Patent
US 10,822,239Patent
Atlas literature
Patent
US 10,822,239Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing graphite intercalation compound (GIC) or graphite oxide. 15
FIG.2(B) Schematic of a ribbon-shape powder of expandable graphitic material having an initial width (first width), which is expanded and exfoliated to a powder …
FIG.3 Schematic of a focused microwave power-based apparatus for producing graphene materials.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
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 of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness, wherein said powder of microwave-expandable un-exfoliated graphite or graphitic carbon further contains 0.1% to 20% by weight of a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Currently amended
The method of claim 1 wherein said microwave-expandable un-exfoliated graphite or graphitic carbon is selected from intercalated natural graphite, oxidized natural graphite, fluorinated natural graphite, intercalated synthetic graphite, oxidized synthetic graphite, fluorinated synthetic graphite, intercalated amorphous graphite, oxidized amorphous graphite, fluorinated amorphous graphite, intercalated highly oriented pyrolytic graphite (HOPG), oxidized HOPG, fluorinated HOPG, intercalated meso-carbon micro-bead, oxidized meso-carbon micro-bead, fluorinated meso-phase carbon, intercalated needle coke, oxidized needle coke, fluorinated needle coke, intercalated carbon or graphite fiber, oxidized carbon or graphite fiber, fluorinated carbon or graphite fiber, intercalated carbon nano-fiber, oxidized carbon nano-fiber, fluorinated carbon nano-fiber, nitrogenated graphite, chlorinated graphite, brominated graphite, iodized graphite, or a combination thereof. Original
The method of claim 1 wherein a residence time for said microwave-expandable un-exfoliated graphite or graphitic carbon in said microwave power zone is from 10 seconds to 5 minutes. Original
The method of claim 1 wherein said residence time is from 30 seconds to 3 minutes. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 mm to 10 cm and said first ribbon thickness is from 10 nm to 3.8 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 5 mm to 5 cm and said first ribbon thickness is from 1 p m to 2.5 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 cm to 3 cm and said first ribbon thickness is from 0.1 mm to 1.0 cm. Original
The method of claim 1 wherein said powder of microwave-expandable un- exfoliated graphite or graphitic carbon is fed and moved into microwave application chamber in a continuous or intermittent manner. Original
The method of claim 1, wherein said graphene sheets are subjected to a mechanical shearing treatment to produce smaller graphene sheets. Original
The method of claim 1 wherein said graphene contains single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a carbon content no less than 95% by weight, or functionalized graphene. Original
Canceled
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness, wherein a ratio of said second width to said first ribbon width is from 3 to 300; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Previously presented
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a volume of the microwave-expandable un-exfoliated graphite or graphitic carbon powder onto a solid substrate surface, wherein the powder volume has a maximum width and a maximum thickness, wherein the microwave-expandable un-exfoliated graphite or graphitic carbon powder further contains a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving the powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein the microwave application width is no less than the maximum width of the powder volume and the microwave penetration depth is no less than the maximum thickness of the powder volume so that the entire powder volume receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate the microwave-expandable un-exfoliated graphite or graphitic carbon into graphene sheets that occupy an expanded volume having a second width, greater than the maximum width, and a second thickness, greater than the maximum thickness; and (c) moving the graphene sheets out of the microwave chamber, cooling the graphene sheets, and collecting the graphene sheets. Currently amended
A focused microwave-based system for producing graphene sheets from a microwave-expandable un-exfoliated graphite or graphitic carbon, said system comprising: (a) solid powder-feeding and guiding means that supplies and feeds a ribbon-shape powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non- metallic solid substrate surface, wherein said ribbon-shape powder has a first ribbon width and a first ribbon thickness; (b) a conveyor device, in working relation to said powder-feeding and guiding device and supporting or containing said non-metallic solid substrate, moves said ribbon-shape powder into at least a microwave applicator chamber; (c) a microwave power supply and power-focusing sub-system that induces a microwave power zone in said microwave application chamber, wherein said microwave power zone has a microwave application width, no less than said first ribbon width, and a microwave penetration depth, no less than said first ribbon thickness, so that the entire ribbon-shape powder receives and absorbs microwave power to form graphene sheets via microwave heat-activated exfoliation and separation of said powder; and (d) a collector to collect said graphene sheets. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a feeder device selected from a vibratory feeder, gravimetric feeder, volumetric auger-type feeder, injector, compressed air-assisted feeder, vacuum-assisted feeder, gravity feeder, drum feeder, wheel feeder, slide, chute, conveyor feeder, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a guiding device to control said first ribbon width and a wiper to control said first thickness of the powder. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system contains multiple microwave application chambers. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system provides a microwave power from 200 W to 200 kW. Withdrawn
The focused microwave-based system of claim 17, further including means of introducing a protective gas atmosphere into said microwave applicator chamber, wherein said protective gas atmosphere contains a noble gas, nitrogen gas, hydrogen gas, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, further including a cooling zone wherein said graphene sheets are cooled after microwave heat-activated exfoliation and separation of said powder. Withdrawn
The focused microwave-based system of claim 17, further including means to allow exhaust gas to exit or scrubber means to capture exhaust gas. Withdrawn
Layer stacks claimed or described, ordered top of device to substrate.
