CN110996412B - Carbon crystal electric heating film and preparation method and application thereof - Google Patents
Carbon crystal electric heating film and preparation method and application thereof Download PDFInfo
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- CN110996412B CN110996412B CN201911307092.7A CN201911307092A CN110996412B CN 110996412 B CN110996412 B CN 110996412B CN 201911307092 A CN201911307092 A CN 201911307092A CN 110996412 B CN110996412 B CN 110996412B
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Abstract
The invention provides a preparation method of a carbon crystal electric heating film, which comprises the following steps: (1) mixing the carbon crystal microsphere powder with a solvent, and uniformly mixing under 100-400W ultrasound; (2) mixing a thermoplastic high polymer material with the mixture obtained in the step (1), and uniformly mixing under 100-400W ultrasound; (3) drying the mixture obtained in the step (2) in vacuum at 45-55 ℃ and-0.15-0.05 MPa until the solvent is completely removed; (4) heating the material obtained in the step (3) to 50-200 ℃, and preserving heat until the material is completely converted into a molten state; (5) hot-press molding the material obtained in the step (4) at 50-300 ℃ and 1-500 MPa for 0.5-1 h, and then cooling to 25 ℃; (6) and (5) pasting an insulating film and a copper electrode on the surface of the material obtained in the step (5), and pressing to obtain the carbon crystal electric heating film. The carbon crystal electric heating material prepared by the invention can further improve the infrared wave emission efficiency of nano carbon crystal electric heating products, control the wave band to be 0.8-4 um and realize long-distance heating.
Description
Technical Field
The invention belongs to the technical field of electric heating materials, and particularly relates to a carbon crystal electric heating film, and a preparation method and application thereof.
Background
At present, electric heating is one of the most environment-friendly heating modes. The electric heating equipment sold in the market mainly comprises an electric heater, a heating cable, an electric heating ceramic piece and the like, wherein the metal resistance wires of the electric heater and the heating cable have high density and high energy consumption, and the electric heating ceramic piece has slow temperature rise and large brittleness, so the electric heating equipment has defects.
With the attention paid to the environmental protection problem in the world, the environmental protection type electric heating product is a necessary trend facing the future development. Further, in accordance with the needs of life, production, and the like, not only the electric heating device is required to have excellent electric heating performance, but also excellent comprehensive properties such as wear resistance, corrosion resistance, aging resistance, and the like are required. In recent years, carbon-series electric heating products are widely concerned, and have the characteristics of energy conservation, environmental protection and uniform heating, but the infrared radiation of the existing carbon-series electric heating products is in middle and far infrared bands, the infrared energy of the existing carbon-series electric heating products is severely attenuated in the transmission process, and the remote heat supply cannot be realized.
The nano carbon crystal microsphere has the characteristics of resistance heating, Brownian motion heating, infrared ray emission and the like under the electrified condition, and can basically meet the development requirements of low-energy-consumption, environment-friendly and multifunctional electric heating products. Many of the carbon nanocrystallines in the market are prepared by taking a microcrystalline carbon material as a core heating material. The micro-crystalline carbon material obtained by the conventional ball-milling carbon crystal technology has low degree of particle size homogenization and poor particle size controllability, so that the nano-carbon crystal electric heating product has low electric heat conversion efficiency and high energy consumption, and cannot realize controllable change of a reflected infrared band, thereby causing loss of partial infrared energy.
The electric heating high molecular device has the advantages of light weight, energy conservation and easy processing, can well overcome the defects of the traditional electric heating equipment, has increasing requirements in life and industrial production, has low energy consumption and high electric heating efficiency as an important development trend, and realizes that the reduction of high conductivity and low energy consumption become a main development stream.
