₂O, and 1.5 ml H₂O2. The supernatant was discarded leaving graphene oxide slurry, which was washed with 400 ml deionized water, then 1:2 aqueous HCl solution, then 400 ml ethanol and 400 ml diethyl ether. The brown solid was dried at room temperature under vacuum.
Materials described outside the worked examples.
hydrogen peroxide
H₂O₂
hydrochloric acid
HCl
ethanol
C₂H₅OH
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
single dominant XRD peak below 10 degrees two-theta (claimed) | ≤ 10 deg | graphene oxide |
Temperature | 35–1000 °C |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,336,619Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is an X-ray Diffraction pattern obtained for a graphene oxide powder according to an example embodiment of the present invention [0014]
FIG. 2 is a Thermogravimetric Analysis spectrum obtained for a graphene oxide according to an example embodiment of the present invention 25 [0015]
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
FIG. 4 are Raman spectra for graphene oxide [0017]
FIG. 5 is a Nuclear Magnetic Resonance (NMR) spectra for graphene oxide [0018]
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
FIG. 8 is an UV/VIS spectrum for highly-oxidized graphene oxide
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
(Twice Amended) A method of synthesizing graphene oxide with an X-ra y diffraction spectrum having a single dominant peak at a two theta angle below 10 degrees without the use of H 3 P O 4 or a nitrogen-containing compound comprising: a. providing a graphite source; b. reacting the graphite source with H 2 S O 4 in a vessel; c. adding KMn O 4 to the vessel to form a reaction mixture, wherein the H 2 S O 4, graphite source, and KMn O 4 are maintained at a temperature between 0 0 C and 10 0 C from the addition of the H 2 S O 4 through reaction with KMn O 4 for a period of more than 8 hours; d. adding H 2 0 2 and H 2 O to the reaction mixture in order to create a supernatant and a graphene oxide slurry; and e. separating the supernatant in order to obtain the graphene oxide slurry. Currently amended
The method of claim 1 further comprising washing the graphene oxide slurry with one or more washing agents. Original
Canceled
The method of claim 9 wherein the ratio of is between about 1: 2 and about 1:5. Original
Canceled
Canceled
Canceled oxide slurry is dried at room temperature under oxide slurry is exfoliated. Original comprises addition of the graphene oxide slurry to mixture to create a sonicated mixture. Original further comprises transfer of the sonicated mixture graphite source (in grams) to KMn O 4 (in grams) source comprises at least 99 % graphite.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Approximately 1.5 g of natural high purity (>99%) vein graphite from Bogala Graphite (Sri Lanka) was added to 100 ml of H₂SO₄ (95-97%, Sigma-Aldrich) at 0°C. The mixture was maintained at 0-10°C while stirring. About 5.4 g of KMnO₄ (99%, Lions Lab Chemicals, India) was added. After adding KMnO₄ the mixture was stirred for 12 hours at 0-10°C; colour turned dark brown. The reaction was quenched with ~200 g ice, 200 ml H₂O, and 1.5 ml H₂O2. The supernatant was discarded leaving graphene oxide slurry, which was washed with 400 ml deionized water, then 1:2 aqueous HCl solution, then 400 ml ethanol and 400 ml diethyl ether. The brown solid was dried at room temperature under vacuum.
Materials described outside the worked examples.
hydrogen peroxide
H₂O₂
hydrochloric acid
HCl
ethanol
C₂H₅OH
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 3 is a Fourier Transform IR spectrum for a graphene oxide powder according to an example embodiment of the present invention [0016]
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
single dominant XRD peak below 10 degrees two-theta (claimed) | ≤ 10 deg | graphene oxide |
Temperature | 35–1000 °C |
Related documents with shared materials, methods, properties, or citations.
diethyl ether
(C₂H₅)2O
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
| — |
Temperature | 130–220 °C | — |
Thickness | 1–3500 cm | — |
Temperature | 0–10 °C | — |
Thickness | 3000–4000 cm | — |
Thickness | 1590–1620 cm | — |
Duration | ≥ 8 hours | — |
diethyl ether
(C₂H₅)2O
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
| — |
Temperature | 130–220 °C | — |
Thickness | 1–3500 cm | — |
Temperature | 0–10 °C | — |
Thickness | 3000–4000 cm | — |
Thickness | 1590–1620 cm | — |
Duration | ≥ 8 hours | — |
diethyl ether
(C₂H₅)2O
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
| — |
Temperature | 130–220 °C | — |
Thickness | 1–3500 cm | — |
Temperature | 0–10 °C | — |
Thickness | 3000–4000 cm | — |
Thickness | 1590–1620 cm | — |
Duration | ≥ 8 hours | — |
diethyl ether
(C₂H₅)2O
FIG. 6 is an Atomic Force Microscopy image of a graphene oxide flake on a mica 30 substrate 4 [0019]
FIG. 7 shows TEM images for graphene oxide obtained on a lacey- carbon TEM grid and SAED pattern [0020]
| — |
Temperature | 130–220 °C | — |
Thickness | 1–3500 cm | — |
Temperature | 0–10 °C | — |
Thickness | 3000–4000 cm | — |
Thickness | 1590–1620 cm | — |
Duration | ≥ 8 hours | — |