CN109264708B - Method for manufacturing two-dimensional material - Google Patents
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- CN109264708B CN109264708B CN201811158662.6A CN201811158662A CN109264708B CN 109264708 B CN109264708 B CN 109264708B CN 201811158662 A CN201811158662 A CN 201811158662A CN 109264708 B CN109264708 B CN 109264708B
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- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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Abstract
The invention discloses a manufacturing method of a two-dimensional material. The manufacturing method comprises the following steps: ionizing the intercalation gas: putting a raw material for manufacturing a two-dimensional material into a reaction kettle, enabling the raw material to be in contact with the negative electrode of a direct current electrode plate, vacuumizing the reaction kettle, introducing intercalation gas to enable the pressure in the kettle to reach a certain pressure, and then opening a plasma generator to ionize the intercalation gas; then, turning on a power supply of the direct current electrode plate to discharge so that positive ions between the single-layer substances are converted into gas molecules after capturing electrons; obtaining a two-dimensional material precursor; ultrasonic stripping: introducing a dispersion liquid containing a separant into a reaction kettle, displacing intercalation gas, carrying out ultrasonic stripping treatment on a two-dimensional material precursor, heating simultaneously, and finishing ultrasonic stripping after keeping for a certain time; optionally, further heating and pressurizing for decomposition to obtain a mixture of the release agent and the two-dimensional material; and finally, sequentially carrying out water washing, purification and drying on the mixture to obtain the two-dimensional material. Compared with the prior art, the invention has the beneficial effects that: the process has the advantages of continuous production, high single-layer rate, extremely low cost and large-scale production.
Description
Technical Field
The invention belongs to the technical field of material manufacturing, and particularly relates to a manufacturing method of a two-dimensional material.
Background
As science develops, the manufacturing microscale recording of materials is constantly being refreshed, and monoatomic or monomolecular steady-state materials have recently emerged. Two-dimensional materials, currently defined temporarily as materials in which electrons are free to move (planar motion) only in two dimensions, on a non-nanoscale (1-100nm), have three fundamental features: 1) the structure is ordered; 2) growing on a two-dimensional plane; 3) and is ultra-thin in the third dimension. Common organic class of two-dimensional materials are: two-dimensional biphenyls and biphenyls; two-dimensional materials of the inorganic type such as: graphene and graphene, two-dimensional hexagonal boron nitride, oxide sulfide selenide of two-dimensional transition group metals, black phosphorus alkene and the like.
The more two-dimensional materials studied at present are represented by the two-dimensional material of carbon, graphene, and the advantages and disadvantages of several common manufacturing methods are listed as follows:
firstly, a mechanical stripping method: the micro-nano manufacturing and stripping method and device are simple to operate, high in product quality and are the main method and device for preparing single-layer high-quality graphene at present. But the controllability is poor, the prepared graphene has small size and great uncertainty, and meanwhile, the efficiency is low, the cost is high, and the method is not suitable for large-scale production.
Secondly, epitaxial growth method: good quality, low yield and high cost.
Thirdly, a graphite oxide reduction method: the prepared single layer rate is small, the single layer rate is easy to agglomerate, the conductivity and the specific surface area of the graphene are reduced, the application of the graphene in photoelectric equipment is further influenced, and in addition, crystal structure defects of the graphene, such as loss of carbon atoms on a carbon ring, serious pollution of production emission and the like, are easily caused in the oxidation-reduction process.
Fourthly, chemical vapor deposition CVD method: the evolution of the second method can be only carried out at lower temperature, so that the energy consumption in the manufacturing process can be reduced, and the graphene and the substrate can be separated by a metal chemical corrosion method and a device, so that the subsequent processing treatment of the graphene is facilitated. But the yield is small and the post-treatment also produces a large amount of contamination.
Fifthly, substance intercalation stripping method: typically, supercritical carbon dioxide intercalation can be added with ultrasonic micro-explosion, large-scale production can be realized, the single-layer rate is the highest except the CVD method, and the single-layer rate exceeds 8 percent. However, since the natural material has a portion of the monolayer overlapped with the other layer closed, the external common substances cannot enter the natural material, and the increase of the monolayer rate is not facilitated by increasing the pressure or other conventional methods.
Based on the above defects in the prior art, the industrialization of the two-dimensional material is a world-level problem which needs to be solved urgently.