focused microwave-based system for graphene production
No layer stack recorded.
Materials described outside the worked examples.
microwave-expandable un-exfoliated graphite or graphitic carbon
graphene sheets
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Thickness |
Patent
Atlas literature
Patent
US 10,822,239Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing graphite intercalation compound (GIC) or graphite oxide. 15
FIG.2(B) Schematic of a ribbon-shape powder of expandable graphitic material having an initial width (first width), which is expanded and exfoliated to a powder …
FIG.3 Schematic of a focused microwave power-based apparatus for producing graphene materials.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
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 of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness, wherein said powder of microwave-expandable un-exfoliated graphite or graphitic carbon further contains 0.1% to 20% by weight of a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Currently amended
The method of claim 1 wherein said microwave-expandable un-exfoliated graphite or graphitic carbon is selected from intercalated natural graphite, oxidized natural graphite, fluorinated natural graphite, intercalated synthetic graphite, oxidized synthetic graphite, fluorinated synthetic graphite, intercalated amorphous graphite, oxidized amorphous graphite, fluorinated amorphous graphite, intercalated highly oriented pyrolytic graphite (HOPG), oxidized HOPG, fluorinated HOPG, intercalated meso-carbon micro-bead, oxidized meso-carbon micro-bead, fluorinated meso-phase carbon, intercalated needle coke, oxidized needle coke, fluorinated needle coke, intercalated carbon or graphite fiber, oxidized carbon or graphite fiber, fluorinated carbon or graphite fiber, intercalated carbon nano-fiber, oxidized carbon nano-fiber, fluorinated carbon nano-fiber, nitrogenated graphite, chlorinated graphite, brominated graphite, iodized graphite, or a combination thereof. Original
The method of claim 1 wherein a residence time for said microwave-expandable un-exfoliated graphite or graphitic carbon in said microwave power zone is from 10 seconds to 5 minutes. Original
The method of claim 1 wherein said residence time is from 30 seconds to 3 minutes. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 mm to 10 cm and said first ribbon thickness is from 10 nm to 3.8 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 5 mm to 5 cm and said first ribbon thickness is from 1 p m to 2.5 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 cm to 3 cm and said first ribbon thickness is from 0.1 mm to 1.0 cm. Original
The method of claim 1 wherein said powder of microwave-expandable un- exfoliated graphite or graphitic carbon is fed and moved into microwave application chamber in a continuous or intermittent manner. Original
The method of claim 1, wherein said graphene sheets are subjected to a mechanical shearing treatment to produce smaller graphene sheets. Original
The method of claim 1 wherein said graphene contains single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a carbon content no less than 95% by weight, or functionalized graphene. Original
Canceled
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness, wherein a ratio of said second width to said first ribbon width is from 3 to 300; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Previously presented
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a volume of the microwave-expandable un-exfoliated graphite or graphitic carbon powder onto a solid substrate surface, wherein the powder volume has a maximum width and a maximum thickness, wherein the microwave-expandable un-exfoliated graphite or graphitic carbon powder further contains a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving the powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein the microwave application width is no less than the maximum width of the powder volume and the microwave penetration depth is no less than the maximum thickness of the powder volume so that the entire powder volume receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate the microwave-expandable un-exfoliated graphite or graphitic carbon into graphene sheets that occupy an expanded volume having a second width, greater than the maximum width, and a second thickness, greater than the maximum thickness; and (c) moving the graphene sheets out of the microwave chamber, cooling the graphene sheets, and collecting the graphene sheets. Currently amended
A focused microwave-based system for producing graphene sheets from a microwave-expandable un-exfoliated graphite or graphitic carbon, said system comprising: (a) solid powder-feeding and guiding means that supplies and feeds a ribbon-shape powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non- metallic solid substrate surface, wherein said ribbon-shape powder has a first ribbon width and a first ribbon thickness; (b) a conveyor device, in working relation to said powder-feeding and guiding device and supporting or containing said non-metallic solid substrate, moves said ribbon-shape powder into at least a microwave applicator chamber; (c) a microwave power supply and power-focusing sub-system that induces a microwave power zone in said microwave application chamber, wherein said microwave power zone has a microwave application width, no less than said first ribbon width, and a microwave penetration depth, no less than said first ribbon thickness, so that the entire ribbon-shape powder receives and absorbs microwave power to form graphene sheets via microwave heat-activated exfoliation and separation of said powder; and (d) a collector to collect said graphene sheets. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a feeder device selected from a vibratory feeder, gravimetric feeder, volumetric auger-type feeder, injector, compressed air-assisted feeder, vacuum-assisted feeder, gravity feeder, drum feeder, wheel feeder, slide, chute, conveyor feeder, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a guiding device to control said first ribbon width and a wiper to control said first thickness of the powder. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system contains multiple microwave application chambers. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system provides a microwave power from 200 W to 200 kW. Withdrawn
