Patent
US 11,970,399 B2THREE-DIMENSIONAL (3D) PRINTING OF GRAPHENE MATERIALS
James M. Tour, Junwei Sha, Yilun Li, Jordan Miller et al.
William Marsh Rice University, Houston, TX (US)·Apr. 30, 2024·US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 11,970,399 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 2C are photographs of 3D printed graphene foam before and after dissolving Ni. The scale bars are 5 mm.
FIG. 3 is a schematic of powder metallurgy-chemical method to prepare 3D graphene foam.
FIG. 4B is a schematic of changing the shape of the pellet to prepare 3D rebar GF in screw shape. 50
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 6 is a schematic of the synthesis of 3D printed Ni/graphene discs. 60
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 8B.
FIGS. 9A-9B are photographs of a power bed system utilized for embodiments of the present invention.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIG. 13B is a schematic of the preparation of 3D graphene material from 3D printed metal/binder object.
FIG. 14 is a photograph of as-printed 3D Ni/binder objects. (70% saturation was used for the 3D printing).
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 18C-18D were intact after CPD drying, but were cut into two pieces before the photographs were taken. 5
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 28A) Raman 65 spectrum, (
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
FIGS. 30A-30B are DMA results of as-prepared 3D printed graphene foam after removing Ni prepared using 100P and 2S in a H₂ atmosphere: (
FIGS. 35 2A-2F of the Tour ’060 PCT Application.
FIGS. 65 27A-27C). The high magnification image in
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 making a 3D graphene material compris-ing: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein 35 (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and 50 (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, B₂ (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form the 3D graphene material.
The method of claim 1, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
The method of claim 1, wherein the laser is set at a scanning speed of at least about 1000 mm/min.
The method of claim 1, wherein the laser is set at a power of at least 4 W.
The method of claim 1, wherein the metal powder comprises a metal is selected from a group consisting of Ni, Cu, Ni—Cu alloys, Ru, Ag, Fe, Co, Al, and combinations and alloys thereof.
The method of claim 1, wherein the metal powder comprise Ni.
The method of claim 1, wherein the metal powder has an average particle size in the range between about 100 nm and about 1 cm.
The method of claim 1, wherein the carbon source comprises a material selected from a group consisting of sucrose, polymethyl methacrylate, glucose, poly(phenylene sulfide), carbohydrates, poly(acrylonitrile), polysaccharides, polyimide, and combinations thereof.
The method of claim 1, wherein the carbon source comprises sucrose.
The method of claim 1, wherein weight ratio of the metal powder to the carbon source is between about 1:1 and 20:1.
The method of claim 1, wherein the 3D graphene material is selected from a group consisting of in-situ N-doped graphene foams, carbon nanotube/graphene com-posites, carbon fibers, carbon nanotube fibers, carbon nanoo-nions/graphene composites, phosphorene foams, 3D MX and/or MX₂ foams, and combinations thereof, wherein (a) M is selected from a group consisting of Mo, W, Bi, Hf, Ga, Ge, Ta, Sn, Zn, Cd, Pb, B, Nb, Zr, and combinations thereof, and (b) X is selected from a group consisting of S, N, Se, P, and combinations thereof.
The method of claim 1, wherein the 3D graphene material has a porosity of at least 98%.
The method of claim 1, wherein the 3D graphene material is a graphene foam.
The method of claim 1, wherein the 3D graphene material has an average pore diameter in the range between 1 nm and about 1 cm.
The method of claim 1, wherein the 3D graphene material comprises a surface area ranging from about m2/g to about 2,500 m2/g.
The method of claim 1, wherein the 3D graphene material has an electrical conductivity ranging from about 6.9 S/cm and about 10.5 D/cm.
The method of claim 1, wherein the 3D graphene material has a mechanical robustness that is at least about 11 kPa storage modulus.
The method of claim 1, wherein the 3D graphene material has a damping capacity of at least 0.05.
The method of claim 1, wherein the step of removing the metal to form the 3D graphene material comprises etching away the metal.
The method of claim 1, wherein the metal powder is at room temperature and the metal powder and the carbon source are converted into graphene sheets that cover the metal powder without preheating.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in air.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in an atmosphere of H2, Ar, or both.
The method of claim 1 wherein the step of converting the carbon source into graphene sheets that cover the metal powder further comprises a step of heat treatment.
