Patent
US 10,392,256METHOD FOR PREPARING GRAPHENE BY USING MOLTEN INORGANIC SALT REACTION BED
Xuyang SUN
US
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Atlas literature
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US 10,392,256Patent drawings and their descriptions. Click a drawing to enlarge it.
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 by using a molten inorganic salt reaction bed, comprising the following steps: using phthalocyanine substance as a reaction raw material, well-mixing an inorganic salt with the phthalocyanine substance in an inorganic salt reaction bed, performing pyrolysis by using a temperature programmed method in an atmosphere furnace under a protective gas, and separating out a highly planar-oriented graphene material.
The method of claim 1 wherein the mass ratio of the phthalocyanine raw material to the inorganic salt is 1:99 to 10:90.
The method of claim 1 wherein the method for well-mixing the inorganic salt with the reaction raw material comprises: well-mixing the phthalocyanine substance with the inorganic salt before temperature rising, or uniformly adding the phthalocyanine substance into the inorganic salt reaction bed after the inorganic salt melted.
The method of claim 1 wherein the protective gas is selected from nitrogen gas, argon gas, argon/hydrogen gas mixture, argon/ammonia gas mixture, nitrogen/hydrogen gas mixture or SVG 15525070.05-07-2017.J₂FI₃GUWRXEAPX0.CLM.2.2.379.518.493.561.svg 0.143 0.38 Chemistry Black and white nitrogen/ammonia gas mixture, and the flow rate of the protective gas is controlled within 1 0-50 cm3.
The method of claim t wherein pyrolysis reaction can be performed in the absence of a catalyst or in the presence of a metal catalyst, and the metal catalyst is selected from a copper foil, a copper mesh, a nickel foil, foam nickel, a copper wherein high-quality graphene seed crystals are substance. 16 alloy or a nickel alloy. 10. The method of claim 1 added to the inorganic salt or the phthalocyanine
The method of claim I wherein the phthalocyanine substance comprises nonmetal phthalocyanines, metal phthalocyanines, metallic oxide phthalocyanines, macromolecules containing p hi thalocyanine ring structures and porphyrin polymers containing phthalocyanine ring structures.
The method of claim I wherein the inorganic salt reaction bed is obtained by filling inorganic salt in a hig h temperature resistant container; and the inorganic salt is one or more substances selected from sodium salt, potassium salt, sulfate, hydrochloride or nitrate.
The method of claim t wherein pyrolysis temperature is 800- 1 000 0 C, and pyrolysis time is 4-24h.
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with sodium chloride at a mass ratio of CuPc:NaCl = 1:99. Pyrolysis was performed in a quartz tube furnace under high-purity argon at 50 cm3/min using a stepwise temperature program: 300°C/1h, 350°C/1h, 400°C/1h, 500°C/4h, then 800°C/8h, followed by natural cooling and water washing to remove salt. 20.7 g of a highly oriented metal graphene material was obtained. XRD and TEM spectra were recorded.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with potassium chloride and pyrolysis was performed (details truncated in source text).
Materials described outside the worked examples.
phthalocyanine substance
inorganic salt
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1000 °C | — |
Thickness |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,392,256Patent drawings and their descriptions. Click a drawing to enlarge it.
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 by using a molten inorganic salt reaction bed, comprising the following steps: using phthalocyanine substance as a reaction raw material, well-mixing an inorganic salt with the phthalocyanine substance in an inorganic salt reaction bed, performing pyrolysis by using a temperature programmed method in an atmosphere furnace under a protective gas, and separating out a highly planar-oriented graphene material.
The method of claim 1 wherein the mass ratio of the phthalocyanine raw material to the inorganic salt is 1:99 to 10:90.
The method of claim 1 wherein the method for well-mixing the inorganic salt with the reaction raw material comprises: well-mixing the phthalocyanine substance with the inorganic salt before temperature rising, or uniformly adding the phthalocyanine substance into the inorganic salt reaction bed after the inorganic salt melted.
