CN109640411B - Graphene constant-temperature electrothermal film and preparation method thereof - Google Patents
Graphene constant-temperature electrothermal film and preparation method thereof Download PDFInfo
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- CN109640411B CN109640411B CN201910083655.2A CN201910083655A CN109640411B CN 109640411 B CN109640411 B CN 109640411B CN 201910083655 A CN201910083655 A CN 201910083655A CN 109640411 B CN109640411 B CN 109640411B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
Abstract
The invention provides a graphene constant-temperature electrothermal film and a preparation method thereof. The graphene constant-temperature electrothermal film prepared by the invention is superior to the prior art in electric conduction and heat conduction performance due to the addition of the graphene material with a special structure, and can realize self-constant temperature (normal temperature PTC thermal control effect) in a low temperature range on the premise of not introducing other temperature control devices. Based on the excellent electric heating performance and far infrared radiation effect of the invention, the invention has wide application prospect in the field of heat preservation and health care products.
Description
Technical Field
The invention relates to the technical field of electric heating materials, in particular to a graphene constant-temperature electric heating film and a preparation method thereof.
Background
The electrothermal film heating system is different from a point heating system represented by a radiator, an air conditioner and a radiator and a line heating system represented by heating electric heating, and adopts a low-carbon heating high-tech product researched and developed by the modern aerospace technology in the field of surface heating. The electric heating film is a semitransparent polyester film which can generate heat after being electrified, a surface type heating mode is adopted, most of heat is emitted in a radiation mode, heating is uniform, and the comprehensive effect is generally superior to that of a traditional convection heating mode, so that the electric heating film is popular among users in recent years.
The prior electric heating film has different electric heating performance due to different used conductive components. If a loop formed by winding metal wires or carbon fibers into a certain shape is used as a heating element, the heating element generally has the defect of uneven heating, cannot be continuously used after being locally damaged, and has potential safety hazards. The electrothermal film is formed by coating conductive ink prepared by taking traditional materials such as graphene, carbon nano tubes, conductive carbon black and the like as conductive fillers, although the nano carbon materials theoretically have good conductivity, in the practical application process, various physical and chemical properties are not ideal due to the instability of the nano structure.
In addition, once the existing electric heating film is manufactured, the resistance (power) of the electric heating film is fixed, the on-off of a circuit is usually controlled by manual operation, the electric heating film is troublesome, and some improved products are provided at present, intelligent adjustment is realized by arranging devices such as a temperature sensor, but the structure is relatively complex.
Therefore, there is an urgent need for a room temperature PTC material which can be thermally controlled at room temperature and has a lower resistivity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the graphene constant-temperature electrothermal film and the preparation method thereof, wherein the safety and the conductivity of the preparation material are ideal, and the temperature and the power can be automatically adjusted.
In order to solve the above problems, the present invention provides the following technical solutions:
in one aspect, the invention provides a graphene constant-temperature electrothermal film, which comprises a conductive composite film,
the conductive composite film comprises the following components in parts by mass: 0.5-2 parts of graphene, and alkane substances: 15-40 parts of resin: 5-20 parts of an auxiliary agent, 0.5-5 parts of an auxiliary agent and the balance of an organic solvent.
Preferably, the conductive composite film comprises the following components in percentage by weight: 0.5-2 wt% of graphene, 15-40 wt% of alkane substances, 5-20 wt% of resin, 0.5-5 wt% of auxiliary agent and the balance of organic solvent, wherein the sum of the weight percentages of the components is 100 wt%.
Further, the graphene is a multi-level structure graphene prepared by a CVD method, has a special micro-morphology, and is a continuous integrated structure formed by combining two-dimensional graphene sheets and one-dimensional carbon nanotubes vertical to the surface of the two-dimensional graphene sheets. The special structure of the graphene has more excellent conductivity, and is more favorable for forming a conductive network.