The method of claim 1, wherein the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in water, and then removing the water to form the metal and carbon source mixture.
The method of claim 1, wherein (a) the carbon source is an organic polymer, and (b) the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in a solvent, and then removing the solvent to form the metal and carbon source mixture.
A method comprising: 30 (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that 45 at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source B₂ mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into a device.
The method of claim 26, wherein the device is selected from is a group consisting of electrodes, battery electrodes, capacitors, supercapacitors, batteries, lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, mechanical dampening devices, cell scaffolds for artificial wood, scaffolds for growth of bone or animal/human tissue in vivo or in vitro, scaffolds for neuronal growth in vitro or in vivo, and spinal cord regeneration scaffolds.
The method of claim 26, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene. ∗ ∗ ∗ ∗ ∗
A method comprising: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into an elec-trode.
The method of claim 28 further comprising incorpo-rating the electrode into a device that is selected from a group consisting of capacitors, supercapacitors, batteries, B₂ lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, and mechanical dampening devices.
The method of claim 28, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
Materials described outside the worked examples.
3D graphene material
metal powder
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
porosity of 3D graphene material | ≥ 98 % | 3D graphene material |
electrical conductivity of 3D graphene material | 6.9–10.5 S/cm |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 10
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,970,399 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 2C are photographs of 3D printed graphene foam before and after dissolving Ni. The scale bars are 5 mm.
FIG. 3 is a schematic of powder metallurgy-chemical method to prepare 3D graphene foam.
FIG. 4B is a schematic of changing the shape of the pellet to prepare 3D rebar GF in screw shape. 50
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 6 is a schematic of the synthesis of 3D printed Ni/graphene discs. 60
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 8B.
FIGS. 9A-9B are photographs of a power bed system utilized for embodiments of the present invention.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIG. 13B is a schematic of the preparation of 3D graphene material from 3D printed metal/binder object.
FIG. 14 is a photograph of as-printed 3D Ni/binder objects. (70% saturation was used for the 3D printing).
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 18C-18D were intact after CPD drying, but were cut into two pieces before the photographs were taken. 5
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 28A) Raman 65 spectrum, (
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
FIGS. 30A-30B are DMA results of as-prepared 3D printed graphene foam after removing Ni prepared using 100P and 2S in a H₂ atmosphere: (
FIGS. 35 2A-2F of the Tour ’060 PCT Application.
FIGS. 65 27A-27C). The high magnification image in
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 making a 3D graphene material compris-ing: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein 35 (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and 50 (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, B₂ (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form the 3D graphene material.
The method of claim 1, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
The method of claim 1, wherein the laser is set at a scanning speed of at least about 1000 mm/min.
The method of claim 1, wherein the laser is set at a power of at least 4 W.
The method of claim 1, wherein the metal powder comprises a metal is selected from a group consisting of Ni, Cu, Ni—Cu alloys, Ru, Ag, Fe, Co, Al, and combinations and alloys thereof.
The method of claim 1, wherein the metal powder comprise Ni.
The method of claim 1, wherein the metal powder has an average particle size in the range between about 100 nm and about 1 cm.
The method of claim 1, wherein the carbon source comprises a material selected from a group consisting of sucrose, polymethyl methacrylate, glucose, poly(phenylene sulfide), carbohydrates, poly(acrylonitrile), polysaccharides, polyimide, and combinations thereof.
The method of claim 1, wherein the carbon source comprises sucrose.
The method of claim 1, wherein weight ratio of the metal powder to the carbon source is between about 1:1 and 20:1.
The method of claim 1, wherein the 3D graphene material is selected from a group consisting of in-situ N-doped graphene foams, carbon nanotube/graphene com-posites, carbon fibers, carbon nanotube fibers, carbon nanoo-nions/graphene composites, phosphorene foams, 3D MX and/or MX₂ foams, and combinations thereof, wherein (a) M is selected from a group consisting of Mo, W, Bi, Hf, Ga, Ge, Ta, Sn, Zn, Cd, Pb, B, Nb, Zr, and combinations thereof, and (b) X is selected from a group consisting of S, N, Se, P, and combinations thereof.
The method of claim 1, wherein the 3D graphene material has a porosity of at least 98%.
The method of claim 1, wherein the 3D graphene material is a graphene foam.
The method of claim 1, wherein the 3D graphene material has an average pore diameter in the range between 1 nm and about 1 cm.
