Patent
US 9,993,749FAST PRODUCTION OF HIGH QUALITY GRAPHENE BY LIQUID PHASE EXFOLIATION
Horst Henning Winter
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 9,993,749Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 4 is a flow diagram illustrating the process by which pristine graphite particles 402 are processed with chaotic- fl ow induced collisions to produce …
FIG. 5 is a schematic diagram of a chaotic fl ow apparatus for pre-treating the graphite suspension. The sample holders rotate around their inwards tilted axis …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
FIG. 14 is a schematic diagram of one embodiment of a batch or semi continuous graphene exfoliation process. [0061]
FIG. 15 is a schematic diagram of another embodiment of a batch or semi continuous graphene exfoliation process. [0062]
FIG. 16 is a schematic diagram of one embodiment of a continuous graphene process using recirculation without a grinder/mixer. [0063]
FIG. 17 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0064]
FIG. 18 is a schematic diagram of one embodiment of a continuous graphene process that uses recirculation without a grinder/mixer. [0065]
FIG. 19 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0066] Fig. 20 schematically …
FIG. 20 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer after the slurry has partially …
FIG. 21 schematically illustrates features of a continuous graphene process using two centrifuges.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) centrifuging said first suspension created in step (b) to create a supe rn atant and a sediment; (d) separating of said supernatant from said sediment; (e) dispersing said sediment in a second liquid to create a second suspension; (f) sonicating said second suspension that resulted from step (e); (g) centrifuging said second suspension that resulted from step (f); (h) separating said second suspension into a second supernatant and a second sediment; (i) recovering at least one graphene flake having a thickness of one to three graphene layers from said second supernatant; and (j) dispersing said second sediment in a third liquid to create a third suspension for recirculation. Currently amended
The sequential process of claim 1, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 1, wherein said first liquid used in step (a) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said second liquid used in step (d-) (e) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said first liquid used in step (a) or said second liquid used in step (4) (e) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein step (b) involves the use of grinding particles. Original
The sequential process of claim 1, wherein either centrifuging step is performed in a solid bowl centrifuge. Original
The sequential process of claim 1, further comprising the step of adding fluid to said suspension of unexfoliated graphite from the centrifuge before pumping it into the step of sonication. Original
The sequential process of claim 1, further comprising, upon recirculation of the third suspension, performing a further flow treatment and a further sonicating. New
Canceled
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) sonicating said first suspension that resulted from step (b); (d) centrifuging said first suspension that resulted from step (c); (e) separating said first suspension into a supernatant and a sediment; (f) recovering at least one graphene flake having a thickness of one to three graphene layers from said supernatant; and (g) dispersing said sediment in a second liquid to create a second suspension for recirculation. Currently amended
The sequential process of claim 10, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 10, wherein said first liquid used in step (a) or said second liquid used in step (0 (g) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 10, wherein step (e) (b) involves the use of pebbles. Currently amended
Canceled
Materials described outside the worked examples.
