CN115520862A - Preparation method of artificial high-thermal-conductivity ultrathin graphite film - Google Patents

Preparation method of artificial high-thermal-conductivity ultrathin graphite film Download PDF

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CN115520862A
CN115520862A CN202211234245.1A CN202211234245A CN115520862A CN 115520862 A CN115520862 A CN 115520862A CN 202211234245 A CN202211234245 A CN 202211234245A CN 115520862 A CN115520862 A CN 115520862A
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polyimide
heat treatment
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heating
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CN115520862B (en
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王文静
唐伟
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Zhonghui Ruineng Fengyang New Material Technology Co ltd
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Zhonghui Ruineng Fengyang New Material Technology Co ltd
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Abstract

The invention relates to a preparation method of an artificial high-thermal-conductivity ultrathin graphite film, which comprises the steps of carrying out pyrolysis treatment on a polyimide PI film at 500-600 ℃, carrying out carbonization treatment on the polyimide PI film after the pyrolysis treatment at 1000-1500 ℃, and carrying out graphitization treatment on the polyimide PI film after the carbonization treatment, wherein a rapid high-temperature heat treatment device is adopted in the graphitization treatment process, and the heating rate of the rapid high-temperature heat treatment device is 10 3 ~10 4 The temperature of the heat treatment is 2500-3500 ℃, and the thickness of the graphitized polyimide PI film is 20-50 mu m. The graphite film prepared by the method has ultrathin thickness, good softness and extremely high heat conductivity coefficient.

Description

Preparation method of artificial high-thermal-conductivity ultrathin graphite film
Technical Field
The invention relates to the field of preparation of high-thermal-conductivity ultrathin graphite films, in particular to a preparation method of an artificial high-thermal-conductivity ultrathin graphite film.
Background
The high heat conduction graphite film is a novel heat conduction and dissipation material, the laminated structure can adapt to uniform heat conduction and heat transfer on the surface, and the high heat conduction graphite film has the advantages of light weight, low density, high specific heat capacity, long-term reliability and the like, and is one of necessary parts for solving the heat dissipation problem of electronic products (or batteries). The natural graphite film has a thermal conductivity of 300-750W/m.K, a thickness of more than 50 μm, and is fragile and unable to be heatedBending; the graphene heat dissipation film has a high heat conductivity coefficient, but is expensive and not beneficial to large-scale production and use. Compared with a natural graphite film and a graphene heat dissipation film, the artificial high-heat-conductivity graphite film has extremely high cost performance. A graphite film with high thermal conductivity, which is obtained by using a highly oriented Polyimide (PI) film as a precursor and performing carbonization and graphitization, has become the main direction of an artificial high thermal conductivity graphite film. The thermal conductivity coefficient of the high thermal conductivity graphite film is 700-1900W/m.K, which is much higher than that of copper (380W/m.K) and aluminum (200W/m.K), and the density of the artificial high thermal conductivity graphite film is about 1.0-2.0 g/cm 3 Also much lower than metallic copper and aluminum. In addition, the artificial high-thermal-conductivity graphite film with high thermal conductivity and light weight can meet various special design requirements of electronic products in high integration, high density and light weight, the market scale of the global artificial high-thermal-conductivity graphite film exceeds billions, and the artificial high-thermal-conductivity graphite film has a wide application prospect.
The manufacturers of artificial high thermal conductivity graphite film mainly use foreign enterprises (such as du pont, korean SKC, japan Kaneka, etc.), and there is still a large gap between the technical level of the domestic graphite film products and the imported films, mainly because: (1) Polyimide (PI) has a low in-plane orientation (less than 25%) and a high thermal expansion coefficient (40 to 55X 10) -6 K), resulting in low interlayer and bulk thermal conductivity of the graphite film; (2) The graphitization process of the graphite film is complex, the temperature rise is slow, and the energy consumption is high, so that the heat conductivity of the film is low due to poor uniformity, a plurality of defects and the like of the graphite film. At present, certain theoretical basis is accumulated for carbonization and graphitization treatment of polyimide films for artificial high-thermal-conductivity graphite films at home and abroad, and an industrial production technology for carbonization and graphitization of oriented polyimide films is formed. In addition, the graphite material has anisotropic performance due to a special layered structure, the in-plane thermal conductivity of the graphite film is as high as 1000-2000W/m.K, and the theoretical thermal conductivity of the vertical plane is only hundreds, so that the improvement of the interlayer thermal conductivity is also a research hotspot of researchers at present.