The method of claim 1, wherein the 3D graphene material comprises a surface area ranging from about m2/g to about 2,500 m2/g.
The method of claim 1, wherein the 3D graphene material has an electrical conductivity ranging from about 6.9 S/cm and about 10.5 D/cm.
The method of claim 1, wherein the 3D graphene material has a mechanical robustness that is at least about 11 kPa storage modulus.
The method of claim 1, wherein the 3D graphene material has a damping capacity of at least 0.05.
The method of claim 1, wherein the step of removing the metal to form the 3D graphene material comprises etching away the metal.
The method of claim 1, wherein the metal powder is at room temperature and the metal powder and the carbon source are converted into graphene sheets that cover the metal powder without preheating.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in air.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in an atmosphere of H2, Ar, or both.
The method of claim 1 wherein the step of converting the carbon source into graphene sheets that cover the metal powder further comprises a step of heat treatment.
The method of claim 1, wherein the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in water, and then removing the water to form the metal and carbon source mixture.
The method of claim 1, wherein (a) the carbon source is an organic polymer, and (b) the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in a solvent, and then removing the solvent to form the metal and carbon source mixture.
A method comprising: 30 (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that 45 at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source B₂ mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into a device.
The method of claim 26, wherein the device is selected from is a group consisting of electrodes, battery electrodes, capacitors, supercapacitors, batteries, lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, mechanical dampening devices, cell scaffolds for artificial wood, scaffolds for growth of bone or animal/human tissue in vivo or in vitro, scaffolds for neuronal growth in vitro or in vivo, and spinal cord regeneration scaffolds.
The method of claim 26, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene. ∗ ∗ ∗ ∗ ∗
A method comprising: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into an elec-trode.
The method of claim 28 further comprising incorpo-rating the electrode into a device that is selected from a group consisting of capacitors, supercapacitors, batteries, B₂ lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, and mechanical dampening devices.
The method of claim 28, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
Materials described outside the worked examples.
3D graphene material
metal powder
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
porosity of 3D graphene material | ≥ 98 % | 3D graphene material |
electrical conductivity of 3D graphene material | 6.9–10.5 S/cm |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 10
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,970,399 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 2C are photographs of 3D printed graphene foam before and after dissolving Ni. The scale bars are 5 mm.
FIG. 3 is a schematic of powder metallurgy-chemical method to prepare 3D graphene foam.
FIG. 4B is a schematic of changing the shape of the pellet to prepare 3D rebar GF in screw shape. 50
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 6 is a schematic of the synthesis of 3D printed Ni/graphene discs. 60
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 8B.
FIGS. 9A-9B are photographs of a power bed system utilized for embodiments of the present invention.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIG. 13B is a schematic of the preparation of 3D graphene material from 3D printed metal/binder object.
FIG. 14 is a photograph of as-printed 3D Ni/binder objects. (70% saturation was used for the 3D printing).
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 18C-18D were intact after CPD drying, but were cut into two pieces before the photographs were taken. 5
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 28A) Raman 65 spectrum, (
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
FIGS. 30A-30B are DMA results of as-prepared 3D printed graphene foam after removing Ni prepared using 100P and 2S in a H₂ atmosphere: (
FIGS. 35 2A-2F of the Tour ’060 PCT Application.
FIGS. 65 27A-27C). The high magnification image in
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 making a 3D graphene material compris-ing: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein 35 (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and 50 (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, B₂ (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form the 3D graphene material.
The method of claim 1, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
The method of claim 1, wherein the laser is set at a scanning speed of at least about 1000 mm/min.
The method of claim 1, wherein the laser is set at a power of at least 4 W.
The method of claim 1, wherein the metal powder comprises a metal is selected from a group consisting of Ni, Cu, Ni—Cu alloys, Ru, Ag, Fe, Co, Al, and combinations and alloys thereof.
The method of claim 1, wherein the metal powder comprise Ni.
The method of claim 1, wherein the metal powder has an average particle size in the range between about 100 nm and about 1 cm.
The method of claim 1, wherein the carbon source comprises a material selected from a group consisting of sucrose, polymethyl methacrylate, glucose, poly(phenylene sulfide), carbohydrates, poly(acrylonitrile), polysaccharides, polyimide, and combinations thereof.
The method of claim 1, wherein the carbon source comprises sucrose.
The method of claim 1, wherein weight ratio of the metal powder to the carbon source is between about 1:1 and 20:1.