Furthermore, the graphene is a graphene nano material, and the specific preparation method is as follows:
I) immersing the copper sheet in a mixed solution of sodium hydroxide solution and ammonia water (25%), standing, washing with deionized water and absolute ethyl alcohol respectively, and airing in the air to obtain Cu/Cu (OH)2A nanorod array; calcining the obtained product in an argon atmosphere to obtain a Cu/CuO nanorod array;
II) mixing and dissolving sodium hydroxide and glucose in water, adding the Cu/CuO nanorod array obtained in the step I), performing microwave hydrothermal reaction, cooling to room temperature, taking out solids, washing with deionized water and absolute ethyl alcohol respectively, and drying to obtain a Cu sheet loaded Cu nanorod array;
III) putting the material obtained in the step II) into a CVD (chemical vapor deposition) tube furnace, heating the tube furnace at the speed of 5 ℃/min under the mixed atmosphere of hydrogen and argon, then adjusting the hydrogen flow rate, introducing methane gas, keeping the temperature, turning off the hydrogen and methane gas, cooling to room temperature in the argon atmosphere, and taking out a sample to obtain the multi-level structure graphene growing on the surface of the copper substrate.
Furthermore, the graphene is subjected to surface spin coating of a layer of resin, then placed in an iron chloride solution, and put into use after the copper substrate is completely corroded, so that the structural integrity of the graphene in the subsequent use process can be guaranteed after the treatment. In the corrosion process, copper can be oxidized into copper ions by iron ions and enters the solution, namely, the copper ions are separated from graphene, and the resin spin-coated on the surface of the graphene can be filled between the nanotube arrays of the multi-level structure graphene, so that structural collapse cannot occur in the subsequent use process, and the structural integrity of the graphene after being removed from the surface of the copper substrate is ensured. The thickness of the resin has no special requirement, and the thickness is preferably 0.5-1 mm only in order to enable the graphene corroded on the substrate to float on the water surface and be taken out conveniently.
Further, the preparation method of the graphene comprises the following steps:
I) the cleaned copper sheet was immersed in a mixture of 200mL of a sodium hydroxide solution (10 mol/L) and 100mL of aqueous ammonia (25%), allowed to stand for 12 hours, and then washed with deionized water and absolute ethanol several times, respectively, in the airAir-drying to obtain Cu/Cu (OH)2Calcining the nanorod array at 550 ℃ for 2h in an argon atmosphere to obtain a Cu/CuO nanorod array;
II) mixing and dissolving 8g of sodium hydroxide and 8g of glucose in 80mL of water, adding the composite material obtained in the step I), carrying out microwave hydrothermal reaction for 1h at 160 ℃, taking out the solid after cooling to room temperature, washing the solid for several times by using deionized water and absolute ethyl alcohol respectively, and drying at 60 ℃ to obtain a Cu sheet loaded Cu nanorod array;
III) putting the material obtained in the step II) into a CVD (chemical vapor deposition) tube furnace, heating the tube furnace to 1000 ℃ at the speed of 5 ℃/min under the mixed atmosphere of hydrogen (the flow rate is 20 sccm) and argon (the flow rate is 800 sccm), then adjusting the flow rate of the hydrogen to 100sccm, introducing methane gas at the flow rate of 30sccm, keeping the temperature for 15min, turning off the hydrogen and the methane gas, cooling to room temperature in the argon atmosphere, and taking out a sample to obtain the multi-stage structure graphene growing on the surface of the copper substrate;
IV) spin-coating a layer of resin on the surface of the multilevel-structure graphene, then placing the multilevel-structure graphene in 0.5mol/L ferric chloride solution, putting the multilevel-structure graphene into use after the copper substrate is completely corroded, and ensuring the structural integrity of the multilevel-structure graphene in the subsequent use process after the multilevel-structure graphene is treated.
Further, the organic solvent is a polar organic solvent such as ethanol, acetone, acetonitrile, dichloromethane, triethylamine, Dimethylformamide (DMF), carbon tetrachloride, etc., preferably DMF.