The focused microwave-based system of claim 17, further including means of introducing a protective gas atmosphere into said microwave applicator chamber, wherein said protective gas atmosphere contains a noble gas, nitrogen gas, hydrogen gas, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, further including a cooling zone wherein said graphene sheets are cooled after microwave heat-activated exfoliation and separation of said powder. Withdrawn
The focused microwave-based system of claim 17, further including means to allow exhaust gas to exit or scrubber means to capture exhaust gas. Withdrawn
Layer stacks claimed or described, ordered top of device to substrate.
focused microwave-based system for graphene production
No layer stack recorded.
Materials described outside the worked examples.
microwave-expandable un-exfoliated graphite or graphitic carbon
graphene sheets
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Thickness |
Patent
Atlas literature
Patent
US 10,822,239Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing graphite intercalation compound (GIC) or graphite oxide. 15
FIG.2(B) Schematic of a ribbon-shape powder of expandable graphitic material having an initial width (first width), which is expanded and exfoliated to a powder …
FIG.3 Schematic of a focused microwave power-based apparatus for producing graphene materials.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
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 of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness, wherein said powder of microwave-expandable un-exfoliated graphite or graphitic carbon further contains 0.1% to 20% by weight of a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Currently amended
The method of claim 1 wherein said microwave-expandable un-exfoliated graphite or graphitic carbon is selected from intercalated natural graphite, oxidized natural graphite, fluorinated natural graphite, intercalated synthetic graphite, oxidized synthetic graphite, fluorinated synthetic graphite, intercalated amorphous graphite, oxidized amorphous graphite, fluorinated amorphous graphite, intercalated highly oriented pyrolytic graphite (HOPG), oxidized HOPG, fluorinated HOPG, intercalated meso-carbon micro-bead, oxidized meso-carbon micro-bead, fluorinated meso-phase carbon, intercalated needle coke, oxidized needle coke, fluorinated needle coke, intercalated carbon or graphite fiber, oxidized carbon or graphite fiber, fluorinated carbon or graphite fiber, intercalated carbon nano-fiber, oxidized carbon nano-fiber, fluorinated carbon nano-fiber, nitrogenated graphite, chlorinated graphite, brominated graphite, iodized graphite, or a combination thereof. Original
The method of claim 1 wherein a residence time for said microwave-expandable un-exfoliated graphite or graphitic carbon in said microwave power zone is from 10 seconds to 5 minutes. Original
The method of claim 1 wherein said residence time is from 30 seconds to 3 minutes. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 mm to 10 cm and said first ribbon thickness is from 10 nm to 3.8 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 5 mm to 5 cm and said first ribbon thickness is from 1 p m to 2.5 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 cm to 3 cm and said first ribbon thickness is from 0.1 mm to 1.0 cm. Original
The method of claim 1 wherein said powder of microwave-expandable un- exfoliated graphite or graphitic carbon is fed and moved into microwave application chamber in a continuous or intermittent manner. Original
The method of claim 1, wherein said graphene sheets are subjected to a mechanical shearing treatment to produce smaller graphene sheets. Original
The method of claim 1 wherein said graphene contains single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a carbon content no less than 95% by weight, or functionalized graphene. Original
Canceled
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness, wherein a ratio of said second width to said first ribbon width is from 3 to 300; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Previously presented
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a volume of the microwave-expandable un-exfoliated graphite or graphitic carbon powder onto a solid substrate surface, wherein the powder volume has a maximum width and a maximum thickness, wherein the microwave-expandable un-exfoliated graphite or graphitic carbon powder further contains a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving the powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein the microwave application width is no less than the maximum width of the powder volume and the microwave penetration depth is no less than the maximum thickness of the powder volume so that the entire powder volume receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate the microwave-expandable un-exfoliated graphite or graphitic carbon into graphene sheets that occupy an expanded volume having a second width, greater than the maximum width, and a second thickness, greater than the maximum thickness; and (c) moving the graphene sheets out of the microwave chamber, cooling the graphene sheets, and collecting the graphene sheets. Currently amended