The method of claim 1, wherein the 3D graphene material is selected from a group consisting of in-situ N-doped graphene foams, carbon nanotube/graphene com-posites, carbon fibers, carbon nanotube fibers, carbon nanoo-nions/graphene composites, phosphorene foams, 3D MX and/or MX₂ foams, and combinations thereof, wherein (a) M is selected from a group consisting of Mo, W, Bi, Hf, Ga, Ge, Ta, Sn, Zn, Cd, Pb, B, Nb, Zr, and combinations thereof, and (b) X is selected from a group consisting of S, N, Se, P, and combinations thereof.
The method of claim 1, wherein the 3D graphene material has a porosity of at least 98%.
The method of claim 1, wherein the 3D graphene material is a graphene foam.
The method of claim 1, wherein the 3D graphene material has an average pore diameter in the range between 1 nm and about 1 cm.
The method of claim 1, wherein the 3D graphene material comprises a surface area ranging from about m2/g to about 2,500 m2/g.
The method of claim 1, wherein the 3D graphene material has an electrical conductivity ranging from about 6.9 S/cm and about 10.5 D/cm.
The method of claim 1, wherein the 3D graphene material has a mechanical robustness that is at least about 11 kPa storage modulus.
The method of claim 1, wherein the 3D graphene material has a damping capacity of at least 0.05.
The method of claim 1, wherein the step of removing the metal to form the 3D graphene material comprises etching away the metal.
The method of claim 1, wherein the metal powder is at room temperature and the metal powder and the carbon source are converted into graphene sheets that cover the metal powder without preheating.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in air.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in an atmosphere of H2, Ar, or both.
The method of claim 1 wherein the step of converting the carbon source into graphene sheets that cover the metal powder further comprises a step of heat treatment.
The method of claim 1, wherein the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in water, and then removing the water to form the metal and carbon source mixture.
The method of claim 1, wherein (a) the carbon source is an organic polymer, and (b) the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in a solvent, and then removing the solvent to form the metal and carbon source mixture.
A method comprising: 30 (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that 45 at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source B₂ mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into a device.
The method of claim 26, wherein the device is selected from is a group consisting of electrodes, battery electrodes, capacitors, supercapacitors, batteries, lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, mechanical dampening devices, cell scaffolds for artificial wood, scaffolds for growth of bone or animal/human tissue in vivo or in vitro, scaffolds for neuronal growth in vitro or in vivo, and spinal cord regeneration scaffolds.
The method of claim 26, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene. ∗ ∗ ∗ ∗ ∗
A method comprising: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into an elec-trode.
The method of claim 28 further comprising incorpo-rating the electrode into a device that is selected from a group consisting of capacitors, supercapacitors, batteries, B₂ lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, and mechanical dampening devices.
The method of claim 28, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
Materials described outside the worked examples.
3D graphene material
metal powder
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
porosity of 3D graphene material | ≥ 98 % | 3D graphene material |
electrical conductivity of 3D graphene material | 6.9–10.5 S/cm |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 10
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,970,399 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 2C are photographs of 3D printed graphene foam before and after dissolving Ni. The scale bars are 5 mm.
FIG. 3 is a schematic of powder metallurgy-chemical method to prepare 3D graphene foam.
FIG. 4B is a schematic of changing the shape of the pellet to prepare 3D rebar GF in screw shape. 50
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 6 is a schematic of the synthesis of 3D printed Ni/graphene discs. 60
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 8B.
FIGS. 9A-9B are photographs of a power bed system utilized for embodiments of the present invention.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIG. 13B is a schematic of the preparation of 3D graphene material from 3D printed metal/binder object.
FIG. 14 is a photograph of as-printed 3D Ni/binder objects. (70% saturation was used for the 3D printing).
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 18C-18D were intact after CPD drying, but were cut into two pieces before the photographs were taken. 5
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 28A) Raman 65 spectrum, (
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
FIGS. 30A-30B are DMA results of as-prepared 3D printed graphene foam after removing Ni prepared using 100P and 2S in a H₂ atmosphere: (
FIGS. 35 2A-2F of the Tour ’060 PCT Application.
FIGS. 65 27A-27C). The high magnification image in
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 making a 3D graphene material compris-ing: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein 35 (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and 50 (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, B₂ (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form the 3D graphene material.
