CN116332163A - Method for rapidly preparing graphene - Google Patents
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- CN116332163A CN116332163A CN202310240019.2A CN202310240019A CN116332163A CN 116332163 A CN116332163 A CN 116332163A CN 202310240019 A CN202310240019 A CN 202310240019A CN 116332163 A CN116332163 A CN 116332163A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 67
- 239000010439 graphite Substances 0.000 claims abstract description 67
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims description 10
- 238000000748 compression moulding Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 239000010410 layer Substances 0.000 abstract description 10
- 239000002356 single layer Substances 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000005411 Van der Waals force Methods 0.000 abstract description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
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- 238000002441 X-ray diffraction Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
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- 239000007772 electrode material Substances 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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- 239000002033 PVDF binder Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
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- 230000037303 wrinkles Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
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Abstract
The invention belongs to the technical field of graphene preparation, and particularly relates to a method for rapidly preparing graphene. The invention provides a method for rapidly preparing graphene, which comprises the following steps: pressing and forming graphite oxide, and then performing flash firing treatment to obtain the graphene; the temperature of the flash treatment is 1000-5000 ℃, and the heat preservation time is 5-500 s. In the invention, in the process of flash firing treatment, the energy of the graphite oxide can be raised instantly, and the thermal movement of the hydroxyl, carboxyl and other oxygen-containing groups on the carbon layer is stimulated, and the reduction of the single-layer graphite oxide is realized through the rapid decomposition and removal of the oxygen-containing groups; meanwhile, the removed oxygen can damage Van der Waals force between the graphite layers, so that stripping between the graphite layers is realized, and finally the graphene is obtained.
Description
Technical Field
The invention belongs to the technical field of graphene preparation, and particularly relates to a method for rapidly preparing graphene.
Background
The existing methods for preparing the graphene mainly comprise a chemical vapor deposition method, a micromechanical stripping method, a chemical stripping method and the like.
The micromechanical stripping method is to strip flake graphite and the like layer by using the adhesive force of the adhesive tape through multiple adhesion, then adhere the adhesive tape with a graphite flake to a target substrate such as a silicon chip and the like, and finally remove the adhesive tape by using solvents such as acetone and the like, so that the single-layer graphene is obtained.
The chemical vapor deposition method takes carbon-containing compounds such as methane and the like as carbon sources, and the graphene grows by high-temperature decomposition on the surface of a machine body, so that the graphene prepared by the method has high quality and can grow in a large area, but the reactant methane required by the reaction is expensive, and the dangerous degree in the experimental operation process is high.
The chemical stripping method is to introduce functional groups on carbon atoms of a graphite layer by utilizing oxidation-reduction reaction, so that the interlayer spacing of graphite is increased, interlayer interaction is weakened, then the graphene oxide layer is separated layer by ultrasonic or rapid expansion to obtain graphene oxide, and finally oxygen-containing functional groups are removed by chemical reduction or high-temperature reduction and other methods to obtain the graphene. The method is an effective method capable of preparing graphene in a large quantity at present, but the preparation period is long, carbon atoms are often lost in the oxidation, ultrasonic and subsequent reduction processes, and the prepared graphene contains more defects, so that the conductivity is poor.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing graphene, which has short production period and can obtain graphene with excellent conductivity.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for rapidly preparing graphene, which comprises the following steps:
pressing and forming graphite oxide, and then performing flash firing treatment to obtain the graphene;
the temperature of the flash treatment is 1000-5000 ℃, and the heat preservation time is 5-500 s.
Preferably, the oxygen content of the graphite oxide is 0.1 to 30%.
Preferably, the flash treatment is performed in a protective atmosphere.
Preferably, the flash treatment is performed at normal pressure.
Preferably, before the compression molding, grinding the graphite oxide; the particle size of the milled graphite oxide is 1-50 mu m.
Preferably, the pressure of the compression molding is 18-24 MPa, and the dwell time is 5-20 s.
Preferably, the heating rate to the flash treatment temperature is 90-300 ℃/s.
Preferably, the flash firing process includes:
and placing the pressed graphite oxide on a conductive carrier, connecting the two ends of the conductive carrier with the anode and the cathode of a power supply, and electrifying to perform flash burning treatment.
Preferably, the conductive carrier comprises carbon paper, graphite sheet, molybdenum boat, tungsten boat or stainless steel sheet;
the thickness of the conductive carrier is 0.1-10 mm.
Preferably, the current for the energization is 1 to 500A.