graphitic material
graphene flakes (one to three graphene layers)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene concentration determined by UV-Vis (Lambert-Beer law, a=3620 ml mg^-1 m^-1) | — | graphene flakes (one to three graphene layers) |
quadrupled graphene yield achieved by introducing chaotic flow pretreatment |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,993,749Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 4 is a flow diagram illustrating the process by which pristine graphite particles 402 are processed with chaotic- fl ow induced collisions to produce …
FIG. 5 is a schematic diagram of a chaotic fl ow apparatus for pre-treating the graphite suspension. The sample holders rotate around their inwards tilted axis …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
FIG. 14 is a schematic diagram of one embodiment of a batch or semi continuous graphene exfoliation process. [0061]
FIG. 15 is a schematic diagram of another embodiment of a batch or semi continuous graphene exfoliation process. [0062]
FIG. 16 is a schematic diagram of one embodiment of a continuous graphene process using recirculation without a grinder/mixer. [0063]
FIG. 17 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0064]
FIG. 18 is a schematic diagram of one embodiment of a continuous graphene process that uses recirculation without a grinder/mixer. [0065]
FIG. 19 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0066] Fig. 20 schematically …
FIG. 20 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer after the slurry has partially …
FIG. 21 schematically illustrates features of a continuous graphene process using two centrifuges.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) centrifuging said first suspension created in step (b) to create a supe rn atant and a sediment; (d) separating of said supernatant from said sediment; (e) dispersing said sediment in a second liquid to create a second suspension; (f) sonicating said second suspension that resulted from step (e); (g) centrifuging said second suspension that resulted from step (f); (h) separating said second suspension into a second supernatant and a second sediment; (i) recovering at least one graphene flake having a thickness of one to three graphene layers from said second supernatant; and (j) dispersing said second sediment in a third liquid to create a third suspension for recirculation. Currently amended
The sequential process of claim 1, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 1, wherein said first liquid used in step (a) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said second liquid used in step (d-) (e) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said first liquid used in step (a) or said second liquid used in step (4) (e) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein step (b) involves the use of grinding particles. Original
The sequential process of claim 1, wherein either centrifuging step is performed in a solid bowl centrifuge. Original
The sequential process of claim 1, further comprising the step of adding fluid to said suspension of unexfoliated graphite from the centrifuge before pumping it into the step of sonication. Original
The sequential process of claim 1, further comprising, upon recirculation of the third suspension, performing a further flow treatment and a further sonicating. New
Canceled
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) sonicating said first suspension that resulted from step (b); (d) centrifuging said first suspension that resulted from step (c); (e) separating said first suspension into a supernatant and a sediment; (f) recovering at least one graphene flake having a thickness of one to three graphene layers from said supernatant; and (g) dispersing said sediment in a second liquid to create a second suspension for recirculation. Currently amended
The sequential process of claim 10, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 10, wherein said first liquid used in step (a) or said second liquid used in step (0 (g) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 10, wherein step (e) (b) involves the use of pebbles. Currently amended
Canceled
Materials described outside the worked examples.
graphitic material
graphene flakes (one to three graphene layers)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene concentration determined by UV-Vis (Lambert-Beer law, a=3620 ml mg^-1 m^-1) | — | graphene flakes (one to three graphene layers) |
quadrupled graphene yield achieved by introducing chaotic flow pretreatment |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,993,749Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 4 is a flow diagram illustrating the process by which pristine graphite particles 402 are processed with chaotic- fl ow induced collisions to produce …
FIG. 5 is a schematic diagram of a chaotic fl ow apparatus for pre-treating the graphite suspension. The sample holders rotate around their inwards tilted axis …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
FIG. 14 is a schematic diagram of one embodiment of a batch or semi continuous graphene exfoliation process. [0061]
FIG. 15 is a schematic diagram of another embodiment of a batch or semi continuous graphene exfoliation process. [0062]
FIG. 16 is a schematic diagram of one embodiment of a continuous graphene process using recirculation without a grinder/mixer. [0063]
FIG. 17 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0064]
FIG. 18 is a schematic diagram of one embodiment of a continuous graphene process that uses recirculation without a grinder/mixer. [0065]
FIG. 19 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0066] Fig. 20 schematically …
FIG. 20 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer after the slurry has partially …
FIG. 21 schematically illustrates features of a continuous graphene process using two centrifuges.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) centrifuging said first suspension created in step (b) to create a supe rn atant and a sediment; (d) separating of said supernatant from said sediment; (e) dispersing said sediment in a second liquid to create a second suspension; (f) sonicating said second suspension that resulted from step (e); (g) centrifuging said second suspension that resulted from step (f); (h) separating said second suspension into a second supernatant and a second sediment; (i) recovering at least one graphene flake having a thickness of one to three graphene layers from said second supernatant; and (j) dispersing said second sediment in a third liquid to create a third suspension for recirculation. Currently amended
The sequential process of claim 1, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 1, wherein said first liquid used in step (a) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said second liquid used in step (d-) (e) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said first liquid used in step (a) or said second liquid used in step (4) (e) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein step (b) involves the use of grinding particles. Original
The sequential process of claim 1, wherein either centrifuging step is performed in a solid bowl centrifuge. Original
The sequential process of claim 1, further comprising the step of adding fluid to said suspension of unexfoliated graphite from the centrifuge before pumping it into the step of sonication. Original
The sequential process of claim 1, further comprising, upon recirculation of the third suspension, performing a further flow treatment and a further sonicating. New
Canceled
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) sonicating said first suspension that resulted from step (b); (d) centrifuging said first suspension that resulted from step (c); (e) separating said first suspension into a supernatant and a sediment; (f) recovering at least one graphene flake having a thickness of one to three graphene layers from said supernatant; and (g) dispersing said sediment in a second liquid to create a second suspension for recirculation. Currently amended
The sequential process of claim 10, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 10, wherein said first liquid used in step (a) or said second liquid used in step (0 (g) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 10, wherein step (e) (b) involves the use of pebbles. Currently amended
Canceled
Materials described outside the worked examples.