Disclosure of Invention
In view of the above problems, in order to further improve the electrothermal efficiency of the nano carbon crystal electrothermal product, reduce the heating energy consumption and realize remote heating, the invention arranges the nano-scale controllable carbon crystal microsphere powder (carbon crystal microsphere powder such as carbon fiber, carbon nano tube, graphite, graphene, polymer microsphere carbide and the like) into a photonic crystal structure by a melting shearing and hot press molding mode based on the coating layer polymer melting shearing principle, thereby realizing strong reflection of near infrared rays. The carbon crystal electric heating film obtained by the preparation method can obtain the nano carbon crystal infrared electric heating film with controllable wave bands by adopting the high polymer film for packaging, and well meets the development requirements of electric heating products with low energy consumption, environmental protection and multiple functions.
The technical scheme for realizing the purpose is as follows:
the invention provides a preparation method of a carbon crystal electric heating film, which comprises the following steps:
(1) mixing the carbon crystal microsphere powder with a solvent, and uniformly mixing under 100-400W ultrasound; wherein the grain diameter of the carbon crystal microsphere powder is 10 nm-100 mu m; the ratio of the mass of the carbon crystal microsphere powder to the volume of the solvent is (7-9) g (200-500) ml; the solvent is selected from acetone and/or ethanol;
(2) mixing a thermoplastic high polymer material with the mixture obtained in the step (1), and uniformly mixing under 100-400W ultrasound;
(3) drying the mixture obtained in the step (2) in vacuum at 45-55 ℃ and-0.15-0.05 MPa until the solvent is completely removed to obtain carbon crystal microsphere powder coated with the thermoplastic high polymer material;
(4) heating the carbon crystal microsphere powder coated with the thermoplastic high polymer material obtained in the step (3) to 50-200 ℃, and preserving heat until the carbon crystal microsphere powder coated with the thermoplastic high polymer material is completely converted into a molten state;
(5) hot-press molding the material obtained in the step (4) at 50-300 ℃ and 1-500 MPa for 0.5-1 h, and then cooling to 25 ℃;
(6) and (5) pasting an insulating film and a copper electrode on the surface of the material obtained in the step (5), and pressing to obtain the carbon crystal electric heating film.
In one embodiment, in the method for preparing a carbon crystal electrothermal film according to the present invention, the method for preparing the carbon crystal microsphere powder in the step (1) includes the following steps:
(1-1) mixing and mixing a carbon raw material and an organic solvent; wherein the ratio of the mass of the carbon raw material to the volume of the organic solvent is (7-9) g (200-500) ml; the organic solvent is selected from acetone and/or ethanol;
(1-2) mixing zirconia ball milling beads with the particle size of 0.01-1 mm with the mixture obtained in the step (1-1), then carrying out ball milling until the particle size of the carbon raw material is 10 nm-100 mu m and the particle size dispersity index is less than 0.2, and then carrying out vacuum drying at 45-55 ℃ and-0.15-0.05 MPa for 11-13 h to obtain carbon crystal microsphere powder with the particle size of 10 nm-100 mu m; wherein the mass ratio of the zirconia ball grinding beads to the carbon raw material is (150-350) g and (1-20) g;
optionally, the carbon crystal microsphere powder is selected from one or more of polystyrene microsphere carbide, organic glass microsphere carbide, polycarbonate microsphere carbide and polyacrylonitrile microsphere carbide.
In one embodiment, in the method for manufacturing a carbon crystal electrothermal film according to the present invention, in the step (1-1), the carbon raw material is selected from one or more of carbon fiber, carbon nanotube, graphite, and graphene.
In one embodiment, in the method for manufacturing a carbon crystal electrothermal film according to the present invention, the carbon raw material is carbon fiber T300.
In one embodiment, in the method for preparing a carbon crystal electrothermal film according to the present invention, in the step (1-2), the zirconia ball-milling beads have a particle size of 0.1 mm.
In one embodiment, in the preparation method of the carbon crystal electrothermal film, in the step (1), the thermoplastic polymer material is selected from one or more of polyethylacrylate, polyurethane, polystyrene, polycarbonate, epoxy resin E-44 and/or epoxy resin E-51.