The heat treatment technology of the polyimide film is the key for preparing the high-heat-conductivity graphite film. Conventional heat treatmentThe process needs to be carried out under the protection of vacuum or inert atmosphere, and mainly comprises the following three steps: (1) Heat treatment at 550-600 deg.c with CO and CO as oxygen atoms 2 The form escapes; (2) High temperature PI film carbonization (1000-1500 ℃), the process is N, H element as N 2 、H 2 And CH 4 The first two processes mainly carry out the removal of hetero atoms; (3) High-temperature graphitization treatment (2500-3000 ℃), in the process, after heteroatoms are almost eliminated, carbon is rearranged and grows from disorder to regular hexagonal carbon net structure, and thus the graphite film is obtained to improve the heat conducting property. However, the conventional heat treatment technology (especially the high-temperature graphitization treatment in the third step) generally has the defects of slow temperature rise rate (10-50 ℃/min) and long heat treatment time (5-10 h), which causes high energy consumption, long time consumption, high cost and the like, and a series of side reactions (poor uniformity, defect generation and the like) are easily caused in the long-time temperature rise process to cause low axial thermal conductivity after film formation and the like, so that the further development and application of the high thermal conductivity graphite film material are greatly limited, and therefore, the selection of a proper heat treatment process is very important.
Disclosure of Invention
Technical problem to be solved
The preparation method of the artificial high-thermal-conductivity ultrathin graphite film can solve the technical problems mentioned above.
(II) technical scheme
In view of the problems in the background art, the present invention provides a method for preparing an artificial high thermal conductivity ultrathin graphite film, and to achieve the technical purpose, the technical scheme adopted by the present invention is as follows:
a preparation method of an artificial high-thermal-conductivity ultrathin graphite film comprises the following steps:
(1) Performing pyrolysis treatment on the polyimide PI film at 500-600 ℃;
(2) Carbonizing the polyimide PI film subjected to pyrolysis treatment at 1000-1500 ℃;
(3) Graphitizing the carbonized polyimide PI film, wherein the graphitizing treatment is carried outThe process adopts a rapid high-temperature heat treatment device, and the heating rate of the rapid high-temperature heat treatment device is 10 3 ~10 4 The temperature is 2500-3500 ℃, the heat treatment temperature is 2500-3500 ℃, and the thickness of the graphitized polyimide PI film is 20-50 mu m.
The rapid high-temperature heat treatment device comprises a plurality of support frames, heat treatment modules and feeding rollers, wherein the heat treatment modules are arranged between the upper ends of the support frames, the heat treatment modules are of rectangular structures, open slots are symmetrically formed in the end parts of the heat treatment modules, and the feeding rollers are symmetrically arranged in the open slots through bearings;
the heat treatment module comprises a shell frame, a heating unit, a pressing unit, an electrifying unit and an electrifying frame, wherein the shell frame is of a rectangular hollow structure, the heating unit is symmetrically arranged in the middle of the shell frame, the pressing unit is arranged between the middle of the outer side of the heating unit and the shell frame, the electrifying unit is symmetrically arranged on the inner side wall of the shell frame and is connected with the end part of the heating unit, the electrifying frame is symmetrically arranged in the middle of the outer side of the shell frame and is electrically connected with the electrifying unit.
The method for preparing the high-heat-conductivity ultrathin graphite film by adopting the rapid high-temperature heat treatment device comprises the following steps:
s1, feeding the carbonized polyimide PI film into a heat treatment module through a feed roller, and enabling the carbonized polyimide PI film to pass through the heat treatment module under the action of a tractor;
s2, the pressing unit drives the heating unit to be tightly attached to the polyimide carbide PI film, the heating area of the heating unit is uniform, the heating rate and uniformity of the polyimide carbide PI film are effectively improved, meanwhile, the pressing unit can be adaptively adjusted according to the size of the polyimide carbide PI film, and further the polyimide carbide PI films with different sizes can be processed;
and S3, the power connection frame drives the power connection unit to be powered on, the power connection unit adopts the joule heat principle, and the powered power connection unit is quickly heated to form a high-temperature zone to realize graphitization treatment on the carbonized film.
Preferably, the polyimide PI film is 20-100 μm thick.
Preferably, the polyimide PI film is internally filled with a nanoparticle filler.
Preferably, the heating carbon strips are made of flexible heat-conducting materials and are one or more of carbon felt and carbon fiber cloth.
Preferably, the heating unit includes leading truck, slider, coupling spring and heating carbon strip, the leading truck is evenly installed to casing frame inside, and the leading truck middle part is provided with the spout, is connected with the slider through sliding fit's mode in the spout, installs coupling spring between the slider outside and the spout, installs the heating carbon strip between the adjacent slider.
Preferably, the compressing unit comprises an electric push rod, a fixed pressing plate, a movable pressing plate and a telescopic rod, the electric push rod is uniformly installed inside the shell frame, the top end of the electric push rod is connected with the fixed pressing plate through a flange, the fixed pressing plate is of a rectangular structure, the movable pressing plate is symmetrically arranged on the outer side of the fixed pressing plate, the telescopic rod is uniformly installed between the movable pressing plate and the fixed pressing plate, and the inner side surfaces of the movable pressing plate and the fixed pressing plate are tightly attached to the heating carbon strip.