The method of claim 1 wherein the protective gas is selected from nitrogen gas, argon gas, argon/hydrogen gas mixture, argon/ammonia gas mixture, nitrogen/hydrogen gas mixture or SVG 15525070.05-07-2017.J₂FI₃GUWRXEAPX0.CLM.2.2.379.518.493.561.svg 0.143 0.38 Chemistry Black and white nitrogen/ammonia gas mixture, and the flow rate of the protective gas is controlled within 1 0-50 cm3.
The method of claim t wherein pyrolysis reaction can be performed in the absence of a catalyst or in the presence of a metal catalyst, and the metal catalyst is selected from a copper foil, a copper mesh, a nickel foil, foam nickel, a copper wherein high-quality graphene seed crystals are substance. 16 alloy or a nickel alloy. 10. The method of claim 1 added to the inorganic salt or the phthalocyanine
The method of claim I wherein the phthalocyanine substance comprises nonmetal phthalocyanines, metal phthalocyanines, metallic oxide phthalocyanines, macromolecules containing p hi thalocyanine ring structures and porphyrin polymers containing phthalocyanine ring structures.
The method of claim I wherein the inorganic salt reaction bed is obtained by filling inorganic salt in a hig h temperature resistant container; and the inorganic salt is one or more substances selected from sodium salt, potassium salt, sulfate, hydrochloride or nitrate.
The method of claim t wherein pyrolysis temperature is 800- 1 000 0 C, and pyrolysis time is 4-24h.
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with sodium chloride at a mass ratio of CuPc:NaCl = 1:99. Pyrolysis was performed in a quartz tube furnace under high-purity argon at 50 cm3/min using a stepwise temperature program: 300°C/1h, 350°C/1h, 400°C/1h, 500°C/4h, then 800°C/8h, followed by natural cooling and water washing to remove salt. 20.7 g of a highly oriented metal graphene material was obtained. XRD and TEM spectra were recorded.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with potassium chloride and pyrolysis was performed (details truncated in source text).
Materials described outside the worked examples.
phthalocyanine substance
inorganic salt
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1000 °C | — |
Thickness |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,392,256Patent drawings and their descriptions. Click a drawing to enlarge it.
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 by using a molten inorganic salt reaction bed, comprising the following steps: using phthalocyanine substance as a reaction raw material, well-mixing an inorganic salt with the phthalocyanine substance in an inorganic salt reaction bed, performing pyrolysis by using a temperature programmed method in an atmosphere furnace under a protective gas, and separating out a highly planar-oriented graphene material.
The method of claim 1 wherein the mass ratio of the phthalocyanine raw material to the inorganic salt is 1:99 to 10:90.
The method of claim 1 wherein the method for well-mixing the inorganic salt with the reaction raw material comprises: well-mixing the phthalocyanine substance with the inorganic salt before temperature rising, or uniformly adding the phthalocyanine substance into the inorganic salt reaction bed after the inorganic salt melted.
The method of claim 1 wherein the protective gas is selected from nitrogen gas, argon gas, argon/hydrogen gas mixture, argon/ammonia gas mixture, nitrogen/hydrogen gas mixture or SVG 15525070.05-07-2017.J₂FI₃GUWRXEAPX0.CLM.2.2.379.518.493.561.svg 0.143 0.38 Chemistry Black and white nitrogen/ammonia gas mixture, and the flow rate of the protective gas is controlled within 1 0-50 cm3.
The method of claim t wherein pyrolysis reaction can be performed in the absence of a catalyst or in the presence of a metal catalyst, and the metal catalyst is selected from a copper foil, a copper mesh, a nickel foil, foam nickel, a copper wherein high-quality graphene seed crystals are substance. 16 alloy or a nickel alloy. 10. The method of claim 1 added to the inorganic salt or the phthalocyanine
The method of claim I wherein the phthalocyanine substance comprises nonmetal phthalocyanines, metal phthalocyanines, metallic oxide phthalocyanines, macromolecules containing p hi thalocyanine ring structures and porphyrin polymers containing phthalocyanine ring structures.
The method of claim I wherein the inorganic salt reaction bed is obtained by filling inorganic salt in a hig h temperature resistant container; and the inorganic salt is one or more substances selected from sodium salt, potassium salt, sulfate, hydrochloride or nitrate.