In one embodiment, in the preparation method of the carbon crystal electrothermal film, in the step (2), the mass ratio of the thermoplastic polymer material to the carbon crystal microsphere powder in the step (1) is (1-2) g and (1-20) g.
In one embodiment, in the method for preparing a carbon crystal electrothermal film according to the present invention, the step (6) is: adhering an insulating film and a copper electrode on the surface of the material obtained in the step (5), and pressing at 1-100MPa and normal temperature for 10-20 min to obtain the carbon crystal electric heating film; wherein the insulating film is selected from one or more of epoxy resin film, PEEK film, PI film and PET film.
The invention also provides the carbon crystal electric heating film prepared by the preparation method of the carbon crystal electric heating film.
The invention also provides application of the carbon crystal electric heating film obtained by the preparation method of the carbon crystal electric heating film in preparation of a carbon crystal electric heating device.
Specifically, the invention provides a preparation method of a waveband-controllable nano carbon crystal electric heating film, which comprises the steps of preparing nano carbon crystal microsphere powder with the grain diameter of 10 nm-100 mu m and the grain size dispersion index of less than 0.2, and further preparing carbon crystal microsphere powder coated with a thermoplastic high polymer material to finally obtain the carbon crystal electric heating film. The infrared reflection band of the nano carbon crystal microsphere powder with the particle size of 10 nm-100 mu m is calculated based on the Bragg reflection law of the face-centered cubic photonic crystal material, the near infrared band which is not easy to lose in the infrared band range in the transmission process is regulated, and the electric heating efficiency of the carbon crystal electric heating film is further improved. The invention is based on the principle of cladding layer macromolecule melting and shearing, and arranges the carbon crystal microsphere powder (carbon crystal microsphere powder such as carbon fiber, carbon nano tube, graphite, graphene, macromolecule microsphere carbide and the like) with controllable nano scale into a photonic crystal structure by the modes of melting, shearing and hot press molding, thereby realizing the strong reflection of near infrared rays.
The carbon crystal electric heating film is a nano carbon system (such as carbon fiber, carbon nano tube, graphite, graphene, high molecular microsphere carbide and the like) infrared electric heating material which is based on a photonic crystal structure and can emit and reflect near infrared rays of 750-4000 nm. The infrared emitted by the traditional carbon series electric heating product is in a mid-infrared band of 8-15 microns, the infrared energy of the traditional carbon series electric heating product is attenuated more in the transmission process, and long-distance heat supply cannot be realized. The invention is based on the principle of cladding layer macromolecule melting and shearing, and arranges the carbon crystal microsphere powder (carbon crystal microsphere powder such as carbon fiber, carbon nano tube, graphite, graphene, macromolecule microsphere carbide and the like) with controllable nano scale into a photonic crystal structure by the modes of melting, shearing and hot press molding, thereby realizing the strong reflection of near infrared rays. The carbon crystal electric heating film prepared by the invention can generate a large amount of heat and infrared rays when being electrified, so that the temperature of surrounding objects can be quickly raised, and the low energy consumption and high efficiency of an electric heating device can be further realized by combining the strong reflection capability of the photonic crystal structure on the near infrared rays which are not easy to attenuate, and the long-distance heat supply is realized.
In the method, the obtained carbon crystal microsphere powder coated with the thermoplastic high polymer material is uniform, the stress of the carbon crystal microsphere powder coated with the thermoplastic high polymer material is symmetrical in the processing process, and the shape of the obtained carbon crystal electric heating material can be controlled in a molten state.
In the method, the carbon crystal microsphere powder and the thermoplastic polymer material (such as polyethylacrylate, polyurethane, polystyrene, polycarbonate, epoxy resin E-44 and/or epoxy resin E-51) have good dispersibility in organic solvents such as ethanol and acetone, and a uniform mixed solution of the two substances can be obtained by an ultrasonic treatment mode; particularly, the carbon crystal microsphere powder can be uniformly dispersed in the mixed solution of the thermoplastic polymer material and the organic solvent by ultrasonic treatment under the power of 100-400W; vacuum drying at 45-55 deg.C, -0.15-0.05 MPa can remove solvent, so that the thermoplastic polymer material is uniformly coated outside the carbon crystal microsphere powder to obtain good flowability at high temperature, and further to ensure the photonic crystal structure with ordered structure obtained during hot press forming.