Disclosure of Invention
In order to solve the technical problem, the invention provides a manufacturing method of a two-dimensional material. The invention has the advantages of continuous production, high single-layer rate, low cost, large-scale production and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of manufacturing a two-dimensional material, comprising the steps of:
(1) ionizing the intercalation gas:
putting a raw material for manufacturing a two-dimensional material with a certain mole number into a reaction kettle, enabling the raw material to be in contact with an electrode plate connected with a negative electrode of a direct-current power supply, vacuumizing the reaction kettle, introducing intercalation gas to enable the pressure in the kettle to reach a certain pressure, then opening a plasma generator, ionizing the intercalation gas, and closing the plasma generator after ionizing for a period of time; then turning on a direct current power supply of the electrode plate, keeping for a certain time to convert positive ions between single-layer substances into gas molecules after capturing electrons, and then stopping direct current discharge; obtaining a two-dimensional material precursor;
(2) ultrasonic stripping:
introducing a dispersion liquid containing a separant into a reaction kettle at a pressure higher than the air pressure in the kettle, replacing intercalation gas in the reaction kettle, starting ultrasonic equipment, carrying out ultrasonic stripping treatment on the two-dimensional material precursor and heating at the same time, keeping for a certain time, closing the ultrasonic equipment, and finishing the ultrasonic stripping treatment;
optionally, after the step (2), performing a step (3) of decomposition under heating and pressure:
decomposing the substances in the reaction kettle subjected to ultrasonic stripping in the step (2) at a certain temperature and pressure, wherein the temperature and pressure can decompose the precursor of the two-dimensional material to obtain the two-dimensional material, and then vacuumizing to remove the solvent to obtain a concentrated mixture of the separant and the two-dimensional material, namely slurry;
optionally, after step (3), further performing step (4) and repeating steps (1) to (3):
and (4) testing the products stripped in the steps (1) to (3), and if the requirements such as the size of the two-dimensional material are not met, repeating the steps (1) to (3) until the products meet the requirements such as the size of the two-dimensional material.
(5) And sequentially carrying out water washing, purification and drying on the mixture to obtain the two-dimensional material.
The invention starts the cold plasma generator to ionize the intercalation gas in the reaction kettle into plasma, for example, hydrogen can be used as the intercalation gas, the diameter of the ionized ion of hydrogen is very small, and the diameter is 1.6 multiplied by 10-6nm, the nano-particles can be very easily permeated into microscopic single-layer substance gaps of all the manufacturing raw materials of the current two-dimensional materials and even molecules of most substances, and then low-voltage direct current is introduced and kept for a certain time, so that ions of gas become atoms after capturing electrons, and the atoms can be combined into gas, and thus the intercalation gas is between the microscopic single-layer substances of the materials to be processed; then pumping solution containing the separant under a larger pressure, and displacing the intercalation gas outside the pores of the microscopic single-layer substances through a filter screen device, wherein the intercalation gas in the material to be treated is not easy to displace due to the damping effect of micro channels between the microscopic single-layer substances; starting an ultrasonic device, wherein ultrasonic waves with certain frequency have strong cavitation effect, so that intercalation gas between microscopic single-layer substances generates instant expansion, once van der Waals force between the single-layer substances is overcome, the single-layer substances can be stripped to obtain dispersion or slurry of the two-dimensional material with the release agent on the surface, and then carrying out post-treatment such as water washing, drying and the like on the product according to requirements. It should be noted that: some ions, such as hydrogen ions, will react with some raw materials after capturing electrons and becoming atoms, and it is necessary to further obtain the target by heating, such as graphite which can react with hydrogen atoms at room temperature, according to the present inventionThe method produces the primary product of the graphene, but if the graphene is heated to be above the decomposition temperature of the graphene and is kept for a corresponding time, the graphene is thoroughly decomposed into graphene and hydrogen, and the final product graphene is prepared.
Further, the raw material for manufacturing the two-dimensional material comprises one or more of graphite, molybdenum disulfide, boron nitride, transition metal chalcogenides, metal halides, layered metal oxides, layered bimetallic oxides, transition metal oxyhalides, layered alpha and gamma zirconium phosphates and phosphates, clays, ternary transition metal nitrides and carbides, preferably graphite. The transition metal chalcogenide is WSe2、ZnPS3Or Sb2Se3(ii) a The metal halide is PbI2、MgBr2Or CrCl3(ii) a The layered metal oxide is MnO2、WO3Or LaNb2O7(ii) a The layered double metal oxide is Mg6Al2(OH)16(ii) a The oxide is perovskite, niobate, rutile or Sr2RuO4(ii) a The transition metal oxyhalide is VOCl or WO2Cl2Or FeOCl; the clay is montmorillonite, mica, vermiculite black mica, phlogopite and fluorophlogopite; the carbide is Ti3C2。
Further, the plasma generator comprises a direct current or pulse discharge plasma generator, an alternating current or alternating discharge plasma generator or a high frequency induction discharge plasma generator, the direct current or pulse power supply: the voltage is 0.01-900 KV, and the current is 0.01-50A; the voltage of an alternating current or alternating current power supply is 0.01-900 KV, the current is 0.01-50A, and the frequency is 1-300 KHZ; the frequency of the induction power supply is 1-90 MHZ.