The method of claim t wherein pyrolysis temperature is 800- 1 000 0 C, and pyrolysis time is 4-24h.
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with sodium chloride at a mass ratio of CuPc:NaCl = 1:99. Pyrolysis was performed in a quartz tube furnace under high-purity argon at 50 cm3/min using a stepwise temperature program: 300°C/1h, 350°C/1h, 400°C/1h, 500°C/4h, then 800°C/8h, followed by natural cooling and water washing to remove salt. 20.7 g of a highly oriented metal graphene material was obtained. XRD and TEM spectra were recorded.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with potassium chloride and pyrolysis was performed (details truncated in source text).
Materials described outside the worked examples.
phthalocyanine substance
inorganic salt
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1000 °C | — |
Thickness |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,392,256Patent drawings and their descriptions. Click a drawing to enlarge it.
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 by using a molten inorganic salt reaction bed, comprising the following steps: using phthalocyanine substance as a reaction raw material, well-mixing an inorganic salt with the phthalocyanine substance in an inorganic salt reaction bed, performing pyrolysis by using a temperature programmed method in an atmosphere furnace under a protective gas, and separating out a highly planar-oriented graphene material.
The method of claim 1 wherein the mass ratio of the phthalocyanine raw material to the inorganic salt is 1:99 to 10:90.
The method of claim 1 wherein the method for well-mixing the inorganic salt with the reaction raw material comprises: well-mixing the phthalocyanine substance with the inorganic salt before temperature rising, or uniformly adding the phthalocyanine substance into the inorganic salt reaction bed after the inorganic salt melted.
The method of claim 1 wherein the protective gas is selected from nitrogen gas, argon gas, argon/hydrogen gas mixture, argon/ammonia gas mixture, nitrogen/hydrogen gas mixture or SVG 15525070.05-07-2017.J₂FI₃GUWRXEAPX0.CLM.2.2.379.518.493.561.svg 0.143 0.38 Chemistry Black and white nitrogen/ammonia gas mixture, and the flow rate of the protective gas is controlled within 1 0-50 cm3.
The method of claim t wherein pyrolysis reaction can be performed in the absence of a catalyst or in the presence of a metal catalyst, and the metal catalyst is selected from a copper foil, a copper mesh, a nickel foil, foam nickel, a copper wherein high-quality graphene seed crystals are substance. 16 alloy or a nickel alloy. 10. The method of claim 1 added to the inorganic salt or the phthalocyanine
The method of claim I wherein the phthalocyanine substance comprises nonmetal phthalocyanines, metal phthalocyanines, metallic oxide phthalocyanines, macromolecules containing p hi thalocyanine ring structures and porphyrin polymers containing phthalocyanine ring structures.
The method of claim I wherein the inorganic salt reaction bed is obtained by filling inorganic salt in a hig h temperature resistant container; and the inorganic salt is one or more substances selected from sodium salt, potassium salt, sulfate, hydrochloride or nitrate.
The method of claim t wherein pyrolysis temperature is 800- 1 000 0 C, and pyrolysis time is 4-24h.
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with sodium chloride at a mass ratio of CuPc:NaCl = 1:99. Pyrolysis was performed in a quartz tube furnace under high-purity argon at 50 cm3/min using a stepwise temperature program: 300°C/1h, 350°C/1h, 400°C/1h, 500°C/4h, then 800°C/8h, followed by natural cooling and water washing to remove salt. 20.7 g of a highly oriented metal graphene material was obtained. XRD and TEM spectra were recorded.
3 materials1 process step
30.0 g of commercially available copper phthalocyanine (CuPc) was mixed with potassium chloride and pyrolysis was performed (details truncated in source text).
Materials described outside the worked examples.
phthalocyanine substance
inorganic salt
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1000 °C | — |
Thickness |
Related documents with shared materials, methods, properties, or citations.
graphene seed crystals
highly oriented metal graphene material
| 0–50 cm |
| — |
graphene seed crystals
highly oriented metal graphene material
| 0–50 cm |
| — |
graphene seed crystals
highly oriented metal graphene material
| 0–50 cm |
| — |
graphene seed crystals
highly oriented metal graphene material
| 0–50 cm |
| — |