The carbon crystal electric heating film prepared by the invention can obtain a nano carbon crystal infrared electric heating device with controllable wave band, low energy consumption, high efficiency and long-distance heat supply by sticking the conductive electrodes at the two ends of the carbon crystal electric heating film.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 shows an electron microscope image of the carbon crystal microsphere powder obtained by the preparation method of the invention;
FIG. 2 shows an electron microscope image of the carbon crystal microsphere powder coated with the thermoplastic polymer material obtained by the preparation method of the invention;
FIG. 3 shows an electron microscope image of a product obtained after a hot pressing step in the preparation method of the present invention;
fig. 4 shows a nano carbon crystal infrared electric heating device prepared by the preparation method of the invention.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
The experimental procedures in the following examples are conventional unless otherwise specified. The raw materials and reagent materials used in the following examples are all commercially available products unless otherwise specified.
Example 1: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Preparing carbon crystal microsphere powder:
(1-1) adding 7g of carbon fiber T300 to 200ml of ethanol, and mixing;
(1-2) adding 1050g of zirconia ball milling beads with the particle size of 0.1mm into the mixture obtained in the step (1-1) for ball milling until the particle size of the carbon fibers T300 is 10 nm-100 microns and the particle size dispersity index is less than 0.2, and then drying in vacuum at 45 ℃ and-0.15 MPa for 11 hours to obtain carbon crystal microsphere powder with the particle size of 10 nm-100 microns;
(2) adding 7g of carbon crystal microsphere powder obtained in the step (1) into 200ml of ethanol, and uniformly mixing under 400W ultrasound;
(3) adding 7g of polyethylacrylate into the mixture obtained in the step (2), and uniformly mixing under 400W ultrasound;
(4) drying the mixture obtained in the step (3) in vacuum at 45 ℃ and-0.15 MPa until ethanol is completely removed to obtain carbon crystal microsphere powder coated with the polyethylacrylate;
(5) heating conditions are obtained by subjecting the carbon crystal microsphere powder coated with the polyethylacrylate obtained in the step (4) to a thermogravimetric analysis experiment and a differential scanning calorimetry experiment, and the decomposition temperature, the glass transition temperature and the viscous flow conversion temperature of the carbon crystal microsphere powder coated with the polyethylacrylate are obtained, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the carbon crystal microsphere powder coated with the polyethylacrylate into a hot pressing die or rolling equipment, heating to 100 ℃, and preserving heat until the carbon crystal microsphere powder coated with the polyethylacrylate is completely converted into a molten state;
(6) hot-press molding the material obtained in the step (5) at 200 ℃ and 250MPa for 0.5h, and then cooling to 25 ℃;
(7) and (4) attaching an epoxy resin film and a copper electrode on the surface of the material obtained in the step (6), and pressing at 1MPa and normal temperature for 10min to obtain the carbon crystal electric heating film.