A focused microwave-based system for producing graphene sheets from a microwave-expandable un-exfoliated graphite or graphitic carbon, said system comprising: (a) solid powder-feeding and guiding means that supplies and feeds a ribbon-shape powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non- metallic solid substrate surface, wherein said ribbon-shape powder has a first ribbon width and a first ribbon thickness; (b) a conveyor device, in working relation to said powder-feeding and guiding device and supporting or containing said non-metallic solid substrate, moves said ribbon-shape powder into at least a microwave applicator chamber; (c) a microwave power supply and power-focusing sub-system that induces a microwave power zone in said microwave application chamber, wherein said microwave power zone has a microwave application width, no less than said first ribbon width, and a microwave penetration depth, no less than said first ribbon thickness, so that the entire ribbon-shape powder receives and absorbs microwave power to form graphene sheets via microwave heat-activated exfoliation and separation of said powder; and (d) a collector to collect said graphene sheets. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a feeder device selected from a vibratory feeder, gravimetric feeder, volumetric auger-type feeder, injector, compressed air-assisted feeder, vacuum-assisted feeder, gravity feeder, drum feeder, wheel feeder, slide, chute, conveyor feeder, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a guiding device to control said first ribbon width and a wiper to control said first thickness of the powder. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system contains multiple microwave application chambers. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system provides a microwave power from 200 W to 200 kW. Withdrawn
The focused microwave-based system of claim 17, further including means of introducing a protective gas atmosphere into said microwave applicator chamber, wherein said protective gas atmosphere contains a noble gas, nitrogen gas, hydrogen gas, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, further including a cooling zone wherein said graphene sheets are cooled after microwave heat-activated exfoliation and separation of said powder. Withdrawn
The focused microwave-based system of claim 17, further including means to allow exhaust gas to exit or scrubber means to capture exhaust gas. Withdrawn
Layer stacks claimed or described, ordered top of device to substrate.
focused microwave-based system for graphene production
No layer stack recorded.
Materials described outside the worked examples.
microwave-expandable un-exfoliated graphite or graphitic carbon
graphene sheets
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Thickness |
Patent
Atlas literature
Patent
US 10,822,239Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG.1 A flow chart showing the most commonly used prior art process of producing graphite intercalation compound (GIC) or graphite oxide. 15
FIG.2(B) Schematic of a ribbon-shape powder of expandable graphitic material having an initial width (first width), which is expanded and exfoliated to a powder …
FIG.3 Schematic of a focused microwave power-based apparatus for producing graphene materials.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
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 of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness, wherein said powder of microwave-expandable un-exfoliated graphite or graphitic carbon further contains 0.1% to 20% by weight of a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Currently amended
The method of claim 1 wherein said microwave-expandable un-exfoliated graphite or graphitic carbon is selected from intercalated natural graphite, oxidized natural graphite, fluorinated natural graphite, intercalated synthetic graphite, oxidized synthetic graphite, fluorinated synthetic graphite, intercalated amorphous graphite, oxidized amorphous graphite, fluorinated amorphous graphite, intercalated highly oriented pyrolytic graphite (HOPG), oxidized HOPG, fluorinated HOPG, intercalated meso-carbon micro-bead, oxidized meso-carbon micro-bead, fluorinated meso-phase carbon, intercalated needle coke, oxidized needle coke, fluorinated needle coke, intercalated carbon or graphite fiber, oxidized carbon or graphite fiber, fluorinated carbon or graphite fiber, intercalated carbon nano-fiber, oxidized carbon nano-fiber, fluorinated carbon nano-fiber, nitrogenated graphite, chlorinated graphite, brominated graphite, iodized graphite, or a combination thereof. Original
The method of claim 1 wherein a residence time for said microwave-expandable un-exfoliated graphite or graphitic carbon in said microwave power zone is from 10 seconds to 5 minutes. Original
The method of claim 1 wherein said residence time is from 30 seconds to 3 minutes. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 mm to 10 cm and said first ribbon thickness is from 10 nm to 3.8 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 5 mm to 5 cm and said first ribbon thickness is from 1 p m to 2.5 cm. Original
The method of claim 1 wherein said first ribbon width is selected from the range of 1 cm to 3 cm and said first ribbon thickness is from 0.1 mm to 1.0 cm. Original
The method of claim 1 wherein said powder of microwave-expandable un- exfoliated graphite or graphitic carbon is fed and moved into microwave application chamber in a continuous or intermittent manner. Original
