CN111960412B - Nanocarbon material and preparation method thereof - Google Patents
Nanocarbon material and preparation method thereof Download PDFInfo
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- CN111960412B CN111960412B CN202010931799.1A CN202010931799A CN111960412B CN 111960412 B CN111960412 B CN 111960412B CN 202010931799 A CN202010931799 A CN 202010931799A CN 111960412 B CN111960412 B CN 111960412B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a nano carbon material, which comprises raw material crystalline flake graphite; the preparation method comprises the following steps: s1: grinding the raw material flake graphite by using grinding equipment, wherein the rotating speed of the grinding equipment is set to 3000-4000r/min, and the temperature inside the grinding equipment is set to 25-30 ℃ to obtain particles with uniform size; s2: soaking the particles in the step S1 in a mixed solution of aromatic hydrocarbon, alcohol and ether for 30-60min, and performing super-temperature drying on the soaked particles in drying equipment at 800-900 ℃ to obtain soaked particles. The nano carbon material prepared by the invention has uniform size and uniform dispersion, is different from common nano carbon materials, has a partial graphene structure and a certain lamellar structure, but has weak bonding between lamellar layers, has apparent density larger than that of common nano carbon materials, is convenient for storage and transportation, and is easy for polymer compounding.
Description
Technical Field
The invention relates to the technical field of nano carbon material preparation, in particular to a nano carbon material and a preparation method thereof.
Background
Carbon has various electron orbital characteristics and sp2 anisotropy, and carbon materials using the same as the only constituent element have various forms and properties. The nano carbon material is widely applied as a common carbon material based on various performance advantages, and the traditional preparation method is mostly a chemical method and an electrochemical method, but the steps are more complicated, and the obtained product is easy to agglomerate, unstable in performance, uneven in particle size distribution, high in collection difficulty and the like. The plasma technology is used for preparing the nano carbon material with the characteristics of high efficiency, simplicity, low pollution and the like, and specific products can be produced or surface modification can be carried out by changing the plasma atmosphere and related technological parameters. For example using plasma treatment or production of nanoparticles: CNTs or graphene. Meanwhile, due to the agglomeration phenomenon of the nano material, the abrasion resistance, lubricity, electric conduction and heat conduction performance of the composite material are improved to a limited extent in actual use, and meanwhile, due to the fact that most of nano carbon materials are powder products at present, dust problems caused in the subsequent storage, transportation and use processes are easy to cause health and potential safety hazards, so that the nano carbon material and the preparation method thereof are provided.
Disclosure of Invention
Based on the problems existing in the prior art, the invention provides a nano carbon material and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a nano carbon material comprises raw material crystalline flake graphite;
the preparation method comprises the following steps:
s1: grinding the raw material flake graphite by using grinding equipment, wherein the rotating speed of the grinding equipment is set to 3000-4000r/min, and the temperature inside the grinding equipment is set to 25-30 ℃ to obtain particles with uniform size;
s2: soaking the particles in the step S1 in a mixed solution of aromatic hydrocarbon, alcohol and ether for 30-60min, and performing super-temperature drying on the soaked particles in drying equipment at 800-900 ℃ to obtain soaked particles;
s3: uniformly dispersing and spreading the soaked particles in the amount of 0.4-0.6g S2 on a sample stage, and then placing the sample stage with the soaked particles spread in a plasma reactor;
s4: vacuumizing the plasma reactor in the step S3 to enable the pressure in the plasma reactor to reach 20-50Pa, starting a plasma emission device in the plasma reactor, and adjusting the amplification power to 50-2000W;
s5: introducing reaction gas into the plasma reactor in the step S4, so that the total pressure in the plasma reactor is set to be 80-500Pa, and the reaction time of the reaction gas is set to be 1-120min;
s6: and (4) closing the plasma emission device in the step (S4), and then introducing nitrogen and inert gas into the plasma reactor to achieve the aim of stopping the reaction, thereby obtaining the nano carbon material.
Preferably, in the step S1, the particle size is 10-150 mesh.