The method of claim 1, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
The method of claim 1, wherein the laser is set at a scanning speed of at least about 1000 mm/min.
The method of claim 1, wherein the laser is set at a power of at least 4 W.
The method of claim 1, wherein the metal powder comprises a metal is selected from a group consisting of Ni, Cu, Ni—Cu alloys, Ru, Ag, Fe, Co, Al, and combinations and alloys thereof.
The method of claim 1, wherein the metal powder comprise Ni.
The method of claim 1, wherein the metal powder has an average particle size in the range between about 100 nm and about 1 cm.
The method of claim 1, wherein the carbon source comprises a material selected from a group consisting of sucrose, polymethyl methacrylate, glucose, poly(phenylene sulfide), carbohydrates, poly(acrylonitrile), polysaccharides, polyimide, and combinations thereof.
The method of claim 1, wherein the carbon source comprises sucrose.
The method of claim 1, wherein weight ratio of the metal powder to the carbon source is between about 1:1 and 20:1.
The method of claim 1, wherein the 3D graphene material is selected from a group consisting of in-situ N-doped graphene foams, carbon nanotube/graphene com-posites, carbon fibers, carbon nanotube fibers, carbon nanoo-nions/graphene composites, phosphorene foams, 3D MX and/or MX₂ foams, and combinations thereof, wherein (a) M is selected from a group consisting of Mo, W, Bi, Hf, Ga, Ge, Ta, Sn, Zn, Cd, Pb, B, Nb, Zr, and combinations thereof, and (b) X is selected from a group consisting of S, N, Se, P, and combinations thereof.
The method of claim 1, wherein the 3D graphene material has a porosity of at least 98%.
The method of claim 1, wherein the 3D graphene material is a graphene foam.
The method of claim 1, wherein the 3D graphene material has an average pore diameter in the range between 1 nm and about 1 cm.
The method of claim 1, wherein the 3D graphene material comprises a surface area ranging from about m2/g to about 2,500 m2/g.
The method of claim 1, wherein the 3D graphene material has an electrical conductivity ranging from about 6.9 S/cm and about 10.5 D/cm.
The method of claim 1, wherein the 3D graphene material has a mechanical robustness that is at least about 11 kPa storage modulus.
The method of claim 1, wherein the 3D graphene material has a damping capacity of at least 0.05.
The method of claim 1, wherein the step of removing the metal to form the 3D graphene material comprises etching away the metal.
The method of claim 1, wherein the metal powder is at room temperature and the metal powder and the carbon source are converted into graphene sheets that cover the metal powder without preheating.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in air.
The method of claim 1, wherein the step of converting the carbon source into graphene sheets that cover the metal powder is performed in an atmosphere of H2, Ar, or both.
The method of claim 1 wherein the step of converting the carbon source into graphene sheets that cover the metal powder further comprises a step of heat treatment.
The method of claim 1, wherein the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in water, and then removing the water to form the metal and carbon source mixture.
The method of claim 1, wherein (a) the carbon source is an organic polymer, and (b) the step of mixing the metal powder and the carbon source to form the metal and carbon source mixture comprises mixing the metal powder and the carbon source in a solvent, and then removing the solvent to form the metal and carbon source mixture.
A method comprising: 30 (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that 45 at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source B₂ mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; and (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into a device.
The method of claim 26, wherein the device is selected from is a group consisting of electrodes, battery electrodes, capacitors, supercapacitors, batteries, lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, mechanical dampening devices, cell scaffolds for artificial wood, scaffolds for growth of bone or animal/human tissue in vivo or in vitro, scaffolds for neuronal growth in vitro or in vivo, and spinal cord regeneration scaffolds.