Example 2: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Preparing carbon crystal microsphere powder:
(1-1) adding 9g of the carbon nanotube material to 500ml of acetone, and mixing;
(1-2) adding 157.5g of zirconia ball milling beads with the particle size of 1mm into the mixture obtained in the step (1-1) for ball milling until the particle size of the carbon nanotube material is 10 nm-100 microns and the particle size dispersity index is less than 0.2, and then carrying out vacuum drying at 55 ℃ and-0.05 MPa for 13h to obtain carbon crystal microsphere powder with the particle size of 10 nm-100 microns;
(2) adding 9g of carbon crystal microsphere powder obtained in the step (1) into 500ml of acetone, and uniformly mixing under 400W ultrasound;
(3) adding 18g of polyurethane into the mixture obtained in the step (2), and uniformly mixing under 400W ultrasound;
(4) drying the mixture obtained in the step (3) in vacuum at 55 ℃ and-0.05 MPa until acetone is completely removed to obtain carbon crystal microsphere powder coated with polyurethane;
(5) heating conditions are obtained by subjecting the polyurethane-coated carbon crystal microsphere powder obtained in the step (4) to a thermogravimetric analysis experiment and a differential scanning calorimetry experiment, and the decomposition temperature, the glass transition temperature and the viscous flow conversion temperature of the polyurethane-coated carbon crystal microsphere powder are obtained, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the carbon crystal microsphere powder coated with the polyurethane in a hot pressing mold or rolling equipment, heating to 200 ℃, and preserving heat until the carbon crystal microsphere powder coated with the polyurethane is completely converted into a molten state;
(6) hot-press molding the material obtained in the step (5) at 300 ℃ and 500MPa for 1h, and then cooling to 25 ℃;
(7) and (4) pasting a PEEK film and a copper electrode on the surface of the material obtained in the step (6), and pressing for 20min at the normal temperature of 100MPa to obtain the carbon crystal electric heating film.
Example 3: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Preparing carbon crystal microsphere powder:
(1-1) adding 8g of graphite material to 300ml of acetone, and mixing;
(1-2) adding 2800g of zirconia ball milling beads with the particle size of 0.1mm into the mixture obtained in the step (1-1) for ball milling until the particle size of the graphite material is 10 nm-100 microns and the particle size dispersity index is less than 0.2, and then carrying out vacuum drying at 50 ℃ and-0.05 MPa for 12 hours to obtain carbon crystal microsphere powder with the particle size of 10 nm-100 microns;
(2) adding 8g of carbon crystal microsphere powder obtained in the step (1) into 300ml of acetone, and uniformly mixing under 300W of ultrasound;
(3) adding 0.8g of polystyrene into the mixture obtained in the step (2), and uniformly mixing under 300W ultrasound;
(4) drying the mixture obtained in the step (3) in vacuum at 50 ℃ and-0.05 MPa until acetone is completely removed to obtain polystyrene-coated carbon crystal microsphere powder;
(5) carrying out thermogravimetric analysis experiments and differential scanning calorimetry experiments on the polystyrene-coated carbon crystal microsphere powder obtained in the step (4) to obtain heating conditions, and obtaining the decomposition temperature, the glass transition temperature and the viscous flow conversion temperature of the polystyrene-coated carbon crystal microsphere powder, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the polystyrene-coated carbon crystal microsphere powder in a hot-pressing die or rolling equipment, heating to 155 ℃, and preserving heat until the polystyrene-coated carbon crystal microsphere powder is completely converted into a molten state;
(6) hot-press molding the material obtained in the step (5) at 200 ℃ and 200MPa for 0.5h, and then cooling to 25 ℃;
(7) and (4) attaching a PI film and a copper electrode on the surface of the material obtained in the step (6), and pressing for 15min at the normal temperature of 50MPa to obtain the carbon crystal electric heating film.