Preferably, in S3, the specification of the sample stage is 300mm×300mm.
Preferably, in S3, the plasma reactor is a low-pressure glow discharge plasma reactor.
Preferably, in the step S5, the flow rate of the reaction gas is controlled by a gas control valve, and the reaction gas is oxygen, hydrogen, nitrogen, hydrocarbon compounds, inert gas, or a mixture of the above gases.
Compared with the prior art, the nano carbon material prepared by the invention has uniform size and uniform dispersion, is different from common nano carbon materials, has a part of graphene structure and a certain lamellar structure, but has weak bonding between lamellar layers, has apparent density larger than that of common nano carbon materials, is convenient for storage and transportation, and is easy for polymer compounding.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments.
Example 1
The embodiment provides a nano carbon material, which comprises raw material crystalline flake graphite;
the preparation method comprises the following steps:
s1: grinding the raw material flake graphite by using grinding equipment, wherein the rotating speed of the grinding equipment is set to 3000r/min, and the temperature inside the grinding equipment is set to 25 ℃ to obtain particles with uniform size, and the size of the particles is 10-150 meshes;
s2: soaking the particles in the step S1 in a mixed solution of aromatic hydrocarbon, alcohol and ether for 30min, and performing super-temperature drying on the soaked particles in drying equipment at 800 ℃ to obtain soaked particles;
s3: uniformly dispersing and flatly spreading the soaked particles in the amount of 0.4g S2 on a sample table with the specification of 300mm, and then placing the sample table flatly spread with the soaked particles into a plasma reactor, wherein the plasma reactor is a low-pressure glow discharge plasma reactor;
s4: vacuumizing the plasma reactor in the step S3 to enable the pressure in the plasma reactor to reach 20Pa, starting a plasma emission device in the plasma reactor, and adjusting the amplification power to 50W;
s5: introducing reaction gas into the plasma reactor in the step S4, wherein the flow rate of the reaction gas is controlled by a gas control valve, and the reaction gas is mixed gas of oxygen, hydrogen, nitrogen, hydrocarbon compounds, inert gas and the above gases, so that the total pressure in the plasma reactor is set to be 80-Pa, and the reaction time of the reaction gas is set to be 1min;
s6: and (4) closing the plasma emission device in the step (S4), and then introducing nitrogen and inert gas into the plasma reactor to achieve the aim of stopping the reaction, thereby obtaining the nano carbon material.
Example two
The embodiment provides a nano carbon material, which comprises raw material crystalline flake graphite;
the preparation method comprises the following steps:
s1: grinding raw material flake graphite by using grinding equipment, wherein the rotating speed of the grinding equipment is 3500r/min, the temperature inside the grinding equipment is 27 ℃, and particles with uniform size are obtained, and the size of the particles is 10-150 meshes;
s2: soaking the particles in the step S1 in a mixed solution of aromatic hydrocarbon, alcohol and ether for 45min, and performing super-temperature drying on the soaked particles in a drying device at 850 ℃ to obtain soaked particles;
s3: uniformly dispersing and flatly spreading the soaked particles in the amount of 0.5g S2 on a sample table with the specification of 300mm, and then placing the sample table flatly spread with the soaked particles into a plasma reactor, wherein the plasma reactor is a low-pressure glow discharge plasma reactor;
s4: vacuumizing the plasma reactor in the step S3 to enable the pressure in the plasma reactor to reach 35Pa, starting a plasma emission device in the plasma reactor, and adjusting the amplification power to 1025W;
s5: introducing reaction gas into the plasma reactor in the step S4, wherein the flow rate of the reaction gas is controlled by a gas control valve, and the reaction gas is mixed gas of oxygen, hydrogen, nitrogen, hydrocarbon compounds, inert gas and the above gases, so that the total pressure in the plasma reactor is set to be 290Pa, and the reaction time of the reaction gas is set to be 60min;
s6: and (4) closing the plasma emission device in the step (S4), and then introducing nitrogen and inert gas into the plasma reactor to achieve the aim of stopping the reaction, thereby obtaining the nano carbon material.