graphitic material
graphene flakes (one to three graphene layers)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene concentration determined by UV-Vis (Lambert-Beer law, a=3620 ml mg^-1 m^-1) | — | graphene flakes (one to three graphene layers) |
quadrupled graphene yield achieved by introducing chaotic flow pretreatment |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,993,749Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 4 is a flow diagram illustrating the process by which pristine graphite particles 402 are processed with chaotic- fl ow induced collisions to produce …
FIG. 5 is a schematic diagram of a chaotic fl ow apparatus for pre-treating the graphite suspension. The sample holders rotate around their inwards tilted axis …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
FIG. 14 is a schematic diagram of one embodiment of a batch or semi continuous graphene exfoliation process. [0061]
FIG. 15 is a schematic diagram of another embodiment of a batch or semi continuous graphene exfoliation process. [0062]
FIG. 16 is a schematic diagram of one embodiment of a continuous graphene process using recirculation without a grinder/mixer. [0063]
FIG. 17 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0064]
FIG. 18 is a schematic diagram of one embodiment of a continuous graphene process that uses recirculation without a grinder/mixer. [0065]
FIG. 19 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer. [0066] Fig. 20 schematically …
FIG. 20 is a schematic diagram of one embodiment of a continuous graphene process with recirculation through a grinder/mixer after the slurry has partially …
FIG. 21 schematically illustrates features of a continuous graphene process using two centrifuges.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) centrifuging said first suspension created in step (b) to create a supe rn atant and a sediment; (d) separating of said supernatant from said sediment; (e) dispersing said sediment in a second liquid to create a second suspension; (f) sonicating said second suspension that resulted from step (e); (g) centrifuging said second suspension that resulted from step (f); (h) separating said second suspension into a second supernatant and a second sediment; (i) recovering at least one graphene flake having a thickness of one to three graphene layers from said second supernatant; and (j) dispersing said second sediment in a third liquid to create a third suspension for recirculation. Currently amended
The sequential process of claim 1, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 1, wherein said first liquid used in step (a) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said second liquid used in step (d-) (e) is N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein said first liquid used in step (a) or said second liquid used in step (4) (e) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 1, wherein step (b) involves the use of grinding particles. Original
The sequential process of claim 1, wherein either centrifuging step is performed in a solid bowl centrifuge. Original
The sequential process of claim 1, further comprising the step of adding fluid to said suspension of unexfoliated graphite from the centrifuge before pumping it into the step of sonication. Original
The sequential process of claim 1, further comprising, upon recirculation of the third suspension, performing a further flow treatment and a further sonicating. New
Canceled
A sequential process for exfoliation of graphite to produce graphene flakes with a thickness of one to three graphene layers, comprising the steps of: (a) creating a first suspension of a graphitic material in a first liquid; (b) treating said first suspension in a flow treatment, the flow treatment being sufficiently benign that the number of at least one of bent edges and bent corners is increased without reducing the lateral size of the graphitic particles below 10 microns; (c) sonicating said first suspension that resulted from step (b); (d) centrifuging said first suspension that resulted from step (c); (e) separating said first suspension into a supernatant and a sediment; (f) recovering at least one graphene flake having a thickness of one to three graphene layers from said supernatant; and (g) dispersing said sediment in a second liquid to create a second suspension for recirculation. Currently amended
The sequential process of claim 10, wherein said graphitic material is pristine graphite. Original
The sequential process of claim 10, wherein said first liquid used in step (a) or said second liquid used in step (0 (g) comprises N-methyl pyrolidone. Currently amended
The sequential process of claim 10, wherein step (e) (b) involves the use of pebbles. Currently amended
Canceled
Materials described outside the worked examples.