The method of claim 1, wherein said graphene sheets are subjected to a mechanical shearing treatment to produce smaller graphene sheets. Original
The method of claim 1 wherein said graphene contains single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains at least 80% single-layer graphene sheets. Original
The method of claim 1 wherein said graphene contains pristine graphene, oxidized graphene with less than 5% oxygen content by weight, graphene fluoride, graphene fluoride with less than 5% fluorine by weight, graphene with a carbon content no less than 95% by weight, or functionalized graphene. Original
Canceled
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non-metallic solid substrate surface, wherein said powder is in a substantially ribbon shape having a first ribbon width and a first ribbon thickness; (b) moving said ribbon-shape powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein said microwave application width is no less than said first ribbon width and said microwave penetration depth is no less than said first ribbon thickness so that the entire ribbon-shape powder receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate said microwave-expandable un-exfoliated graphite or graphitic carbon for producing graphene sheets that occupy an expanded volume having a second width, greater than said first ribbon width, and a second thickness, greater than said first ribbon thickness, wherein a ratio of said second width to said first ribbon width is from 3 to 300; and (c) moving said graphene sheets out of said microwave chamber, cooling said graphene sheets, and collecting said graphene sheets. Previously presented
A method of producing graphene from a microwave-expandable un- exfoliated graphite or graphitic carbon, said method comprising: (a) supplying and feeding a volume of the microwave-expandable un-exfoliated graphite or graphitic carbon powder onto a solid substrate surface, wherein the powder volume has a maximum width and a maximum thickness, wherein the microwave-expandable un-exfoliated graphite or graphitic carbon powder further contains a dielectric heating promotor selected from water, polar organic molecule, or a combination thereof; (b) moving the powder into a microwave applicator chamber containing a microwave power zone having a microwave application width and a microwave penetration depth, wherein the microwave application width is no less than the maximum width of the powder volume and the microwave penetration depth is no less than the maximum thickness of the powder volume so that the entire powder volume receives and absorbs microwave power with a sufficient power level for a sufficient length of time to exfoliate and separate the microwave-expandable un-exfoliated graphite or graphitic carbon into graphene sheets that occupy an expanded volume having a second width, greater than the maximum width, and a second thickness, greater than the maximum thickness; and (c) moving the graphene sheets out of the microwave chamber, cooling the graphene sheets, and collecting the graphene sheets. Currently amended
A focused microwave-based system for producing graphene sheets from a microwave-expandable un-exfoliated graphite or graphitic carbon, said system comprising: (a) solid powder-feeding and guiding means that supplies and feeds a ribbon-shape powder of said microwave-expandable un-exfoliated graphite or graphitic carbon onto a non- metallic solid substrate surface, wherein said ribbon-shape powder has a first ribbon width and a first ribbon thickness; (b) a conveyor device, in working relation to said powder-feeding and guiding device and supporting or containing said non-metallic solid substrate, moves said ribbon-shape powder into at least a microwave applicator chamber; (c) a microwave power supply and power-focusing sub-system that induces a microwave power zone in said microwave application chamber, wherein said microwave power zone has a microwave application width, no less than said first ribbon width, and a microwave penetration depth, no less than said first ribbon thickness, so that the entire ribbon-shape powder receives and absorbs microwave power to form graphene sheets via microwave heat-activated exfoliation and separation of said powder; and (d) a collector to collect said graphene sheets. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a feeder device selected from a vibratory feeder, gravimetric feeder, volumetric auger-type feeder, injector, compressed air-assisted feeder, vacuum-assisted feeder, gravity feeder, drum feeder, wheel feeder, slide, chute, conveyor feeder, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, wherein said solid powder- feeding and guiding means contains a guiding device to control said first ribbon width and a wiper to control said first thickness of the powder. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system contains multiple microwave application chambers. Withdrawn
The focused microwave-based system of claim 17, wherein said microwave power supply and power-focusing sub-system provides a microwave power from 200 W to 200 kW. Withdrawn
The focused microwave-based system of claim 17, further including means of introducing a protective gas atmosphere into said microwave applicator chamber, wherein said protective gas atmosphere contains a noble gas, nitrogen gas, hydrogen gas, or a combination thereof. Withdrawn
The focused microwave-based system of claim 17, further including a cooling zone wherein said graphene sheets are cooled after microwave heat-activated exfoliation and separation of said powder. Withdrawn
The focused microwave-based system of claim 17, further including means to allow exhaust gas to exit or scrubber means to capture exhaust gas. Withdrawn
Layer stacks claimed or described, ordered top of device to substrate.