Further, the alkane substance is one of straight-chain alkane or branched-chain alkane with 14-24 carbon atoms. The addition of the alkane can endow the material with PTC effect, the Curie temperature of the selected alkane substance adjusting material is 5-50 ℃, the Curie temperature is generally related to the melting point of the matrix, and different alkane substances have different melting points and also have different Curie temperatures. Preferably, the alkane substance is one of straight-chain alkane or branched alkane with 14, 15, 16, 17, 18, 19, 20, 21, 22, 23 and 24 carbon atoms; n-eicosane, n-tetradecane and n-tetracosane are preferred.
Further, the resin is one of polyurethane resin, acrylic resin or epoxy resin. The resin in the conductive composite film is consistent with the resin used for the surface spin coating of the graphene.
Furthermore, the auxiliary agent comprises a dispersing agent, a defoaming agent and a flatting agent, and the dosage of the three auxiliary agents is equal.
Further, the dispersing agent is HT-5027 of break Tai chemical industry Co., Ltd in Nantong, and the components can be uniformly dispersed by adding the dispersing agent; the leveling agent is SN-612 of auxiliary agent of Nippon Nuopaco, and the addition of the leveling agent enables the surface of a coating film to be smoother; the defoaming agent is T-7511 of Wanhuan environmental protection science and technology Limited company in Guangzhou, and the defoaming agent can remove bubbles generated in the stirring process.
On the other hand, the invention provides a preparation method of the graphene constant-temperature electrothermal film, which comprises the following specific steps:
1) fully stirring graphene, alkane substances, resin, an organic solvent and an auxiliary agent to prepare mixed slurry, coating the slurry on the surface of a base film, and drying to obtain a conductive composite film;
2) arranging conductive electrodes on two sides of the conductive composite film, and then removing the base film;
3) and covering insulating films on two sides of the conductive composite film to obtain the graphene constant-temperature electrothermal film.
Further, the base membrane is one of a PP membrane, a PE membrane, a PVC membrane or a PTFE membrane and plays a supporting role.
Furthermore, the coating thickness of the slurry is 80-160 μm, and a conductive composite film with a thickness of 20-40 μm can be formed after drying.
Further, the conductive electrode is printed conductive silver paste or copper paste, or pressed conductive copper tape or conductive cloth.
Further, the insulating film is a polyurethane film and plays roles of insulation, water resistance and protection.
In another aspect, the present invention provides a graphene having a special micro-morphology, wherein the specific structure is a continuous integral structure formed by combining two-dimensional graphene sheets and one-dimensional carbon nanotubes perpendicular to the surface of the graphene sheets. The special structure of the graphene has more excellent conductivity, and is more favorable for forming a conductive network.
Further, the graphene is a multi-level structure graphene prepared by a CVD method.
Further, the graphene is a graphene nano material, and the specific preparation method is as follows:
I) immersing the copper sheet in a mixed solution of sodium hydroxide solution and ammonia water (25%), standing, washing with deionized water and absolute ethyl alcohol respectively, and airing in the air to obtain Cu/Cu (OH)2A nanorod array; calcining the obtained product in an argon atmosphere to obtain a Cu/CuO nanorod array;
II) mixing and dissolving sodium hydroxide and glucose in water, adding the Cu/CuO nanorod array obtained in the step I), performing microwave hydrothermal reaction, cooling to room temperature, taking out solids, washing with deionized water and absolute ethyl alcohol respectively, and drying to obtain a Cu sheet loaded Cu nanorod array;
III) putting the material obtained in the step II) into a CVD (chemical vapor deposition) tube furnace, heating the tube furnace at the speed of 5 ℃/min under the mixed atmosphere of hydrogen and argon, then adjusting the hydrogen flow rate, introducing methane gas, keeping the temperature, turning off the hydrogen and methane gas, cooling to room temperature in the argon atmosphere, and taking out a sample to obtain the multi-level structure graphene growing on the surface of the copper substrate.