The method of claim 26, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene. ∗ ∗ ∗ ∗ ∗
A method comprising: (a) mixing a metal powder and a carbon source to form a metal and carbon source mixture, wherein (i) the carbon source is not graphene, graphene oxide, or a graphene derivative, and (ii) at least some of the metal powder is covered by the carbon source; (b) utilizing a 3D printing process to fuse the metal powder in the metal and carbon source mixture into a specific structure, wherein the 3D printing process comprises (i) depositing one or more layers of the metal and carbon source mixture, (ii) performing a first laser sintering step, wherein (A) the metal powder in the one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together to form a laser sintered structure comprising metal, (iii) depositing an additional one or more layers of the metal and carbon source mixture on the laser sintered structure, (iv) performing an additional laser sintering step, wherein (A) the metal powder in the additional one or more layers of the metal and carbon source mixture is fused such that at least some of the metal power bonds together and bonds with the metal of the laser sintered structure to form a further laser sintered structure comprising the metal, and (v) repeating steps (iii)-(iv) utilizing the further laser sintered structure as the laser sintered structure, to form the specific structure comprising the metal; (c) using a laser to convert the carbon source in the metal and carbon source mixture into graphene to form a graphene and metal scaffold, wherein (i) during or after performing the first laser sintering step, using a laser to convert the carbon source in the one or more layers of the metal and carbon source mixture into first graphene that is on a surface and interface regions of the laser sintered structure, (ii) during or after performing the additional laser sintering step, using the laser to convert the carbon source in the additional one or more layers of the metal and carbon source mixture into additional graphene that is on a surface and interface regions of the further laser sintered structure, (iii) the graphene and metal scaffold comprises the specific structure and the graphene, wherein the graphene comprises the first graphene and the addi-tional graphene, and (iv) the graphene is on a surface and interface regions of the specific structure; (d) removing the metal from the graphene and metal scaffold to form 3D graphene material; and (e) incorporating the 3D graphene material into an elec-trode.
The method of claim 28 further comprising incorpo-rating the electrode into a device that is selected from a group consisting of capacitors, supercapacitors, batteries, B₂ lithium batteries, lithium ion batteries, photovoltaic devices, photovoltaic cells, transistors, current collectors, fuel cell devices, water desalination devices, capacitive deionization devices, water-splitting devices, water-oil separation devices, water/gas purification devices, sensors, and mechanical dampening devices.
The method of claim 28, wherein (a) the first laser sintering step is performed while per-forming the step of using the laser to convert the carbon source into the first graphene; and (b) the additional laser sintering step is performed while performing the step of using the laser to convert the carbon source into the additional graphene.
Materials described outside the worked examples.
3D graphene material
metal powder
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
porosity of 3D graphene material | ≥ 98 % | 3D graphene material |
electrical conductivity of 3D graphene material | 6.9–10.5 S/cm |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 10
Related documents with shared materials, methods, properties, or citations.
carbon source
Ni powder
Ni
sucrose
C₁₂H₂₂O₁₁
graphene foam
Ni powder with sucrose
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
mechanical robustness (storage modulus) of 3D graphene material | ≥ 11 kPa | 3D graphene material |
damping capacity of 3D graphene material | ≥ 0.05 | 3D graphene material |
BET surface area of 3D graphene material | ≤ 2500 m2/g | 3D graphene material |
Thickness | 1–10000000 nm | — |
Thickness | 1–500 nm | — |
Thickness | 100–10000000 nm | — |
Thickness | 1–100 µm | — |
Thickness | 2.2–3 µm | — |
Thickness | ≥ 1 mm | — |
— | ≥ 4 W | — |
Thickness | 1–10 nm | — |
Flow Rate | 500–1000 sccm | — |
Pressure | 5–15 Torr | — |
Thickness | ≤ 1 nm | — |
— | ≥ 15 W | — |
— | ≥ 37.5 W | — |
Temperature | ≥ 800 °C | — |
Temperature | ≥ 1 °C | — |
Duration | ≥ 10 minutes | — |
Cited non-patent literature · 3
carbon source
Ni powder
Ni
sucrose
C₁₂H₂₂O₁₁
graphene foam