The invention provides a method for rapidly preparing graphene, which comprises the following steps: pressing and forming graphite oxide, and then performing flash firing treatment to obtain the graphene; the temperature of the flash treatment is 1000-5000 ℃, and the heat preservation time is 5-500 s. In the invention, in the process of flash firing treatment, the energy of graphite oxide can be instantaneously raised to generate strong thermal shock, and the thermal motion of hydroxyl, carboxyl and other oxygen-containing groups on a carbon layer is stimulated, and the reduction of single-layer graphite oxide is realized through the rapid decomposition and removal of the oxygen-containing groups; meanwhile, the removed oxygen can damage Van der Waals force between the graphite layers, so that stripping between the graphite layers is realized, and finally the graphene is obtained.
Drawings
Fig. 1 is an SEM image of graphene obtained in example 1;
fig. 2 is an SEM image of graphene obtained in example 2;
fig. 3 is an SEM image of graphene obtained in example 3;
fig. 4 is an SEM image of graphene obtained in comparative example 1;
FIG. 5 is an SEM image of graphite oxide;
fig. 6 is a TEM image of graphene obtained in example 1;
FIG. 7 is an XRD pattern of graphite oxide;
FIG. 8 is an XRD pattern of graphene obtained in example 1;
fig. 9 is a graph showing the rate performance of a sodium ion half cell assembled by using graphene obtained in example 1 as an electrode material;
fig. 10 is a cycle performance chart of a sodium ion half cell assembled by using graphene obtained in example 1 as an electrode material;
FIG. 11 is a schematic view of the apparatus of the present invention during a flash process.
Detailed Description
The invention provides a method for rapidly preparing graphene, which comprises the following steps:
pressing and forming graphite oxide, and then performing flash firing treatment to obtain the graphene;
the temperature of the flash treatment is 1000-5000 ℃, and the heat preservation time is 5-500 s.
In the present invention, all raw materials are commercially available products well known to those skilled in the art unless specified otherwise.
In the present invention, the oxygen content of the graphite oxide is preferably 0.1 to 30%, more preferably 5 to 25%, and even more preferably 10 to 20%.
The present invention also preferably includes grinding the graphite oxide prior to the press forming.
In the present invention, the time for the grinding is preferably 10 minutes. In the present invention, the particle diameter of the milled graphite oxide is preferably 1 to 50. Mu.m, more preferably 5 to 40. Mu.m, and still more preferably 20 to 30. Mu.m. In the present invention, the grinding is preferably performed in a mortar.
In the present invention, the pressure of the press molding is preferably 18 to 24MPa, more preferably 19 to 23MPa, and still more preferably 20 to 22MPa; the dwell time is preferably 5 to 20s, more preferably 8 to 18s, still more preferably 10 to 15s.
In the invention, the diameter of the graphite oxide sheet obtained after the compression molding is preferably 12-13 mm, and the thickness is preferably 0.1cm; the mass of the individual graphite oxide flakes is preferably 20 to 100mg.
In the present invention, the temperature of the flash treatment is 1000 to 5000 ℃, more preferably 1500 to 4000 ℃, still more preferably 2000 to 3000 ℃; the heating rate to the flash treatment temperature is preferably 90 to 300 ℃/s, more preferably 100 to 250 ℃/s, and even more preferably 150 to 200 ℃/s; the holding time is 5 to 500 seconds, more preferably 50 to 400 seconds, still more preferably 100 to 300 seconds.
In the present invention, the flash treatment is preferably performed in a protective atmosphere; the protective atmosphere is preferably nitrogen.
In the present invention, the flash treatment is preferably performed under normal pressure.
In the present invention, the flash treatment preferably includes:
and placing the pressed graphite oxide on a conductive carrier, connecting the two ends of the conductive carrier with the anode and the cathode of a power supply, and electrifying to perform flash burning treatment.
In the present invention, the conductive carrier preferably includes carbon paper, graphite sheet, molybdenum boat, tungsten boat or stainless steel sheet. In the present invention, the thickness of the conductive carrier is preferably 0.1 to 10mm, more preferably 1 to 9mm, and still more preferably 2 to 8mm. In a specific embodiment of the present invention, the size of the carbon paper is preferably 10cm×5cm×1mm; the positive electrode and the negative electrode of the power supply are preferably connected with the short sides of the carbon paper respectively. The schematic diagram of the device provided by the invention is shown in fig. 11.
In the present invention, the current to be applied is preferably 1 to 500A, more preferably 50 to 400A, and even more preferably 100 to 300A.