Example 4: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Preparing carbon crystal microsphere powder:
(1-1) adding 7g of graphene material to 400ml of ethanol, and mixing;
(1-2) adding 52.5g of zirconia ball milling beads with the particle size of 0.1mm into the mixture obtained in the step (1-1) for ball milling until the particle size of the graphene material is 10 nm-100 microns and the particle size dispersity index is less than 0.2, and then carrying out vacuum drying at 45 ℃ and-0.15 MPa for 10 hours to obtain carbon crystal microsphere powder with the particle size of 10 nm-100 microns;
(2) adding 9g of carbon crystal microsphere powder obtained in the step (1) into 500ml of ethanol, and uniformly mixing under 100W of ultrasound;
(3) adding 10g of polycarbonate into the mixture obtained in the step (2), and uniformly mixing under 100W ultrasound;
(4) drying the mixture obtained in the step (3) in vacuum at 55 ℃ and-0.15 MPa until ethanol is completely removed to obtain polycarbonate-coated carbon crystal microsphere powder;
(5) heating conditions are obtained by subjecting the polycarbonate-coated carbon crystal microsphere powder obtained in the step (4) to a thermogravimetric analysis experiment and a differential scanning calorimetry experiment, and the decomposition temperature, the glass transition temperature and the viscous flow conversion temperature of the polycarbonate-coated carbon crystal microsphere powder are obtained, wherein the decomposition temperature is determined by taking the weight loss as a standard of reaching 1%; then placing the polycarbonate-coated carbon crystal microsphere powder in a hot pressing mold or rolling equipment, heating to 100 ℃, and preserving heat until the polycarbonate-coated carbon crystal microsphere powder is completely converted into a molten state;
(6) hot-press molding the material obtained in the step (5) at 100 ℃ and 100MPa for 1h, and then cooling to 25 ℃;
(7) and (4) attaching a PET film and a copper electrode on the surface of the material obtained in the step (6), and pressing at 20MPa and normal temperature for 20min to obtain the carbon crystal electric heating film.
Example 5: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Adding 7g of polystyrene microsphere carbide into 200ml of acetone, and uniformly mixing under 400W ultrasound;
(2) adding 14g of epoxy resin E-44 into the mixture obtained in the step (2), and uniformly mixing under 400W ultrasound;
(3) drying the mixture obtained in the step (2) in vacuum at 50 ℃ and-0.15 MPa until acetone is completely removed to obtain carbon crystal microsphere powder coated with epoxy resin E-44;
(4) carrying out thermogravimetric analysis experiments and differential scanning calorimetry experiments on the carbon crystal microsphere powder coated with the epoxy resin E-44 obtained in the step (3) to obtain heating conditions, and obtaining the decomposition temperature, the glass transition temperature and the viscous flow conversion temperature of the carbon crystal microsphere powder coated with the epoxy resin E-44, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the carbon crystal microsphere powder coated with the epoxy resin E-44 in a hot pressing die or rolling equipment, heating to 80 ℃, and preserving heat until the carbon crystal microsphere powder coated with the epoxy resin E-44 is completely converted into a molten state;
(5) hot-press molding the material obtained in the step (4) at 250 ℃ and 400MPa for 0.5h, and then cooling to 25 ℃;
(6) and (5) attaching a PET film and a copper electrode on the surface of the material obtained in the step (5), and pressing at the normal temperature of 10MPa for 20min to obtain the carbon crystal electric heating film.
Example 6: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Adding 9g of organic glass microsphere carbide into 500ml of ethanol, and uniformly mixing under 350W of ultrasound;
(2) adding 17g of epoxy resin E-44 into the mixture obtained in the step (2), and uniformly mixing under 350W ultrasound;
(3) drying the mixture obtained in the step (2) in vacuum at 55 ℃ and-0.05 MPa until ethanol is completely removed to obtain carbon crystal microsphere powder coated with epoxy resin E-44;
(4) carrying out thermogravimetric analysis experiments and differential scanning calorimetry experiments on the carbon crystal microsphere powder coated with the epoxy resin E-44 obtained in the step (3) to obtain heating conditions, and obtaining the decomposition temperature, the glass transition temperature and the viscous flow conversion temperature of the carbon crystal microsphere powder coated with the epoxy resin E-44, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the carbon crystal microsphere powder coated with the epoxy resin E-44 in a hot pressing die or rolling equipment, heating to 200 ℃, and preserving heat until the carbon crystal microsphere powder coated with the epoxy resin E-44 is completely converted into a molten state;
(5) hot-press molding the material obtained in the step (4) at 80 ℃ and 400MPa for 0.5h, and then cooling to 25 ℃;
(6) and (5) attaching an epoxy resin film and a copper electrode on the surface of the material obtained in the step (5), and pressing at 1MPa and normal temperature for 10min to obtain the carbon crystal electric heating film.