Advantageous effects
The invention provides a graphene constant-temperature electrothermal film and a preparation method thereof.
The graphene constant-temperature electrothermal film prepared by the invention has a normal-temperature PTC effect, when the temperature of the heating film rises to the Curie temperature of a material, the resistance of the heating film is sharply increased, so that the power is reduced, then the temperature of the heating film is reduced, and when the temperature of the heating film is lower than the Curie temperature, the heating film can continue to be heated, so that the self-constant temperature can be realized in a lower temperature range, additional devices such as a temperature sensor and the like are not required, and the graphene constant-temperature electrothermal film is simple.
Compared with other carbon materials, the graphene has higher conductivity, smaller specific gravity and better flexibility, so that the overall low-temperature resistivity of the material prepared by the invention is lower, the consumption of raw materials is less, and the flexibility is better. The heating film has ultrahigh electric conduction and heat conduction performance due to the adoption of the multi-level structure graphene and the special three-dimensional electric conduction network structure, is superior to an electric heating film which takes electric conduction carbon black, electric conduction carbon fiber, carbon nano tube or traditional two-dimensional graphene as electric conduction filler in the prior art, and has the advantages of less graphene consumption and cost saving.
The selected resin enables the prepared graphene constant-temperature electrothermal film to have excellent resistance stability, and has the characteristics of high temperature resistance, no toxicity, no harm and high strength.
In the thermal cycle process, the alkane substance can drive the graphene conductive network to change, so that the resistance inside the coating is changed, a positive temperature resistance effect is obtained, and the resistivity is regulated and controlled.
The surface of the graphene is modified by using the alkane substance and the resin, so that partial defects on the surface of the graphene are eliminated, the surface energy is reduced, the mechanical strength of the material is effectively improved, the mechanical property and the dispersion property of the graphene are improved,
the ester group of the resin is combined with the group on the surface of the graphene for reaction, and simultaneously, a layer of alkane substance is coated on the surface of the graphene to enhance the binding property of the graphene and the polymer matrix, so that a conductive network which is mutually bridged is formed, and the ultralow resistance of the PTC is realized.
Through the effect of the auxiliary agent, the problems of dispersion and defoaming of the graphene are solved. The contents and the proportions of the alkane substances, the resin and the graphene adjust the resistivity so as to meet different market demands.
The graphene material with a special structure is added, so that the electric conduction and heat conduction performance of the graphene material is superior to that of the prior art, and the self-constant temperature (normal temperature PTC thermal control effect) in a low temperature range can be realized on the premise of not introducing other temperature control devices. Based on the excellent electric heating performance and far infrared radiation effect of the invention, the invention has wide application prospect in the field of heat preservation and health care products.
Drawings
Fig. 1 is a schematic microscopic cross-sectional view of a multi-level structure graphene.
Fig. 2 is a temperature change curve of the graphene constant-temperature electrothermal film.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described below with reference to specific embodiments.
Example 1
I) Immersing the cleaned copper sheet in a mixed solution of 200mL of sodium hydroxide solution (10 mol/L) and 100mL of ammonia water (25%), standing for 12h, washing with deionized water and absolute ethyl alcohol for several times respectively, and airing in the air to obtain Cu/Cu (OH)2Calcining the nanorod array at 550 ℃ for 2h in an argon atmosphere to obtain a Cu/CuO nanorod array;
II) mixing and dissolving 8g of sodium hydroxide and 8g of glucose in 80mL of water, adding the composite material obtained in the step I), carrying out microwave hydrothermal reaction for 1h at 160 ℃, taking out the solid after cooling to room temperature, washing the solid for several times by using deionized water and absolute ethyl alcohol respectively, and drying at 60 ℃ to obtain a Cu sheet loaded Cu nanorod array;
III) putting the material obtained in the step II) into a CVD (chemical vapor deposition) tube furnace, heating the tube furnace to 1000 ℃ at the speed of 5 ℃/min under the mixed atmosphere of hydrogen (the flow rate is 20 sccm) and argon (the flow rate is 800 sccm), then adjusting the flow rate of the hydrogen to 100sccm, introducing methane gas at the flow rate of 30sccm, keeping the temperature for 15min, turning off the hydrogen and the methane gas, cooling to room temperature in the argon atmosphere, and taking out a sample to obtain the multi-stage structure graphene growing on the surface of the copper substrate;
IV) spin-coating a layer of resin on the surface of the multilevel-structure graphene, then placing the multilevel-structure graphene in 0.5mol/L ferric chloride solution, putting the multilevel-structure graphene into use after the copper substrate is completely corroded, and ensuring the structural integrity of the multilevel-structure graphene in the subsequent use process after the multilevel-structure graphene is treated.
