CN114538425A - Production equipment and preparation method of graphene heat dissipation film - Google Patents
Production equipment and preparation method of graphene heat dissipation film Download PDFInfo
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- CN114538425A CN114538425A CN202210156916.0A CN202210156916A CN114538425A CN 114538425 A CN114538425 A CN 114538425A CN 202210156916 A CN202210156916 A CN 202210156916A CN 114538425 A CN114538425 A CN 114538425A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 160
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 49
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- 238000000926 separation method Methods 0.000 claims abstract description 28
- 238000003860 storage Methods 0.000 claims abstract description 25
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 27
- 239000001257 hydrogen Substances 0.000 claims description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims description 27
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- 238000005096 rolling process Methods 0.000 claims description 16
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- 230000008569 process Effects 0.000 claims description 8
- 239000002912 waste gas Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 5
- 238000007750 plasma spraying Methods 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
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- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 4
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- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B16/00—Spray booths
- B05B16/20—Arrangements for spraying in combination with other operations, e.g. drying; Arrangements enabling a combination of spraying operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/16—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed
- B05B7/22—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
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Abstract
Production equipment and a preparation method of a graphene heat dissipation film are provided, wherein the production equipment comprises a separation part, a drying part, a spraying reduction repair part, a conveying part, a soaking part, a UV light reaction part, a washing part and a drying part, wherein the separation part comprises a separation barrel capable of separating graphene particles with relatively large sheet diameters from a graphene dispersion liquid to separate the graphene oxide dispersion liquid with large sheet diameters; the drying part comprises a spray dryer which can dry the large-sheet-diameter graphene oxide dispersion liquid into powder; the spraying reduction repairing part comprises a plasma sprayer, a working gas storage tank, a carbon source storage tank and a closed heating furnace, and the conveying part comprises an unreeling machine, a base band, a calender and a reeling machine. The graphene heat dissipation film prepared by the method can exert higher heat conduction capability, and the strength of the heat dissipation film can be improved, so that the heat dissipation film is more resistant to bending.
Description
Technical Field
The invention relates to the field of graphene application, in particular to production equipment and a preparation method of a graphene heat dissipation film.
Background
With the progress of technology, various electronic products are miniaturized and integrated, the use of large heat dissipation devices is limited in space, and heat dissipation devices with thin size, high thermal conductivity and flexibility are required to be developed for more effective heat dissipation, single-layer graphene has high thermal conductivity exceeding 5000W/m.k but is not suitable for being used as a heat dissipation material, and the current industrialized flexible heat dissipation film mainly depends on flexible pyrolytic graphite or graphitized polyimide, and the highest thermal conductivity in the plane of the flexible heat dissipation film is 1950W/m.k. The graphene oxide is an oxide of graphene, and a large number of oxygen-containing functional groups such as hydroxyl carboxyl and the like are introduced on the surface and the edge of the graphene oxide, so that the graphene oxide can exist stably in an aqueous solution and a polar solvent, the prepared solution can be manufactured into a film by various technologies (including vacuum filtration, spray coating, bar coating, electrochemical deposition and shearing arrangement), but a large number of groups in the graphene oxide destroy sp2 carbon hybrid structures, so that the thermal conductivity is greatly reduced, and if the graphene oxide is reduced, the groups can be eliminated.
In the prior art, a graphene heat dissipation film is prepared by coating graphene oxide slurry to obtain a graphene oxide film through the steps of coating, drying, carbonizing, graphitizing, rolling, and the like, and the graphene oxide film is carbonized and graphitized after drying to obtain the graphene heat dissipation film, wherein the thermal conductivity of the graphene heat dissipation film is generally 400-1000W/mK, and the thickness of the graphene heat dissipation film is generally 10-100 micrometers. In the process, after the graphene oxide is carbonized and graphitized, some lattice defects still remain and are not repaired, so that the heat conduction capability of the graphene is reduced, and the finally produced graphene heat dissipation film is not tightly bonded with the sheet layers, so that the flexibility of the heat dissipation film is influenced. The scheme is generated.