graphitic material
graphene flakes (one to three graphene layers)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1 B is an image that demonstrates the Tyndall effect generated by graphene colloids produced via direct 0.5h sonication (Vial A) and novel ChF-pretreatment …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene concentration determined by UV-Vis (Lambert-Beer law, a=3620 ml mg^-1 m^-1) | — | graphene flakes (one to three graphene layers) |
quadrupled graphene yield achieved by introducing chaotic flow pretreatment |
Related documents with shared materials, methods, properties, or citations.
pristine graphite
N-methyl pyrrolidone (NMP)
C₅H₉NO
stabilized zirconium oxide rods (pebbles)
zirconium oxide (95% ZrO2, 5% Y₂O₃)
ZrO₂
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
graphene flakes (one to three graphene layers) |
Thickness | 0.4–1 nm | — |
Duration | 0.5–8 hours | — |
Thickness | 400–1000 nm | — |
Thickness | ≤ 10 µm | — |
pristine graphite
N-methyl pyrrolidone (NMP)
C₅H₉NO
stabilized zirconium oxide rods (pebbles)
zirconium oxide (95% ZrO2, 5% Y₂O₃)
ZrO₂
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
graphene flakes (one to three graphene layers) |
Thickness | 0.4–1 nm | — |
Duration | 0.5–8 hours | — |
Thickness | 400–1000 nm | — |
Thickness | ≤ 10 µm | — |
pristine graphite
N-methyl pyrrolidone (NMP)
C₅H₉NO
stabilized zirconium oxide rods (pebbles)
zirconium oxide (95% ZrO2, 5% Y₂O₃)
ZrO₂
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
graphene flakes (one to three graphene layers) |
Thickness | 0.4–1 nm | — |
Duration | 0.5–8 hours | — |
Thickness | 400–1000 nm | — |
Thickness | ≤ 10 µm | — |
pristine graphite
N-methyl pyrrolidone (NMP)
C₅H₉NO
stabilized zirconium oxide rods (pebbles)
zirconium oxide (95% ZrO2, 5% Y₂O₃)
ZrO₂
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 2A is an AFM height image of graphene flakes produced via ChF- sonication (8h) and deposited on silicon, with detailed measurements at locations 202, 204 …
FIG. 3F is a close up SEM image of sediment produced after 2 m in of chaotic flow processing in which a particle may be seen with a "dog-ear" 302 in the upper …
FIG. 6 is a diagram showing the representative UV-vis absorbance curves of the GS/NMP colloid. Curve 602 is for the chaotic-flow pre-treatment followed by 0.5h …
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 7C is another 2 dimensional AF M height image of ChF-Sonication produced graphene flakes deposited on Si substrate. [0047]
FIG. 8D are HRTEM images of ChF-Sonication produced graphene flakes deposited on Si substrate. [0050]
FIG. 9A. Below each of the images is the corresponding height pro fi le taken along the marked horizontal line. [0052]
FIG. 10 A is a TEM image of a graphene flake generated by direct sonication of pristine graphite. [0053] FIG. lO B is a SAED pattern of the black circle area in …
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 11 C is a graph of powder XRD patterns of completely dried graphite powder (curve 1102) and ChF-Sonication graphene (curve 1104) [0057]
FIG. 12D are three zoomed-in 2 dimensional AFM height images of three individual flakes (scale bar represents 100 nm). Below each of the images is the …
FIG. 13 is a graph of graphene concentration after chaotic flow treatment and centrifugation as a function of chaotic flow time. [0060]
graphene flakes (one to three graphene layers) |
Thickness | 0.4–1 nm | — |
Duration | 0.5–8 hours | — |
Thickness | 400–1000 nm | — |
Thickness | ≤ 10 µm | — |