Example 7: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Adding 9g of polycarbonate microsphere carbide into 500ml of ethanol, and uniformly mixing under 350W of ultrasound;
(2) adding 18g of epoxy resin E-51 into the mixture obtained in the step (2), and uniformly mixing under 350W ultrasound;
(3) drying the mixture obtained in the step (2) in vacuum at 55 ℃ and-0.05 MPa until ethanol is completely removed to obtain carbon crystal microsphere powder coated with epoxy resin E-51;
(4) carrying out thermogravimetric analysis experiments and differential scanning calorimetry experiments on the epoxy resin E-51-coated carbon crystal microsphere powder obtained in the step (3) to obtain heating conditions, and obtaining the decomposition temperature, glass transition temperature and viscous flow conversion temperature of the epoxy resin E-51-coated carbon crystal microsphere powder, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the carbon crystal microsphere powder coated with the epoxy resin E-51 in a hot pressing die or rolling equipment, heating to 50 ℃, and preserving heat until the carbon crystal microsphere powder coated with the epoxy resin E-51 is completely converted into a molten state;
(5) hot-press molding the material obtained in the step (4) at 50 ℃ and 500MPa for 0.5h, and then cooling to 25 ℃;
(6) and (5) attaching an epoxy resin film and a copper electrode on the surface of the material obtained in the step (5), and pressing for 15min at the normal temperature of 100MPa to obtain the carbon crystal electric heating film.
Example 8: the invention relates to a preparation method of a carbon crystal electric heating film
(1) Adding 7g of polyacrylonitrile microsphere carbide into 200ml of ethanol, and uniformly mixing under 400W of ultrasound;
(2) adding 14g of epoxy resin E-51 into the mixture obtained in the step (2), and uniformly mixing under 400W ultrasound;
(3) drying the mixture obtained in the step (2) in vacuum at 55 ℃ and-0.05 MPa until ethanol is completely removed to obtain carbon crystal microsphere powder coated with epoxy resin E-51;
(4) carrying out thermogravimetric analysis experiments and differential scanning calorimetry experiments on the epoxy resin E-51-coated carbon crystal microsphere powder obtained in the step (3) to obtain heating conditions, and obtaining the decomposition temperature, glass transition temperature and viscous flow conversion temperature of the epoxy resin E-51-coated carbon crystal microsphere powder, wherein the decomposition temperature is determined by taking the weight loss reaching 1% as a standard; then placing the carbon crystal microsphere powder coated with the epoxy resin E-51 in a hot pressing die or rolling equipment, heating to 200 ℃, and preserving heat until the carbon crystal microsphere powder coated with the epoxy resin E-51 is completely converted into a molten state;
(5) hot-press molding the material obtained in the step (4) at 300 ℃ and 500MPa for 0.5h, and then cooling to 25 ℃;
(6) and (5) attaching an epoxy resin film and a copper electrode on the surface of the material obtained in the step (5), and pressing at the normal temperature of 80MPa for 10min to obtain the carbon crystal electric heating film.
Conductive electrodes are stacked on two ends of the carbon crystal electric heating film prepared in the above embodiments 1 to 8, so that a nano carbon crystal infrared electric heating device with low energy consumption, high efficiency and long-distance heat supply can be obtained.
In the above embodiments 1 to 8 of the present invention, in the step of preparing the carbon crystal microsphere powder, the carbon crystal microsphere powder with uniform particle size is obtained after ball milling, which ensures the excellent optical performance of the final product, see fig. 1; the thermoplastic polymer material is coated in the step (4), so that carbon crystal microsphere powder with uniform components is obtained, and the attached figure 2 is shown; through the hot pressing process in the step (6), a good photonic crystal arrangement structure is obtained, and the structure is shown in figure 3; conductive electrodes are stacked on two ends of the carbon crystal electric heating film prepared in the above embodiments 1 to 8, so that a nano carbon crystal infrared electric heating device which has low energy consumption and high efficiency and realizes remote heat supply can be obtained, and the attached figure 4 shows.