Example 2
Accurately weighing 1g of graphene prepared in example 1, 30g of n-eicosane, 10g of polyurethane resin, 56g of DMF, 1gHT-5027, 1g of SN-612 and 1g T-7511, mixing the materials, stirring vigorously for 2 hours to fully dissolve or disperse solids to obtain mixed slurry, coating the slurry on the surface of a PVC film by adopting a coating process, setting the thickness of the coating to be 120 mu m, drying at 120 ℃ to obtain a conductive composite film with the thickness of about 30 mu m, attaching two conductive copper adhesive tapes at two ends of the film in parallel to serve as electrodes, attaching a layer of polyurethane film on the surface of the film, removing the PVC film on the other surface of the film, and attaching a layer of polyurethane film on the surface of the film to obtain the self-constant-temperature graphene electrothermal film.
Example 3
Accurately weighing 0.5g of graphene prepared in example 1, 40g of tetracosan, 5g of epoxy resin, 51.5g of triethylamine, 1gHT-5027, 1g of SN-612 and 1g T-7511, mixing the materials, stirring vigorously for 2 hours to fully dissolve or disperse solids to obtain mixed slurry, coating the slurry on the surface of a PTFE (polytetrafluoroethylene) film by adopting a coating process, setting the thickness of the coating to be 160 mu m, drying at 130 ℃ to obtain a conductive composite film with the thickness of about 40 mu m, attaching two conductive copper adhesive tapes at two ends of the film in parallel to serve as electrodes, then attaching a polyurethane film on the surface of the film, removing the PVC film on the other surface, and attaching a polyurethane film on the surface in the same way to obtain the self-constant temperature graphene electrothermal film.
Example 4
Accurately weighing 2g of graphene prepared in example 1, 20g of n-octadecane, 20g of acrylic resin, 55g of acetone, 1g of HT-5027, 1g of SN-612 and 1g T-7511, mixing the materials, stirring vigorously for 2 hours to fully dissolve or disperse solids to obtain mixed slurry, coating the slurry on the surface of a PE (polyethylene) film by adopting a coating process, setting the thickness of the coating to be 80 micrometers, drying at 120 ℃ to obtain a conductive composite film with the thickness of about 20 micrometers, printing two conductive silver paste belts in parallel at two ends of the film to serve as electrodes, then attaching a layer of polyurethane film on the surface of the film, removing the PVC film on the other surface of the film, and attaching a layer of polyurethane film on the surface of the film to obtain the self-constant-temperature graphene electrothermal film.
Example 5
And (3) performance testing:
two ends of the graphene constant-temperature electrothermal film prepared in the embodiment 2-4 are connected with wires, the tail ends of the wires are connected with electrodes inside the electrothermal film, and the other ends of the wires are connected with a power supply. The relationship of the temperature of the electrothermal film with time is tested under the voltage of 220V, and the obtained result is shown in figure 2, and the graph shows that the graphene constant-temperature electrothermal film prepared by the invention is rapid in temperature rise, the temperature tends to be constant after reaching a certain value, and the equilibrium temperatures of the three embodiments are 34 ℃, 48 ℃ and 27 ℃, respectively, which shows that the invention has good self-constant temperature effect.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and these changes and modifications are also considered to be included in the scope of the invention.