Preferably, the electrifying unit comprises a transverse plate, electric sliders, a movable plate, an electrifying assembly and pressing rollers, the transverse plate is symmetrically arranged inside the shell frame, the electric sliders are arranged on the transverse plate, the movable plate is arranged between the outer sides of the electric sliders, the electrifying assembly is arranged in the middle of the movable plate, the pressing rollers are symmetrically arranged on the movable plate, a guide groove is formed between the pressing rollers and the electrifying assembly, and the heating carbon strips are located inside the guide groove.
Preferably, the circular telegram subassembly includes link, pressure strip, baffle, guide bar, briquetting, expanding spring and iron sheet, install the link between the movable plate, the link middle part is hollow structure, logical groove is installed to the symmetry on the link, it is connected with the pressure strip to lead to the inslot through sliding fit's mode, the link mid-mounting has the baffle, the baffle middle part is provided with the through-hole, be connected with the guide bar through sliding fit's mode in the through-hole, the briquetting is installed to guide bar one end, the briquetting is the trapezium structure, the briquetting lateral surface is hugged closely with the pressure strip, be located and be provided with expanding spring on the guide bar between baffle and the briquetting, the guide bar other end outside is provided with the electrical coil, link internally mounted has the iron sheet.
Preferably, state the pressure strip up end and be the arcwall face, the pressure strip is electrically conductive material, and the pressure strip is connected with the electricity between the connecing the electric rack, evenly is provided with electrically conductive copper sheet on the pressure strip indent face.
(III) advantageous effects
1. The rapid high-temperature heat treatment device provided by the invention can rapidly reach the ultrahigh temperature (reaching 3000 ℃ in 1 min), and is beneficial to improving the crystallinity of graphite, thereby improving the heat-conducting property of the graphite.
2. The rapid high-temperature heat treatment device provided by the invention effectively improves the condition that the temperature zone of the traditional heat treatment technology is not uniform, the polyimide carbide PI film is directly contacted with the heating carbon strip, the heating zone is uniform, and the heating rate and uniformity of the polyimide carbide PI film can be effectively improved.
3. The rapid high-temperature heat treatment device provided by the invention is beneficial to reducing the defects of the graphite film, improving the crystallinity of the graphite film and optimizing the interlayer spacing of the graphite film, thereby improving the plane and radial heat conductivity of the graphite film.
4. The rapid high-temperature heat treatment device provided by the invention can simplify the production process, reduce the energy consumption, and is beneficial to improving the production efficiency and reducing the time and labor cost.
5. The length and the shape of the heating carbon strip provided by the invention can be designed according to the heated polyimide PI film, and the length of the heating carbon strip can be changed to adapt to the polyimide PI films with different sizes, so that the continuous preparation of the high-thermal-conductivity graphite film is facilitated.
6. The graphite film prepared by adopting the rapid high-temperature heat treatment technology has ultrathin thickness, good softness and extremely high heat conductivity coefficient, can effectively adapt to the requirements and trends of increasingly thinner consumer electronic products, realizes the localization of the high-heat-conductivity graphite film, has simple and flexible high-temperature heat treatment technology, greatly reduces the production energy consumption and time cost through the rapid high-temperature heat treatment technology, can improve the uniformity of the graphite film, reduces the defects of the graphite film, and improves the quality of the graphite film such as heat conductivity.
Drawings
The invention is further illustrated by the following examples in conjunction with the drawings.
FIG. 1 is a process flow diagram of the present application.
Fig. 2 is a schematic perspective view of the present application.
Fig. 3 is a schematic perspective view of the present application.
Fig. 4 is a sectional structure diagram of the present application.
Fig. 5 is a schematic cross-sectional structure of the present application.
Fig. 6 is a schematic view of the present application in partial cross-section of fig. 5.
FIG. 7 is a perspective view of the energizing assembly of the present application;
fig. 8 is a schematic cross-sectional view of the energizing assembly of the present application.
Detailed Description
Example 1:
a preparation method of an artificial high-thermal-conductivity ultrathin graphite film comprises the following steps:
(1) Performing pyrolysis treatment on the polyimide PI film at 500-600 ℃;
(2) And (3) carbonizing the polyimide PI film subjected to pyrolysis treatment by heating from room temperature to 1300 ℃ in a vacuum state, wherein the carbonization heating procedure is as follows: heating to 600 ℃ from room temperature at a heating rate of 20 ℃/min, keeping the temperature of 1 h, and then continuously heating to 1300 ℃ according to the original heating rate;
(3) Graphitizing the carbonized polyimide PI film, wherein the graphitizing process adopts a rapid high-temperature heat treatment device, the cooled carbonized polyimide PI film is transferred into the rapid high-temperature heat treatment device after vacuum carbonization is finished, and the temperature rise rate of the rapid high-temperature heat treatment device is 10 3 ~10 4 Graphitizing at room temperature to 2800 deg.C under argon gas for 1min, and maintaining the temperature for 10 min.