Disclosure of Invention
The invention aims to provide production equipment and a preparation method of a graphene heat dissipation film, which can enable the graphene heat dissipation film to exert higher heat conduction capacity, and can improve the strength of the heat dissipation film so as to enable the heat dissipation film to be more resistant to bending.
In order to achieve the above purpose, the solution of the invention is:
a production device of a graphene heat dissipation film comprises a separation part, a drying part, a spraying reduction repair part, a conveying part, a soaking treatment part, a UV photoreaction part, a washing part and a drying part, wherein,
the separation part comprises a separation barrel capable of separating graphene particles with relatively large sheet diameters from the graphene dispersion liquid to separate the graphene oxide dispersion liquid with large sheet diameters;
the drying part comprises a spray dryer which can dry the graphene oxide dispersion liquid with large sheet diameter into powder;
the spraying reduction repair part comprises a plasma sprayer, a working gas storage tank, a carbon source storage tank and a closed heating furnace, the conveying part comprises an unreeling machine, a baseband, a calender and a reeling machine, the drying part and the working gas storage tank are respectively communicated with the plasma sprayer, the working gas in the working gas storage tank enters the plasma sprayer and is ionized into hydrogen plasma, the plasma sprayer is positioned above the closed heating furnace, large-sheet-diameter graphene oxide powder in the drying part enters the plasma sprayer and is sprayed on the baseband sent out by the unreeling machine under the pushing of the hydrogen plasma to form a reduced graphene oxide radiating film, carbon source gas in the carbon source storage tank is introduced into the closed heating furnace, the unreeling machine sends the baseband to the closed heating furnace, the carbon source gas is sequentially sent to the soaking treatment part, the UV light reaction part, the washing part and the drying part after the graphene radiating film is formed in the closed heating furnace, finally, the mixture passes through a calender and a winding machine;
the soaking part is filled with soaking liquid, the washing part is filled with washing solution, and the UV light reaction part is provided with a UV light source.
Further, be equipped with centrifugal device in the separator vat, the separation portion still includes a big piece footpath oxidation graphite alkene dispersion collecting vessel and a small footpath graphite alkene dispersion collecting vessel that collects relative small footpath graphite alkene granule, is equipped with feed inlet and small footpath graphite alkene dispersion export, big piece footpath graphite alkene dispersion export in the separator vat.
Further, the drying part still includes the cyclone that can follow the powder and separate out in the air current, and spray dryer's both ends are connected with first inlet pipe and first discharging pipe, are equipped with the charge pump in the first inlet pipe, and first discharging pipe is connected to cyclone.
Further, the spraying reduction repair part further comprises a second feeding pipe, large-sheet-diameter graphene oxide powder enters the plasma sprayer from the second feeding pipe, a spraying opening is formed in the plasma sprayer, the large-sheet-diameter graphene oxide powder is sprayed into the closed heating furnace through the spraying opening, and a working gas input pipe is connected between the working gas storage tank and the plasma sprayer.
And furthermore, a waste gas treatment tank and a waste gas collecting device are arranged outside the closed heating furnace, and waste gas discharged by reaction in the closed heating furnace is introduced into the waste gas treatment tank through an exhaust pipe for absorption treatment and then is collected into the waste gas collecting device for harmless treatment.
A preparation method of a graphene heat dissipation film comprises the following steps:
step 3, reducing the large-sheet-diameter graphene oxide powder in a hydrogen plasma spraying mode and spraying the reduced graphene oxide powder on a base band to form a reduced graphene oxide heat dissipation film;
and 5, sequentially carrying out soaking treatment, UV light irradiation, washing and drying on the repaired graphene heat dissipation film, and finally carrying out calendaring and rolling to form a finished graphene heat dissipation film product, wherein the graphene heat dissipation film is subjected to crosslinking between graphene sheet layers through a bis-aziridine compound in the soaking treatment and UV light irradiation processes.