For further explanation of the present invention, a method for rapidly preparing graphene according to the present invention is described in detail below with reference to the accompanying drawings and examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Placing graphite oxide with the oxygen content of 20% in a mortar, grinding for 20min, placing the obtained graphite oxide (with the particle size of 20-30 mu m) in a die, performing compression molding under the pressure of 15MPa, and maintaining the pressure for 20s to obtain graphite oxide sheets (with the mass of about 51 mg) with the diameter of 12mm and the thickness of 0.1cm;
and placing the obtained graphite oxide sheet on carbon paper with the size of 10cm x 5cm x 1mm, respectively connecting the short sides of the carbon paper with the anode and the cathode of a power supply, and electrifying under normal pressure and nitrogen atmosphere to perform flash treatment, wherein the current is 160A, the flash treatment temperature is 1300 ℃, the heating rate is 90 ℃/s, and the heat preservation time is 100s, so as to obtain the graphene.
Example 2
Placing graphite oxide with the oxygen content of 20% in a mortar, grinding for 20min, placing the obtained graphite oxide (with the particle size of 20-30 mu m) in a die, performing compression molding under the pressure of 15MPa, and maintaining the pressure for 20s to obtain graphite oxide sheets (with the mass of about 51 mg) with the diameter of 12mm and the thickness of 0.1cm;
and placing the obtained graphite oxide sheet on carbon paper with the size of 10cm x 5cm x 1mm, respectively connecting the short sides of the carbon paper with the anode and the cathode of a power supply, and electrifying under normal pressure and nitrogen atmosphere to perform flash treatment, wherein the current is 150A, the flash treatment temperature is 1200 ℃, the heating rate is 90 ℃/s, and the heat preservation time is 100s, so as to obtain the graphene.
Example 3
Placing graphite oxide with the oxygen content of 20% in a mortar, grinding for 20min, placing the obtained graphite oxide (with the particle size of 20-30 mu m) in a die, performing compression molding under the pressure of 15MPa, and maintaining the pressure for 20s to obtain graphite oxide sheets (with the mass of about 51 mg) with the diameter of 12mm and the thickness of 0.1cm;
and placing the obtained graphite oxide sheet on carbon paper with the size of 10cm x 5cm x 1mm, respectively connecting the short sides of the carbon paper with the anode and the cathode of a power supply, and electrifying under normal pressure and nitrogen atmosphere to perform flash treatment, wherein the current is 180A, the flash treatment temperature is 1500 ℃, the heating rate is 100 ℃/s, and the heat preservation time is 100s, so as to obtain the graphene.
Example 4
Placing graphite oxide with the oxygen content of 20% in a mortar, grinding for 20min, placing the obtained graphite oxide (with the particle size of 20-30 mu m) in a die, performing compression molding under the pressure of 15MPa, and maintaining the pressure for 20s to obtain graphite oxide sheets (with the mass of about 51 mg) with the diameter of 12mm and the thickness of 0.1cm;
and placing the obtained graphite oxide sheet on carbon paper with the size of 10cm x 5cm x 1mm, respectively connecting the short sides of the carbon paper with the anode and the cathode of a power supply, and electrifying under normal pressure and nitrogen atmosphere to perform flash treatment, wherein the current is 200A, the flash treatment temperature is 2500 ℃, the heating rate is 200 ℃/s, and the heat preservation time is 50s, so as to obtain the graphene.
Comparative example 1
Placing graphite oxide with the oxygen content of 20% in a mortar, grinding for 20min, placing the obtained graphite oxide (with the particle size of 20-30 mu m) in a die, performing compression molding under the pressure of 15MPa, and maintaining the pressure for 20s to obtain graphite oxide sheets (with the mass of about 51 mg) with the diameter of 12mm and the thickness of 0.1cm;
and (3) placing the obtained graphite oxide sheet on carbon paper with the size of 10cm x 5cm x 1mm, then placing the carbon paper in a tube furnace, carbonizing at a high temperature of 1500 ℃ under normal pressure and nitrogen atmosphere, and obtaining a sample, wherein the heating rate is 30 ℃/min and the heat preservation time is 10 h.
Performance testing
Test example 1
Scanning electron microscope tests are carried out on the graphene and graphite oxide raw materials obtained in examples 1-3 and comparative example 1, and the obtained SEM images are shown in figures 1-5, wherein figure 1 is example 1, figure 2 is example 2, figure 3 is example 3, figure 4 is comparative example 1, and figure 5 is graphite oxide, and as can be seen from figures 1-5, the graphite oxide is of a monolithic structure and has no obvious lamellar structure; in the comparative example, the graphite oxide is not completely peeled off, and the block structure of the graphite oxide still exists; the graphene obtained by the method has a layered fold structure, and the single-layer graphene sheet is very thin.