Ni powder with sucrose
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
mechanical robustness (storage modulus) of 3D graphene material | ≥ 11 kPa | 3D graphene material |
damping capacity of 3D graphene material | ≥ 0.05 | 3D graphene material |
BET surface area of 3D graphene material | ≤ 2500 m2/g | 3D graphene material |
Thickness | 1–10000000 nm | — |
Thickness | 1–500 nm | — |
Thickness | 100–10000000 nm | — |
Thickness | 1–100 µm | — |
Thickness | 2.2–3 µm | — |
Thickness | ≥ 1 mm | — |
— | ≥ 4 W | — |
Thickness | 1–10 nm | — |
Flow Rate | 500–1000 sccm | — |
Pressure | 5–15 Torr | — |
Thickness | ≤ 1 nm | — |
— | ≥ 15 W | — |
— | ≥ 37.5 W | — |
Temperature | ≥ 800 °C | — |
Temperature | ≥ 1 °C | — |
Duration | ≥ 10 minutes | — |
Cited non-patent literature · 3
carbon source
Ni powder
Ni
sucrose
C₁₂H₂₂O₁₁
graphene foam
Ni powder with sucrose
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
mechanical robustness (storage modulus) of 3D graphene material | ≥ 11 kPa | 3D graphene material |
damping capacity of 3D graphene material | ≥ 0.05 | 3D graphene material |
BET surface area of 3D graphene material | ≤ 2500 m2/g | 3D graphene material |
Thickness | 1–10000000 nm | — |
Thickness | 1–500 nm | — |
Thickness | 100–10000000 nm | — |
Thickness | 1–100 µm | — |
Thickness | 2.2–3 µm | — |
Thickness | ≥ 1 mm | — |
— | ≥ 4 W | — |
Thickness | 1–10 nm | — |
Flow Rate | 500–1000 sccm | — |
Pressure | 5–15 Torr | — |
Thickness | ≤ 1 nm | — |
— | ≥ 15 W | — |
— | ≥ 37.5 W | — |
Temperature | ≥ 800 °C | — |
Temperature | ≥ 1 °C | — |
Duration | ≥ 10 minutes | — |
Cited non-patent literature · 3
carbon source
Ni powder
Ni
sucrose
C₁₂H₂₂O₁₁
graphene foam
Ni powder with sucrose
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIG. 1B is an SEM image of LIG patterned into an owl 20 shape (scale bar, 1 mm). The bright contrast corresponds to LIG surrounded by the darker-colored …
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIGS. 5A-5C are SEM images of graphene grown by laser 55 using Ni/sucrose precursor.
FIG. 7 is the Raman spectra of 3D printed Ni/graphene discs using 10, 20, 50, and 100% of power.
FIG. 10 is the Raman spectra of laser-irradiated Ni/su- crose powders with different laser scanning speeds.
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIGS. 11E-11F are, respectively, an SEM image and the Raman spectra of a laser-irradiated Ni/sucrose powder with a laser setting of 2,000 mm/min, 100% power of …
FIG. 12 is an ATR-IR spectra of Ni powder, sucrose, and Ni/sucrose hybrid powder.
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 15C-15D are Raman characterizations for the 3D printed Ni/binder objects shown in
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 16A-16B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 17A-17B are SEM images for as-grown 3D Ni/gra- phene objects after CVD treatments with
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 19C-19D are Raman characterizations for the 3D graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 20C-20D are Raman characterizations for the 3D 20 graphene foam after CPD drying shown in
FIGS. 21A-21H are SEM images of 3D printed graphene foams with a Ni scaffold prepared using 100P and (
FIGS. 22A-22D are low magnification SEM images of 3D printed graphene foams with Ni scaffold prepared using 100P and (
FIGS. 23A-23H are SEM images of 3D printed graphene foams with Ni scaffold prepared using 5S and (
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIGS. 24A-24B are SEM images of a Ni/sucrose mixture sample without laser treatment.
FIG. 25A.
FIG. 25A.
FIGS. 26A-26B are Raman spectra of 3D printed gra- phene foams with a Ni scaffold prepared using (
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIGS. 27D-27F are TEM images of 3D printed graphene foams after removing Ni scaffolds prepared using 100P and 2S in a H₂ atmosphere. The inset in
FIG. 29A is a schematic diagram of electrical conductiv- ity testing. The scale bar is 1 cm.
mechanical robustness (storage modulus) of 3D graphene material | ≥ 11 kPa | 3D graphene material |
damping capacity of 3D graphene material | ≥ 0.05 | 3D graphene material |
BET surface area of 3D graphene material | ≤ 2500 m2/g | 3D graphene material |
Thickness | 1–10000000 nm | — |
Thickness | 1–500 nm | — |
Thickness | 100–10000000 nm | — |
Thickness | 1–100 µm | — |
Thickness | 2.2–3 µm | — |
Thickness | ≥ 1 mm | — |
— | ≥ 4 W | — |
Thickness | 1–10 nm | — |
Flow Rate | 500–1000 sccm | — |
Pressure | 5–15 Torr | — |
Thickness | ≤ 1 nm | — |
— | ≥ 15 W | — |
— | ≥ 37.5 W | — |
Temperature | ≥ 800 °C | — |
Temperature | ≥ 1 °C | — |
Duration | ≥ 10 minutes | — |
Cited non-patent literature · 3