Further, in the step 1, adding the graphene oxide dispersion liquid into the separation barrel, and centrifuging the graphene oxide dispersion liquid in the separation barrel at 8000RPM of 5000-.
8. The method for preparing a graphene heat dissipation film according to claim 6, wherein: and 3, enabling the working gas to enter a plasma sprayer to be ionized into hydrogen plasma, enabling the large-sheet-diameter graphene oxide powder to enter the plasma sprayer and be sprayed into the sealed heating furnace under the pushing of the hydrogen plasma, reducing the large-sheet-diameter graphene oxide powder by the hydrogen plasma, spraying the graphene oxide powder onto a base band sent out by an unreeling machine to form a reduced graphene oxide heat dissipation film, wherein the working gas in the working gas storage tank is hydrogen and argon gas =5: 95-10: 90, or hydrogen and helium gas =5: 95-10: 90, or ammonia gas.
Further, in step 4, the carbon source gas is one of methane, ethylene or acetylene, and the carbon source gas is put into a closed heating furnace and reacts with the reduced graphene oxide heat dissipation film for 10min to 40min at the temperature of 800-.
Further, in the step 5, the repaired graphene heat dissipation film is soaked in dichloromethane or trichloromethane solution of 1-10% bis-aziridine compound for 5-20min, then irradiated by UV light with the wavelength of 365-400nm for 30s-120s to form cross-linking between graphene layers, then washed by dichloromethane or trichloromethane, baked at 60-80 ℃ for 5-10min, dried, rolled in a rolling mill at the pressure of 20-30MPa, and then rolled by a rolling machine.
After the scheme is adopted, through the process flow and the production equipment, the sheet diameter of the graphene is screened firstly, the graphene oxide with large sheet diameter is selected, spray drying is carried out to obtain the graphene oxide powder with large sheet diameter, then the graphene oxide powder with large sheet diameter is reduced in a hydrogen plasma spraying mode and sprayed on the base band to form the heat dissipation film, and the defects on the surface of the graphene are repaired under the action of a carbon source and high temperature, so that the obtained graphene heat dissipation film reduces the scattering of phonons and can play higher heat conduction capability due to the fact that the lattice defects are repaired. And then crosslinking the graphene film by using the bis-aziridine compound to enable graphene sheet layers to be closely linked together, so that the strength of the heat dissipation film is improved, and the heat dissipation film is more resistant to bending.
Drawings
FIG. 1 is a schematic view of the structure of a production apparatus of the present invention;
FIG. 2 is a process flow diagram of the present invention;
fig. 3 is a graph of the cross-linking reaction of graphene sheets.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
As shown in FIG. 1, the invention discloses a production device of a graphene heat dissipation film, which comprises a separation part 1, a drying part 2, a spray reduction repair part 3, a conveying part 4, a soaking treatment part 5, a UV photoreaction part 6, a washing part 7 and a drying part 8.
The separation part 1 includes a separation barrel 11 capable of separating graphene particles with relatively large sheet diameters from the graphene dispersion liquid, so as to separate the graphene oxide dispersion liquid with large sheet diameters. The separation barrel 11 is provided with a centrifugal device (not shown in the figure), and the separation part further comprises a large-diameter graphene oxide dispersion liquid collection barrel 12 and a small-diameter graphene dispersion liquid collection barrel 13 for collecting relatively small-diameter graphene particles. The separation barrel 11 is provided with a feed port 111, a small-diameter graphene dispersion liquid outlet 112, and a large-diameter graphene dispersion liquid outlet 113. When the graphene oxide particle separation device is used, graphene oxide dispersion liquid is added from the feeding hole 111, and is subjected to centrifugal treatment at 8000RPM for 10-30min through a centrifugal device in the separation barrel at 5000-8000RPM, and due to the fact that the sizes of the graphene particle sheet diameters are different, the sedimentation speed is different, large sheet diameters are easy to settle, the graphene particle separation device can be more easily centrifuged to the edge, small sheet diameters are not easy to settle, and the graphene particle separation device can be relatively concentrated in the middle of a vortex, so that separation can be achieved. Therefore, the small-diameter graphene oxide dispersion liquid can enter the small-diameter graphene oxide dispersion liquid collecting barrel 13 through the small-diameter graphene oxide dispersion liquid outlet 112, and the large-diameter graphene oxide dispersion liquid enters the large-diameter graphene oxide dispersion liquid collecting barrel 11 through the large-diameter graphene oxide dispersion liquid outlet 113. Because graphite alkene heat conduction relies on the transmission of phonon, when having met fracture or defect department, phonon transmission meets hindering the emergence scattering, can reduce heat conduction efficiency, and the sheet diameter of graphite alkene is big more, and graphite alkene is just more complete, and the transmission efficiency of phonon is just also higher, so utilize the separation part to leave out the great graphene oxide of sheet diameter in this case.