Preferably, the plasma generator is an alternating current discharge plasma generator, the voltage of a power supply is 800KV, the frequency is 200KHZ, and the current is 5A.
Further, the pressure of the reaction kettle in the step (1) is 1-1000 Pa after vacuum pumping; the pressure after the intercalation gas is introduced is 0.11-100 MPa, and the time for ionizing the intercalation gas is 0.01-12 hours.
Preferably, the relative vacuum degree of the reaction kettle in the step (1) is 10Pa after the reaction kettle is vacuumized; the pressure after the intercalation gas is introduced is 7MPa, the voltage is 10-100KV, and the reaction time is 4 hours.
Further, the intercalation gas in step (1) may include carbon dioxide, nitrogen, hydrogen, helium, neon, or argon.
Preferably, the intercalation gas is hydrogen.
Further, the molar ratio of the intercalation gas to the manufacturing raw materials is 1-10000: 1.
Further, in the step (1), the direct current voltage is 0.11-1000V, the current is 0.01-2A, and the direct current discharge time is 0.01-18 hours.
Preferably, in the step (1), the direct current voltage is 4V, the current is 0.1A, and the direct current discharge time is 8 hours.
Further, the dispersion liquid containing the separant with the mass concentration of 0.01-19% is pumped into the reaction kettle at a pressure higher than the air pressure in the kettle, and the molar ratio of the dispersion liquid to the raw materials for manufacturing the two-dimensional material is 0.5-900: 1.
Preferably, the mass concentration of the isolating agent dispersion liquid is 0.3%, and the isolating agent dispersion liquid is pumped into the reaction kettle at the pressure of 8 MPa.
Further, the release agent in the step (2) comprises one or more of linear alkyl benzene sodium sulfonate (LAS), fatty alcohol polyoxyethylene ether sodium sulfate (AES), fatty alcohol polyoxyethylene ether ammonium sulfate (AESA), sodium lauryl sulfate (K12 or SDS), lauroyl glutamic acid, nonylphenol polyoxyethylene ether (TX-10), peregal, diethanol amide (6501) stearic acid monoglyceride, lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate (petroleum sulfonate), dispersing agent NNO, dispersing agent MF, alkyl polyether (PO-EO copolymer), and fatty alcohol polyoxyethylene ether (AEO-3).
Preferably, the release agent in step (2) is monoethanolamine.
Further, the solvent of the separator dispersion comprises one or more of water, molten oxides, molten sulfides, molten salts, or organic solvents.
Preferably, the solvent is water.
Further, in the step (2), the ultrasonic frequency is 1-30 KHz, the power is 2-400 KW, the heating temperature is room temperature-180 ℃, and the reaction time is 0.11-30 hours.
Preferably, the ultrasonic frequency in the step (2) is 20KHz, the power is 3KW, and the heating temperature is 90 ℃ at room temperature.
Further, the temperature of the step (3) is room temperature-900 ℃, the pressure is 0.101-90 MPa, the reaction time is 0.11-12 hours, and the vacuumizing pressure is 0-1000 Pa.
Preferably, the temperature of the step (3) is 105 ℃, the pressure is 90MPa, the reaction time is 8 hours, and the vacuumizing pressure is 10 Pa.
Further, the drying temperature of the step (4) is between room temperature and 1500 DEG C
The invention has the following technical characteristics:
1) the invention is suitable for the large-batch continuous production of two-dimensional materials, and has the advantages of wide application range, simple operation and low cost.
2) The two-dimensional material prepared by the method has high purity, high single-layer rate and few defects.
Drawings
Fig. 1 is a transmission electron micrograph of graphene, the product of example 2.
Fig. 2 is a raman spectrum of graphene which is a product of example 2.
Detailed Description
The following specific examples are further illustrative of the methods and techniques provided by the present invention and should not be construed as limiting the invention thereto.