Test example 2
Transmission electron microscopy is carried out on the graphene obtained in the embodiment 1, the obtained TEM image is shown in fig. 6, and it can be seen from fig. 6 that the graphene shows a transparent structure, which indicates that the graphene is very thin, and wrinkles can be observed in a partial area of the sample, which is caused by overlapping graphene sheets or curling edges; meanwhile, the graphene surface has obvious texture, and is smooth and orderly.
Test example 3
The graphene obtained in the embodiment 1 and the graphite oxide raw material are subjected to an X-ray diffraction test, the obtained XRD patterns are shown in figures 7 and 8, wherein figure 7 is graphite oxide, and figure 8 is embodiment 1, and as can be seen from figures 7-8, the graphene provided by the invention has diffraction peaks near 23 degrees of 2 theta, the peaks are widened and weakened, and the intensity is very close to that of the graphite 2 theta, so that the experimental product is graphene; after the graphite oxide is changed into graphene, the (001) crystal plane diffraction peak in fig. 7 completely disappears, which indicates that the graphite oxide has been completely reduced into a single-layer graphene; the broadening of the graphene diffraction peaks is due to interlayer exfoliation of the single layer graphite, and the reduction in monolithic size, decrease in crystalline structure integrity and increase in disorder.
Test example 4
The graphene obtained in the example 3 is used as an electrode active material, and electrochemical performance is tested;
mixing graphene, acetylene black and PVDF solution (dissolved in polypyrrolidone) with the mass concentration of 2% according to the proportion of 8:1:1, mixing to be sticky, coating the mixture on a copper current collector, then drying the mixture in a vacuum drying oven at 110 ℃ for 12 hours, cutting a pole piece with the diameter of 12mm by a cutting machine, weighing, and calculating the loading amount of the graphene on the pole piece to be about 2 mg; drying in an oven at 60 ℃ for 6 hours to obtain a positive electrode;
in a glove box protected by argon, a metal sodium sheet is used as a negative electrode, a glass fiber membrane is used as a diaphragm, and 1mol/LNaPF is used 6 (EC: dmc=1:1) as electrolyte, assembled into a 2032 type button sodium ion half-cell;
testing the half-cell in a constant current charge-discharge mode, wherein the current density is 0.05A/g-10A/g, the voltage range is 0.01-3V, and the obtained test curves are shown in figures 9 and 10;
wherein FIG. 9 is a graph of rate performance, as can be seen from FIG. 9, the specific capacity at a current density of 0.05A/g is 200mAh/g, and the specific capacity at a current density of 10A/g is 30mAh/g, with excellent rate performance;
FIG. 10 is a graph of cycle performance, and as can be seen from FIG. 10, there is still a specific capacity of 100mAh/g after 100 cycles of 0.1A/g, indicating that the material has a high specific capacity and high cycle stability.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. The method for rapidly preparing the graphene is characterized by comprising the following steps of:
pressing and forming graphite oxide, and then performing flash firing treatment to obtain the graphene;
the temperature of the flash treatment is 1000-5000 ℃, and the heat preservation time is 5-500 s.
2. The method of claim 1, wherein the graphite oxide has an oxygen content of 0.1 to 30%.
3. The method of claim 1, wherein the flash treatment is performed in a protective atmosphere.
4. A method according to claim 1 or 3, characterized in that the flash treatment is carried out at atmospheric pressure.
5. The method of claim 1, further comprising grinding the graphite oxide prior to the compression molding; the particle size of the milled graphite oxide is 1-50 mu m.
6. The method according to claim 1, wherein the pressure of the press forming is 18 to 24MPa and the dwell time is 5 to 20s.
7. The method according to claim 1, wherein the rate of heating up to the flash treatment temperature is 90 to 300 ℃/s.
8. The method of claim 1, wherein the flash processing comprises:
and placing the pressed graphite oxide on a conductive carrier, connecting the two ends of the conductive carrier with the anode and the cathode of a power supply, and electrifying to perform flash burning treatment.
9. The method of claim 8, wherein the conductive carrier comprises carbon paper, graphite sheet, molybdenum boat, tungsten boat, or stainless steel sheet;
the thickness of the conductive carrier is 0.1-10 mm.
10. The method of claim 8, wherein the energized current is 1-500A.
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| CN113003567A (en) * | 2021-05-06 | 2021-06-22 | 哈尔滨工程大学 | Device and method for reducing graphene oxide |
| CN113165880A (en) * | 2018-09-05 | 2021-07-23 | 威廉马什赖斯大学 | Flash joule heating synthesis method and composition thereof |
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| US20130015409A1 (en) * | 2009-12-18 | 2013-01-17 | Bunshi Fugetsu | Graphene oxide sheet, article containing graphene-containing substance produced by reducing the graphene oxide sheet, and process for production of the graphene oxide sheet |
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