Example III
The embodiment provides a nano carbon material, which comprises raw material crystalline flake graphite;
the preparation method comprises the following steps:
s1: grinding the raw material flake graphite by using grinding equipment, wherein the rotating speed of the grinding equipment is set to 4000r/min, and the temperature inside the grinding equipment is set to 30 ℃ to obtain particles with uniform size, and the size of the particles is 150 meshes;
s2: soaking the particles in the step S1 in a mixed solution of aromatic hydrocarbon, alcohol and ether for 60min, and performing super-temperature drying on the soaked particles in a drying device at 900 ℃ to obtain soaked particles;
s3: uniformly dispersing and flatly spreading the soaked particles in the amount of 0.6g S2 on a sample table with the specification of 300mm, and then placing the sample table flatly spread with the soaked particles into a plasma reactor, wherein the plasma reactor is a low-pressure glow discharge plasma reactor;
s4: vacuumizing the plasma reactor in the step S3 to enable the pressure in the plasma reactor to reach 50Pa, starting a plasma emission device in the plasma reactor, and adjusting the amplification power to 2000W;
s5: introducing reaction gas into the plasma reactor in the step S4, wherein the flow rate of the reaction gas is controlled by a gas control valve, and the reaction gas is mixed gas of oxygen, hydrogen, nitrogen, hydrocarbon compounds, inert gas and the above gases, so that the total pressure in the plasma reactor is set to be 500Pa, and the reaction time of the reaction gas is set to be 120min;
s6: and (4) closing the plasma emission device in the step (S4), and then introducing nitrogen and inert gas into the plasma reactor to achieve the aim of stopping the reaction, thereby obtaining the nano carbon material.
The nano carbon material prepared by the first to third embodiments has uniform size and uniform dispersion, and is different from the common nano carbon material, the material has a partial graphene structure and a certain lamellar structure, but weak bonding is arranged between lamellar layers, the apparent density is greater than that of the common nano carbon material, the storage and transportation are convenient, and the polymer is easy to compound, wherein the second embodiment is the best embodiment.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. The nano carbon material is characterized by comprising raw material crystalline flake graphite;
the preparation method comprises the following steps:
s1: grinding the raw material flake graphite by using grinding equipment, wherein the rotating speed of the grinding equipment is set to 3000-4000r/min, and the temperature inside the grinding equipment is set to 25-30 ℃ to obtain particles with uniform size;
s2: soaking the particles in the step S1 in a mixed solution of aromatic hydrocarbon, alcohol and ether for 30-60min, and performing super-temperature drying on the soaked particles in drying equipment at 800-900 ℃ to obtain soaked particles;
s3: uniformly dispersing and spreading the soaked particles in the amount of 0.4-0.6g S2 on a sample stage, and then placing the sample stage with the soaked particles spread in a plasma reactor;
s4: vacuumizing the plasma reactor in the step S3 to enable the pressure in the plasma reactor to reach 20-50Pa, starting a plasma emission device in the plasma reactor, and adjusting the amplification power to 50-2000W;
s5: introducing reaction gas into the plasma reactor in the step S4, so that the total pressure in the plasma reactor is set to be 80-500Pa, and the reaction time of the reaction gas is set to be 1-120min;
s6: and (4) closing the plasma emission device in the step (S4), and then introducing nitrogen and inert gas into the plasma reactor to achieve the aim of stopping the reaction, thereby obtaining the nano carbon material.
2. The nanocarbon material according to claim 1, wherein the size of the particles in S1 is 10 to 150 mesh.
3. The nanocarbon material according to claim 1, wherein in S3, the sample stage has a specification of 300mm by 300mm.
4. The nanocarbon material according to claim 1, wherein in S3, the plasma reactor is a low-pressure glow discharge plasma reactor.
5. The nanocarbon material according to claim 1, wherein in S5, the flow rate of the reaction gas is controlled by a gas control valve, and the reaction gas is a mixture of oxygen, hydrogen, nitrogen, hydrocarbon compounds, inert gas and the above.
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