The drying section 2 comprises a spray dryer 21 for drying the large-sheet-diameter graphene oxide dispersion liquid into powder, and a cyclone separator 22 for separating the powder from the airflow, wherein the cyclone separator can separate particles in the airflow. The both ends of spray dryer 21 are connected with first inlet pipe 23 and first discharging pipe 24, are equipped with charge-in pump 25 in the first inlet pipe, and first inlet pipe 24 stretches into in big piece footpath oxidation graphite alkene dispersion collecting vessel 12, and first discharging pipe 24 is connected to cyclone. During operation, the dispersion liquid in the large-diameter graphene oxide dispersion liquid collecting barrel 11 is sucked into the spray dryer 21 through the first feeding pipe 23 and the feeding pump 25, and the dried powder enters the cyclone separator 22 through the first discharging pipe 24 to separate the large-diameter graphene oxide powder from the air flow.
The spray reduction repair part 3 includes a plasma sprayer 31, a working gas storage tank 32, a carbon source storage tank 33 and a closed heating furnace 34, and the conveying part 4 includes an unreeling machine 41, a base band 42, a calender 43 and a reeling machine 44. The drying part and the working gas storage tank 32 are respectively communicated to the plasma sprayer 31, the plasma sprayer 31 is positioned above the closed heating furnace 34, the carbon source gas in the carbon source storage tank 33 is introduced into the closed heating furnace 34, the unreeling machine 41 sends out the base band 42 to the closed heating furnace 34, the base band 42 passes through the closed heating furnace and then is sequentially conveyed to the soaking treatment part 5, the UV light reaction part 6, the washing part 7 and the drying part 8, and finally, the base band is rolled by the reeling machine after being rolled by the rolling machine 43. The working gas input pipe 35 is connected between the working gas storage tank 32 and the plasma sprayer 31, the working gas in the working gas storage tank enters the plasma sprayer through the working gas input pipe 35 and is ionized into hydrogen plasma, and the working gas can be hydrogen gas and argon gas =5: 95-10: 90, or hydrogen gas and helium gas =5: 95-10: 90, or ammonia gas. The spraying reduction repair part further comprises a second feeding pipe 36, the large-sheet-diameter graphene oxide powder enters the plasma sprayer 31 from the second feeding pipe 36, a spraying opening 311 is formed in the plasma sprayer 31, and the large-sheet-diameter graphene oxide powder is sprayed into the closed heating furnace 34 through the spraying opening 311. The large-diameter graphene oxide powder reduced by the hydrogen plasma is sprayed on the base tape 42 fed from the unreeling machine 41 to form a reduced graphene oxide heat dissipation film (not specifically shown in the figure). The working gas enters the plasma sprayer and is ionized between the electrodes, and then the graphene oxide powder is sprayed on the base material, and in the process, the large-sheet-diameter graphene oxide powder is reduced by hydrogen plasma. The carbon source gas in the carbon source storage tank 33 is introduced into the closed heating furnace 34, and the carbon source gas (one of methane, ethylene and acetylene) in the carbon source storage tank 33 enters the closed heating furnace 34 to react with the graphene heat dissipation film, so that the defects of the graphene in the graphene heat dissipation film are repaired.