Example 1
The method for producing the graphene comprises the following steps:
(a) after 120 g of natural crystalline flake graphite is put into a reaction kettle, closing each valve, sealing equipment, and starting a vacuum pump to vacuumize the reaction kettle to 8 Pa;
(b) taking hydrogen as intercalation gas, opening a gas supply valve until the pressure of the hydrogen in the reaction kettle is 4MPa, and closing the gas supply valve;
(c) starting a plasma generator, wherein the time for plasma treatment of the material is 3 hours, so that ions are inserted into micro gaps of the microscopic single-layer substance, and then closing the plasma generator;
(d) starting a low-voltage direct-current power supply and keeping for a certain time, contacting the negative electrode of direct current with the material to be treated, keeping the voltage of the direct current at 15V for 2 hours to ensure that ions of hydrogen become atoms after obtaining electrons, the atoms can be combined into gas, and then closing the direct-current power supply;
(e) pumping water added with 0.9% of monoethanolamine into a reaction kettle at the pressure of 5MPa, completely replacing hydrogen out of the reaction kettle through a filtering device, so that the hydrogen is between micro single-layer substances, starting an ultrasonic device, wherein the frequency of ultrasonic waves is 20KHz, the power is 3KW, heating is carried out simultaneously, the temperature is 50 ℃, the holding time is 3 hours, then closing a valve and releasing intercalation gas to normal pressure, so that the single layers of raw materials are completely stripped and dispersed in aqueous solution added with monoethanolamine, and the two-dimensional material mixed dispersion liquid or slurry with the separant on the surface and difficult to agglomerate is obtained;
(f) heating to the boiling temperature of water above 100 ℃, and keeping for 1 hour; vacuumizing to remove water, wherein the vacuum pressure is 200Pa, and concentrating the product to obtain the mixed slurry of the graphite with the release agent on the surface and difficult to agglomerate and the release agent;
(g) and washing and drying the product according to the requirement, wherein the drying temperature is 179-220 ℃, evaporating and purifying to obtain a pure two-dimensional material, and packaging and leaving a factory.
Example 2
The graphene manufacturing method comprises the following steps:
(a) after 130 g of natural crystalline flake graphite is put into a reaction kettle, closing each valve, sealing equipment, and starting a vacuum pump to vacuumize the reaction kettle to 10 Pa;
(b) taking hydrogen as intercalation gas, opening a gas supply valve until the pressure of the hydrogen in the reaction kettle is 7MPa, and closing the gas supply valve;
(c) starting a plasma generator, wherein the time for plasma treatment of the material is 2 hours, so that ions are inserted into micro gaps of the microscopic single-layer substance, and then closing the plasma generator;
(d) starting a low-voltage direct-current power supply and keeping for a certain time, wherein the negative electrode of direct current is in contact with the material to be treated, the voltage of the direct current is 10V, and the direct current is kept for 1 hour, so that ions of hydrogen become atoms after obtaining electrons, and the atoms can be combined into gas to close the direct-current power supply;
(e) pumping glycerol added with 0.5% of monoethanolamine into a reaction kettle at the pressure of 8MPa, completely replacing hydrogen out of the reaction kettle through a filtering device, so that the hydrogen is between micro single-layer substances, starting an ultrasonic device, wherein the frequency of ultrasonic waves is 30KHz, the power is 4KW, heating is carried out simultaneously, the temperature is 90 ℃, the holding time is 2 hours, then closing a valve and releasing intercalation gas to normal pressure, so that the single layers of raw materials are completely stripped and dispersed in the glycerol solution added with monoethanolamine, and the two-dimensional material mixed dispersion liquid or slurry with the separant on the surface and difficult to agglomerate is obtained;
(f) heating and pressurizing to the decomposition temperature of the graphite alkane of more than 455 ℃, keeping for 12 hours, and keeping the maximum pressure of 90 MPa; closing the valve, releasing the intercalation gas, vacuumizing at the vacuum pressure of 200Pa, removing and recycling the solvent, and concentrating the product to obtain the graphene and separant mixed slurry with the separant on the surface and difficult to agglomerate;
(g) and washing and drying the product according to the requirement, wherein the drying temperature is 178-210 ℃, evaporating and purifying to obtain a pure two-dimensional material, and packaging and leaving a factory. The transmission electron micrograph and the raman spectrogram of the product graphene are shown in fig. 1 and fig. 2.