focused microwave-based system for graphene production
No layer stack recorded.
Materials described outside the worked examples.
microwave-expandable un-exfoliated graphite or graphitic carbon
graphene sheets
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG.4 A TEM image of representative graphene sheets produced by the instant method.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Thickness | 0.34–3.4 nm | — |
Thickness |
dielectric heating promotor (water, polar organic molecule, or combination)
oxidized graphene with less than 5% oxygen content by weight
graphene fluoride with less than 5% fluorine by weight
functionalized graphene
| — |
Duration | 0.5–96 hours | — |
Duration | 48–72 hours | — |
Duration | 5–120 hours | — |
Temperature | 800–1200 °C | — |
Temperature | 950–1050 °C | — |
Temperature | 150–250 °C | — |
Duration | 2–5 hours | — |
Duration | 48–96 hours | — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 1 minute | — |
Duration | 10–300 s | — |
Duration | 30–180 s | — |
Thickness | 1000000–100000000 nm | — |
Thickness | 10–38000000 nm | — |
Thickness | 5000000–50000000 nm | — |
Thickness | 1–3 cm | — |
Thickness | 100000–10000000 nm | — |
dielectric heating promotor (water, polar organic molecule, or combination)
oxidized graphene with less than 5% oxygen content by weight
graphene fluoride with less than 5% fluorine by weight
functionalized graphene
| — |
Duration | 0.5–96 hours | — |
Duration | 48–72 hours | — |
Duration | 5–120 hours | — |
Temperature | 800–1200 °C | — |
Temperature | 950–1050 °C | — |
Temperature | 150–250 °C | — |
Duration | 2–5 hours | — |
Duration | 48–96 hours | — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 1 minute | — |
Duration | 10–300 s | — |
Duration | 30–180 s | — |
Thickness | 1000000–100000000 nm | — |
Thickness | 10–38000000 nm | — |
Thickness | 5000000–50000000 nm | — |
Thickness | 1–3 cm | — |
Thickness | 100000–10000000 nm | — |
dielectric heating promotor (water, polar organic molecule, or combination)
oxidized graphene with less than 5% oxygen content by weight
graphene fluoride with less than 5% fluorine by weight
functionalized graphene
| — |
Duration | 0.5–96 hours | — |
Duration | 48–72 hours | — |
Duration | 5–120 hours | — |
Temperature | 800–1200 °C | — |
Temperature | 950–1050 °C | — |
Temperature | 150–250 °C | — |
Duration | 2–5 hours | — |
Duration | 48–96 hours | — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 1 minute | — |
Duration | 10–300 s | — |
Duration | 30–180 s | — |
Thickness | 1000000–100000000 nm | — |
Thickness | 10–38000000 nm | — |
Thickness | 5000000–50000000 nm | — |
Thickness | 1–3 cm | — |
Thickness | 100000–10000000 nm | — |
dielectric heating promotor (water, polar organic molecule, or combination)
oxidized graphene with less than 5% oxygen content by weight
graphene fluoride with less than 5% fluorine by weight
functionalized graphene
| — |
Duration | 0.5–96 hours | — |
Duration | 48–72 hours | — |
Duration | 5–120 hours | — |
Temperature | 800–1200 °C | — |
Temperature | 950–1050 °C | — |
Temperature | 150–250 °C | — |
Duration | 2–5 hours | — |
Duration | 48–96 hours | — |
Duration | ≤ 5 minutes | — |
Duration | ≤ 3 minutes | — |
Duration | ≤ 1 minute | — |
Duration | 10–300 s | — |
Duration | 30–180 s | — |
Thickness | 1000000–100000000 nm | — |
Thickness | 10–38000000 nm | — |
Thickness | 5000000–50000000 nm | — |
Thickness | 1–3 cm | — |
Thickness | 100000–10000000 nm | — |