Furthermore, an exhaust gas treatment tank 37 and an exhaust gas collecting device 38 are arranged outside the closed heating furnace 34, and exhaust gas discharged by reaction in the closed heating furnace 34 is introduced into the exhaust gas treatment tank through an exhaust pipe for absorption treatment and then collected into the exhaust gas collecting device for harmless treatment.
The repaired graphene heat dissipation film is sequentially conveyed to the soaking treatment part 5, the UV light reaction part 6, the washing part 7 and the drying part 8, and finally rolled by the rolling machine 44 after being rolled by the rolling machine 43. The soaking part 5 includes a soaking tank 51 filled with a soaking solution of 1-10% methylene chloride or chloroform of a bisaziridine compound. The UV light source 61 is arranged in the UV light reaction part 6, and the soaked graphene heat dissipation film can be crosslinked between graphene layers after being irradiated by UV light. Among them, the bisaziridine compound produces a highly active intermediate under UV light irradiation, which possesses four active bisaziridine groups and can rapidly undergo an insertion reaction with a portion of C (sp3) -H bonds remaining adjacent to graphene, thereby achieving chemical crosslinking, as shown in fig. 3. Then washing with a washing solution (dichloromethane or chloroform) in washing section 7, and baking and drying in drying section 8, washing section 7 may comprise a washing tank filled with the washing solution, and drying section 8 may comprise a drying oven or a drying oven. The rolling mill and the winding machine are located behind the drying part, and finally enter the rolling mill 43 for rolling treatment at the pressure of 20-30MPa, and then are wound by the winding machine 44 to form a graphene heat dissipation film finished product.
The invention also discloses a preparation method of the graphene heat dissipation film, and each step of the preparation method can be completed by means of the production equipment. Referring to fig. 2, the preparation method of the present invention includes the following steps:
step 3, reducing the large-sheet-diameter graphene oxide powder in a hydrogen plasma spraying mode and spraying the reduced graphene oxide powder on a base band to form a reduced graphene oxide heat dissipation film;
and 5, sequentially carrying out soaking treatment, UV light irradiation, washing and drying on the repaired graphene heat dissipation film, and finally carrying out calendaring and rolling to form a finished graphene heat dissipation film product, wherein the graphene heat dissipation film is subjected to crosslinking between graphene sheet layers through a bis-aziridine compound in the soaking treatment and UV light irradiation processes.
In the step 1, the graphene oxide dispersion liquid can be added into the separation barrel 11, and the graphene oxide dispersion liquid is subjected to centrifugal treatment for 10-30min at 8000RPM in the separation barrel with 5000-. The large-sheet-diameter graphene oxide dispersion liquid with a relatively large sheet diameter can be separated and collected in the large-sheet-diameter graphene oxide dispersion liquid collection barrel 12.
In the step 2, after the large-sheet-diameter graphene oxide dispersion liquid can be dried into powder by using the spray dryer 21, the method further includes a step 21 of separating the powder from the airflow, and the particles in the airflow can be separated by using the cyclone separator 22, so that the large-sheet-diameter graphene oxide powder enters the plasma sprayer 31 in the step 3.
In step 3, the working gas enters the plasma sprayer 31 and is ionized into hydrogen plasma, the graphene oxide powder with large sheet diameter enters the plasma sprayer and is sprayed into the closed heating furnace 34 under the pushing of the hydrogen plasma, the graphene oxide powder with large sheet diameter is reduced by the hydrogen plasma, and the graphene oxide powder is sprayed onto the base band 42 sent out by the unreeling machine 41 to form the reduced graphene oxide heat dissipation film. The working gas in the working gas storage tank 32 is hydrogen and argon =5: 95-10: 90, or hydrogen and helium =5: 95-10: 90, or ammonia.