Claims (7)
1. A graphene constant-temperature electrothermal film is characterized by comprising a conductive composite film,
the conductive composite film comprises the following components in parts by mass: 0.5-2 parts of graphene, and alkane substances: 15-40 parts of resin: 5-20 parts of an auxiliary agent, 0.5-5 parts of an auxiliary agent and the balance of an organic solvent;
the graphene is a multi-level structure graphene prepared by a CVD method;
the graphene is a graphene nano material, and the specific preparation method comprises the following steps:
I) immersing the copper sheet in a mixed solution of sodium hydroxide solution and ammonia water (25%), standing, washing with deionized water and absolute ethyl alcohol respectively, and airing in the air to obtain Cu/Cu (OH)2A nanorod array; calcining the obtained product in an argon atmosphere to obtain a Cu/CuO nanorod array;
II) mixing and dissolving sodium hydroxide and glucose in water, adding the Cu/CuO nanorod array obtained in the step I), performing microwave hydrothermal reaction, cooling to room temperature, taking out solids, washing with deionized water and absolute ethyl alcohol respectively, and drying to obtain a Cu sheet loaded Cu nanorod array;
III) putting the material obtained in the step II) into a CVD (chemical vapor deposition) tube furnace, heating the tube furnace at the speed of 5 ℃/min under the mixed atmosphere of hydrogen and argon, then adjusting the hydrogen flow rate, introducing methane gas, keeping the temperature, turning off the hydrogen and methane gas, cooling to room temperature in the argon atmosphere, and taking out a sample to obtain the multi-level structure graphene growing on the surface of the copper substrate.
2. The graphene constant-temperature electrothermal film according to claim 1, wherein the specific structure of the graphene is a continuous integral structure formed by combining two-dimensional graphene sheets and one-dimensional carbon nanotubes vertical to the surface of the two-dimensional graphene sheets.
3. The graphene constant-temperature electrothermal film according to claim 1, wherein a layer of resin is coated on the surface of the graphene, and then the graphene is placed in ferric chloride solution and put into use after the copper substrate is completely corroded.
4. The graphene constant-temperature electrothermal film according to claim 1, wherein the organic solvent is ethanol, acetone, acetonitrile, dichloromethane, triethylamine, dimethylformamide or carbon tetrachloride;
the resin is one of polyurethane resin, acrylic resin or epoxy resin;
the auxiliary agent comprises a dispersing agent, a defoaming agent and a flatting agent, and the dosage of the three auxiliary agents is equal;
the alkane substance is one of straight-chain alkane or branched-chain alkane with 14-24 carbon atoms.
5. A preparation method of the graphene constant-temperature electrothermal film according to any one of claims 1 to 4, which is characterized by comprising the following specific steps:
1) fully stirring graphene, alkane substances, resin, an organic solvent and an auxiliary agent to prepare mixed slurry, coating the slurry on the surface of a base film, and drying to obtain a conductive composite film;
2) arranging conductive electrodes on two sides of the conductive composite film, and then removing the base film;
3) and covering insulating films on two sides of the conductive composite film to obtain the graphene constant-temperature electrothermal film.
6. The production method according to claim 5, wherein the base film is one of a PP film, a PE film, a PVC film, or a PTFE film;
the coating thickness of the slurry is 80-160 mu m, and a conductive composite film with the thickness of 20-40 mu m can be formed after drying;
the conductive electrode is printed with conductive silver paste or copper paste, or pressed with conductive copper adhesive tape or conductive cloth;
the insulating film is a polyurethane film.
7. The application of the graphene constant-temperature electrothermal film of any one of claims 1 to 4 in preparation of electrothermal films.
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| CN110713821A (en) * | 2019-10-10 | 2020-01-21 | 杨道源 | Electric-conductive and heat-conductive composite material and preparation method thereof |
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