In conclusion, the above description of the embodiments of the present invention is not intended to limit the present invention, and those skilled in the art can make various changes or modifications according to the present invention without departing from the spirit of the present invention, which falls within the scope of the appended claims.
Claims (9)
1. A preparation method of a carbon crystal electric heating film comprises the following steps:
(1) mixing the carbon crystal microsphere powder with a solvent, and uniformly mixing under 100-400W ultrasound; wherein the grain diameter of the carbon crystal microsphere powder is 10 nm-100 mu m; the ratio of the mass of the carbon crystal microsphere powder to the volume of the solvent is (7-9) g (200-500) ml; the solvent is selected from acetone and/or ethanol;
(2) mixing a thermoplastic high polymer material with the mixture obtained in the step (1), and uniformly mixing under 100-400W ultrasound;
(3) drying the mixture obtained in the step (2) in vacuum at 45-55 ℃ and-0.15-0.05 MPa until the solvent is completely removed to obtain carbon crystal microsphere powder coated with the thermoplastic high polymer material;
(4) heating the carbon crystal microsphere powder coated with the thermoplastic high polymer material obtained in the step (3) to 50-200 ℃, and preserving heat until the carbon crystal microsphere powder coated with the thermoplastic high polymer material is completely converted into a molten state;
(5) hot-press molding the material obtained in the step (4) at 50-300 ℃ and 1-500 MPa for 0.5-1 h, and then cooling to 25 ℃;
(6) pasting an insulating film and a copper electrode on the surface of the material obtained in the step (5), and pressing to obtain the carbon crystal electric heating film;
the preparation method of the carbon crystal microsphere powder in the step (1) comprises the following steps:
(1-1) mixing and mixing a carbon raw material and an organic solvent; wherein the ratio of the mass of the carbon raw material to the volume of the organic solvent is (7-9) g (200-500) ml; the organic solvent is selected from acetone and/or ethanol;
(1-2) mixing zirconia ball milling beads with the particle size of 0.01-1 mm with the mixture obtained in the step (1-1), then carrying out ball milling until the particle size of the carbon raw material is 10 nm-100 mu m and the particle size dispersity index is less than 0.2, and then carrying out vacuum drying at 45-55 ℃ and-0.15-0.05 MPa for 11-13 h to obtain carbon crystal microsphere powder with the particle size of 10 nm-100 mu m; wherein the mass ratio of the zirconia ball grinding beads to the carbon raw material is (150-350) g and (1-20) g.
2. The method of claim 1, wherein in step (1-1), the carbon material is selected from one or more of carbon fiber, carbon nanotube, graphite, and graphene.
3. The method of claim 2, wherein the carbon material is carbon fiber T300.
4. The method for preparing a carbon crystal electrothermal film according to claim 1, wherein in the step (1-2), the zirconia ball milling beads have a particle size of 0.1 mm.
5. The method for preparing a carbon crystal electrothermal film according to claim 1, wherein in the step (1), the thermoplastic polymer material is one or more selected from polyethylacrylate, polyurethane, polystyrene, polycarbonate, epoxy resin E-44 and epoxy resin E-51.
6. The preparation method of the carbon crystal electrothermal film according to claim 1, wherein in the step (2), the mass ratio of the thermoplastic polymer material to the carbon crystal microsphere powder in the step (1) is (1-2) g and (1-20) g.
7. The method for preparing a carbon crystal electrothermal film according to claim 1, wherein the step (6) is: adhering an insulating film and a copper electrode on the surface of the material obtained in the step (5), and pressing at 1-100MPa and normal temperature for 10-20 min to obtain the carbon crystal electric heating film; wherein the insulating film is selected from one or more of epoxy resin film, PEEK film, PI film and PET film.
8. The carbon crystal electric heating film obtained by the preparation method of the carbon crystal electric heating film according to any one of claims 1 to 7.
9. Use of the carbon crystal electric heating film obtained by the preparation method of the carbon crystal electric heating film according to any one of claims 1 to 7 in preparation of a carbon crystal electric heating device.
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