In the step 4, the carbon source gas is one of methane, ethylene or acetylene, and the carbon source gas enters the closed heating furnace 34 and reacts with the reduced graphene oxide heat dissipation film for 10min to 40min at the temperature of 800-.
In the step 5, the repaired heat dissipation film is soaked in a dichloromethane or trichloromethane solution of 1-10% bis-aziridine compound for 5-20min, then irradiated by UV light with the wavelength of 365-400nm for 30s-120s to form cross-linking between graphene layers, then washed by dichloromethane or trichloromethane, baked at 60-80 ℃ for 5-10min, dried, rolled in a rolling machine 43 at the pressure of 20-30MPa, and then rolled by a rolling machine 44.
Through the process flow, the sheet diameter of graphene is screened firstly, graphene oxide with large sheet diameter is selected, spray drying is carried out, then the graphene oxide with large sheet diameter is reduced in a hydrogen plasma spraying mode and sprayed on a base band to form a heat dissipation film, and the defects on the surface of the graphene are repaired under the action of a carbon source and high temperature, so that the obtained graphene heat dissipation film is repaired due to the lattice defects, the scattering of phonons is reduced, and higher heat conductivity coefficient can be exerted. And then crosslinking the graphene film by using a bis-aziridine compound, so that graphene sheet layers are closely connected, and the strength of the heat dissipation film is improved, and the heat dissipation film is more resistant to bending.
Referring to the following table 1, by comparison, the graphene heat dissipation film prepared by the present invention can improve the overall strength of the graphene heat dissipation film, improve the bending capability thereof, and simultaneously improve the thermal conductivity.
TABLE 1
The above embodiments and drawings are not intended to limit the form and style of the present invention, and any suitable changes or modifications thereof by those skilled in the art should be considered as not departing from the scope of the present invention.
Claims (10)
1. The utility model provides a production facility of graphite alkene heat dissipation membrane which characterized in that: comprises a separation part, a drying part, a spray coating reduction repair part, a conveying part, a soaking part, a UV photoreaction part, a washing part and a drying part, wherein,
the separation part comprises a separation barrel capable of separating graphene particles with relatively large sheet diameters from the graphene dispersion liquid to separate the graphene oxide dispersion liquid with large sheet diameters;
the drying part comprises a spray dryer which can dry the graphene oxide dispersion liquid with large sheet diameter into powder;
the spraying reduction repair part comprises a plasma sprayer, a working gas storage tank, a carbon source storage tank and a closed heating furnace, the conveying part comprises an unreeling machine, a baseband, a calender and a reeling machine, the drying part and the working gas storage tank are respectively communicated with the plasma sprayer, the working gas in the working gas storage tank enters the plasma sprayer and is ionized into hydrogen plasma, the plasma sprayer is positioned above the closed heating furnace, large-sheet-diameter graphene oxide powder in the drying part enters the plasma sprayer and is sprayed on the baseband sent out by the unreeling machine under the pushing of the hydrogen plasma to form a reduced graphene oxide radiating film, carbon source gas in the carbon source storage tank is introduced into the closed heating furnace, the unreeling machine sends the baseband to the closed heating furnace, the carbon source gas is sequentially sent to the soaking treatment part, the UV light reaction part, the washing part and the drying part after the graphene radiating film is formed in the closed heating furnace, finally, the mixture passes through a calender and a winding machine;
the soaking part is filled with soaking liquid, the washing part is filled with washing solution, and the UV light reaction part is provided with a UV light source.
2. The production equipment of the graphene heat dissipation film as recited in claim 1, wherein: the separating part comprises a large-sheet-diameter graphene oxide dispersion liquid collecting barrel and a small-sheet-diameter graphene dispersion liquid collecting barrel for collecting relatively small-sheet-diameter graphene particles, and the separating barrel is internally provided with a feed inlet, a small-sheet-diameter graphene dispersion liquid outlet and a large-sheet-diameter graphene dispersion liquid outlet.