Example 3
The manufacturing method of the two-dimensional molybdenum disulfide comprises the following steps:
(a) after 120 g of molybdenum disulfide raw material is put into a reaction kettle, closing each valve, sealing equipment, and starting a vacuum pump to vacuumize the reaction kettle to 16 Pa;
(b) taking hydrogen as intercalation gas, opening a gas supply valve until the pressure of the hydrogen in the reaction kettle is 6MPa, and closing the gas supply valve;
(c) starting a plasma generator, wherein the time for plasma treatment of the material is 7 hours, so that ions are inserted into micro gaps of the microscopic single-layer substance, and then closing the plasma generator;
(d) starting a low-voltage direct-current power supply and keeping for a certain time, contacting the negative electrode of direct current with the material to be processed, keeping the voltage of the direct current at 15V for 2 hours, so that the ions of hydrogen capture electrons and become atoms, and the atoms can be combined into gas to close the direct-current power supply;
(e) pumping an aqueous solution added with 0.2 percent of monoethanolamine into a reaction kettle at the pressure of 7MPa, completely replacing hydrogen out of the reaction kettle through a filtering device, so that the hydrogen is between micro single-layer substances, starting an ultrasonic device, wherein the frequency of ultrasonic waves is 25KHz, the power is 1KW, heating is carried out simultaneously, the temperature is 70 ℃, the holding time is 6 hours, then closing a valve and releasing intercalation gas to normal pressure, so that the single layers of raw materials are completely stripped and dispersed in the aqueous solution added with monoethanolamine, and the two-dimensional material mixed dispersion liquid or slurry with the separant on the surface and difficult to agglomerate is obtained;
(f) heating to a temperature of more than 105 ℃, keeping for 1 hour, then vacuumizing to remove water, wherein the vacuum pressure is 200Pa, and concentrating the product to obtain the molybdenum disulfide and separant mixed slurry with the separant on the surface and difficult to agglomerate;
(g) and washing and drying the product according to the requirement, wherein the drying temperature is 175-213 ℃, evaporating and purifying to obtain a pure two-dimensional material, and packaging and leaving a factory.
Example 4
The manufacturing method of the two-dimensional hexagonal boron nitride comprises the following steps:
(a) after 400 g of hexagonal boron nitride raw material is put into a reaction kettle, closing each valve, sealing equipment, and starting a vacuum pump to vacuumize the reaction kettle to 19 Pa;
(b) taking hydrogen as intercalation gas, opening a gas supply valve until the pressure of the hydrogen in the reaction kettle is 4MPa, and closing the gas supply valve;
(c) starting a plasma generator, wherein the time for plasma treatment of the material is 7 hours, so that ions are inserted into micro gaps of the microscopic single-layer substance, and then closing the plasma generator;
(d) starting a low-voltage direct-current power supply and keeping for a certain time, contacting the negative electrode of direct current with the material to be processed, keeping the voltage of the direct current at 6V for 3 hours, so that ions of the intercalation gas become atoms after capturing electrons, and the atoms can be combined into gas to close the direct-current power supply;
(e) pumping an aqueous solution added with 0.3 percent of monoethanolamine into a reaction kettle at the pressure of 5MPa, completely replacing hydrogen out of the reaction kettle through a filtering device, so that the hydrogen is between micro single-layer substances, starting an ultrasonic device, wherein the frequency of ultrasonic waves is 18KHz, the power is 5KW, heating is carried out simultaneously, the temperature is 80 ℃, the holding time is 4 hours, then closing a valve and releasing intercalation gas to normal pressure, so that the single layers of raw materials are completely stripped and dispersed in the aqueous solution added with the monoethanolamine, and the two-dimensional material hexagonal boron nitride mixed dispersion liquid or slurry which has a separant monoethanolamine on the surface and is not easy to agglomerate is obtained;
(f) heating to the boiling temperature of water above 100 ℃, and keeping for 1 hour; vacuumizing to remove water, wherein the vacuum pressure is 200Pa, and concentrating the product to obtain the mixed slurry of the hexagonal boron nitride and the separant, the surface of which is provided with the separant and is not easy to agglomerate;
(g) and washing and drying the product according to the requirement, wherein the drying temperature is 176-206 ℃, evaporating and purifying to obtain a pure two-dimensional material, and packaging and leaving a factory.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core ideas. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A method of manufacturing a two-dimensional material, comprising the steps of:
(1) ionizing the intercalation gas:
putting a raw material for manufacturing a two-dimensional material with a certain mole number into a reaction kettle, enabling the raw material to be in contact with an electrode plate connected with a negative electrode of a direct-current power supply, vacuumizing the reaction kettle, introducing intercalation gas to enable the pressure in the kettle to reach a certain pressure, then opening a plasma generator, ionizing the intercalation gas, and closing the plasma generator after ionizing for a period of time; then, turning on a direct current power supply of the electrode plate to discharge, keeping for a certain time to convert positive ions between single-layer substances into gas molecules after capturing electrons, and then stopping discharging; obtaining a two-dimensional material precursor;
in the step (1), the direct current voltage is 0.11-1000V, the current is 0.01-2A, and the direct current discharge time is 0.01-18 hours;
(2) ultrasonic stripping:
introducing a dispersion liquid containing a separant into a reaction kettle at a pressure higher than the air pressure in the kettle, replacing intercalation gas in the reaction kettle, starting ultrasonic equipment, carrying out ultrasonic stripping treatment on the two-dimensional material precursor and heating at the same time, keeping for a certain time, closing the ultrasonic equipment, and finishing the ultrasonic stripping treatment;
and (3) heating and pressurizing decomposition:
decomposing the substances in the reaction kettle subjected to ultrasonic stripping in the step (2) at a certain temperature and pressure, wherein the temperature and pressure can decompose the precursor of the two-dimensional material to obtain the two-dimensional material, and then vacuumizing to remove the solvent to obtain a concentrated mixture of the separant and the two-dimensional material, namely slurry;
and (4) repeating the steps (1) - (3):
testing the products stripped in the steps (1) to (3), and if the size requirement of the two-dimensional material is not met, repeating the steps (1) to (3) until the products meet the size requirement of the two-dimensional material;
(5) and sequentially carrying out water washing, purification and drying on the mixture to obtain the two-dimensional material.
2. A two-dimensional material according to claim 1The manufacturing method is characterized in that the manufacturing raw material of the two-dimensional material comprises one or more of graphite, molybdenum disulfide, boron nitride, transition metal chalcogenide, metal halide, layered metal oxide, layered double metal oxide, transition metal oxyhalide and clay; the layered metal oxide is MnO2、WO3Or LaNb2O7(ii) a The layered double metal oxide is Mg6Al2(OH)16(ii) a The oxide is perovskite, niobate, rutile or Sr2RuO4。
3. The method for manufacturing the two-dimensional material according to claim 1, wherein the pressure of the reaction kettle in the step (1) is 1-1000 Pa after vacuum pumping; the pressure after the intercalation gas is introduced is 0.11-100 MPa, and the time for ionizing the intercalation gas is 0.01-12 hours.
4. The method of claim 1, wherein the intercalation gas of step (1) comprises one or more of carbon dioxide, nitrogen, hydrogen, helium, neon, or argon.
5. The method according to claim 1, wherein in the step (2), the dispersion containing the release agent at a mass concentration of 0.01 to 19% is pumped into the reaction vessel at a pressure higher than the pressure in the reaction vessel, and the molar ratio of the dispersion to the raw materials for producing the two-dimensional material is 0.5 to 900: 1.
6. The method according to claim 1, wherein the release agent in step (2) comprises one or more of linear alkylbenzene sulfonate, fatty alcohol-polyoxyethylene ether sodium sulfate, fatty alcohol-polyoxyethylene ether ammonium sulfate, sodium lauryl sulfate, lauroyl glutamic acid, nonylphenol polyoxyethylene ether, peregal, lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate, NNO, MF, alkyl polyether, and fatty alcohol-polyoxyethylene ether.
7. The method for manufacturing a two-dimensional material according to claim 1, wherein in the step (2), the ultrasonic frequency is 1 to 30KHz, the power is 2 to 400KW, the heating temperature is between room temperature and 180 ℃, and the reaction time is 0.11 to 30 hours.
8. The method for manufacturing a two-dimensional material according to claim 1, wherein the temperature in the step (3) is between room temperature and 900 ℃, the pressure is between 0.101 and 90MPa, the reaction time is between 0.11 and 12 hours, and the vacuum pressure is between 0 and 1000 Pa.
9. A method for manufacturing a two-dimensional material according to claim 1, wherein the plasma generator of step (1) comprises a dc or pulsed discharge plasma generator, an ac or alternating discharge plasma generator or a high frequency induction discharge plasma generator, and the dc or pulsed power supply comprises: the voltage is 0.01-900 KV, and the current is 0.01-50A; the voltage of an alternating current or alternating current power supply is 0.01-900 KV, the current is 0.01-50A, and the frequency is 1-300 KHZ; the frequency of the induction power supply is 1-90 MHZ.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2018108241729 | 2018-07-25 | ||
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