3. The apparatus for producing a graphene heat dissipation film according to claim 1 or 2, wherein: the drying part still includes the cyclone that can follow the powder and separate out in the air current, and spray dryer's both ends are connected with first inlet pipe and first discharging pipe, are equipped with the charge pump in the first inlet pipe, and first discharging pipe is connected to cyclone.
4. The production equipment of the graphene heat dissipation film as recited in claim 1, wherein: the spraying reduction repairing part further comprises a second feeding pipe, large-sheet-diameter graphene oxide powder enters the plasma sprayer from the second feeding pipe, a spraying opening is formed in the plasma sprayer, the large-sheet-diameter graphene oxide powder is sprayed into the closed heating furnace through the spraying opening, and a working gas input pipe is connected between the working gas storage tank and the plasma sprayer.
5. The production equipment of the graphene heat dissipation film as recited in claim 4, wherein: and the waste gas discharged by the reaction in the closed heating furnace is introduced into the waste gas treatment tank through the exhaust pipe for absorption treatment and then is collected into the waste gas collection device for harmless treatment.
6. A preparation method of a graphene heat dissipation film is characterized by comprising the following steps:
step 1, screening the sheet diameter of graphene, and separating a large-sheet-diameter graphene oxide dispersion liquid from a graphene oxide dispersion liquid;
step 2, carrying out spray drying on the large-sheet-diameter graphene oxide dispersion liquid to form large-sheet-diameter graphene oxide powder;
step 3, reducing the large-sheet-diameter graphene oxide powder in a hydrogen plasma spraying mode and spraying the reduced graphene oxide powder on a base band to form a reduced graphene oxide heat dissipation film;
step 4, utilizing a carbon source gas to react with the reduced graphene oxide heat dissipation film, and repairing the defects of graphene in the heat dissipation film under the action of a carbon source and high temperature;
and 5, sequentially carrying out soaking treatment, UV light irradiation, washing and drying on the repaired graphene heat dissipation film, and finally carrying out calendaring and rolling to form a finished graphene heat dissipation film product, wherein the graphene heat dissipation film is subjected to crosslinking between graphene sheet layers through a bis-aziridine compound in the soaking treatment and UV light irradiation processes.
7. The method for preparing a graphene heat dissipation film according to claim 6, wherein: in the step 1, adding the graphene oxide dispersion liquid into a separation barrel, and centrifuging the graphene oxide dispersion liquid in the separation barrel at 8000RPM of 5000-.
8. The method for preparing a graphene heat dissipation film according to claim 6, wherein: and 3, enabling the working gas to enter a plasma sprayer to be ionized into hydrogen plasma, enabling the large-sheet-diameter graphene oxide powder to enter the plasma sprayer and be sprayed into the sealed heating furnace under the pushing of the hydrogen plasma, reducing the large-sheet-diameter graphene oxide powder by the hydrogen plasma, spraying the graphene oxide powder onto a base band sent out by an unreeling machine to form a reduced graphene oxide heat dissipation film, wherein the working gas in the working gas storage tank is hydrogen and argon gas =5: 95-10: 90, or hydrogen and helium gas =5: 95-10: 90, or ammonia gas.
9. The method for preparing a graphene heat dissipation film according to claim 6 or 8, wherein: in the step 4, the carbon source gas is one of methane, ethylene or acetylene, and the carbon source gas is put into a closed heating furnace and reacts with the reduced graphene oxide heat dissipation film for 10min to 40min at the temperature of 800-.
10. The method for preparing a graphene heat dissipation film according to claim 6, wherein: in the step 5, the repaired graphene heat dissipation film is soaked in dichloromethane or trichloromethane solution of 1-10% bis-aziridine compound for 5-20min, then irradiated by UV light with the wavelength of 365-400nm for 30s-120s to form cross-linking between graphene layers, then washed by dichloromethane or trichloromethane, baked at 60-80 ℃ for 5-10min, dried, rolled in a rolling machine at the pressure of 20-30MPa, and then rolled by a rolling machine.
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