Above-mentioned quick high temperature heat treatment device includes support frame 1, thermal treatment module 2 and feed roll 3, 1 quantity of support frame is a plurality of, installs thermal treatment module 2 between 1 upper ends of support frame, and thermal treatment module 2 is the rectangle structure, and 2 tip symmetries of thermal treatment module are provided with the open slot, installs feed roll 3 through the bearing symmetry in the open slot.
The heat treatment module 2 comprises a shell frame 21, a heating unit 22, a pressing unit 23, an electrifying unit 24 and an electrifying frame 25, wherein the shell frame 21 is of a rectangular hollow structure, the heating unit 22 is symmetrically installed in the middle of the shell frame 21, the pressing unit 23 is installed between the middle of the outer side of the heating unit 22 and the shell frame 21, the electrifying unit 24 is symmetrically installed on the inner side wall of the shell frame 21, the electrifying unit 24 is connected with the end part of the heating unit 22, the electrifying frame 25 is symmetrically installed in the middle of the outer side of the shell frame 21, and the electrifying frame 25 is electrically connected with the electrifying unit 24.
The method for preparing the high-heat-conductivity ultrathin graphite film by adopting the rapid high-temperature heat treatment device comprises the following steps:
s1, feeding the carbonized polyimide PI film into a heat treatment module 2 through a feed roller 3, and enabling the carbonized polyimide PI film to pass through the heat treatment module 2 under the action of a tractor;
s2, the pressing unit 23 drives the heating unit 22 to be tightly attached to the polyimide carbide PI film, the heating area of the heating unit 22 is uniform, the heating rate and uniformity of the polyimide carbide PI film are effectively improved, meanwhile, the pressing unit 23 can be adaptively adjusted according to the size of the polyimide carbide PI film, and therefore the polyimide carbide PI films with different sizes can be processed;
and S3, the electrifying frame 25 drives the electrifying unit 24 to be electrified, the electrifying unit 24 adopts the joule heat principle, and the electrified electrifying unit 24 is rapidly heated to form a high-temperature zone so as to realize graphitization treatment on the carbonized film.
The thickness of the polyimide PI film is 20-100 mu m.
The polyimide PI film is internally filled with nano particle fillers, the nano particle fillers are added in the preparation process of the PI film, and the content of the nano particle fillers can be 0.01-20% of one or more combinations.
The nano particle filler can be one or a combination of more of carbon material, metal simple substance or alloy material and inorganic non-metal material. The carbon material is one or more of carbon black, carbon quantum dots, graphene, carbon nanotubes and carbon fibers; the metal simple substance or alloy material is one or more of silver, gold, aluminum, copper, magnesium, tungsten, zinc, aluminum alloy, copper alloy and magnesium alloy; the inorganic non-metallic material is one or more of aluminum oxide, silicon oxide, zinc oxide, boron nitride, aluminum nitride, silicon nitride and silicon carbide.
The heating unit 22 comprises a guide frame 221, sliders 222, connecting springs 223 and heating carbon strips 224, the guide frame 221 is uniformly installed inside the shell frame 21, sliding grooves are formed in the middle of the guide frame 221, the sliders 222 are connected in the sliding grooves in a sliding fit mode, the connecting springs 223 are installed between the outer sides of the sliders 222 and the sliding grooves, and the heating carbon strips 224 are installed between the adjacent sliders 222.
The heating carbon strips 224 are made of flexible heat conducting materials, the heating carbon strips 224 are made of one or more of carbon felts and carbon fiber cloth, and the carbon felts are made of one or more of polyacrylonitrile-based carbon felts, asphalt-based carbon felts or adhesive-based carbon felts.
As is known from joule's theorem, the amount of heat generated by the current passing through the conductor is proportional to the square of the current intensity, inversely proportional to the resistance of the conductor, and proportional to the energization time, and when the current passes through the heated carbon strip 224, the heated carbon strip 224 rapidly generates a large amount of heat. The temperature rise rate can be adjusted by adjusting the current, and the temperature rise rate can reach 10 3 ~10 4 The temperature reduction rate is as high as 10℃/min 4 The temperature is lower than the min, so that the energy consumption can be effectively reduced.
The pressing unit 23 comprises an electric push rod 231, a fixed pressing plate 232, a movable pressing plate 233 and an expansion link 234, the electric push rod 231 is uniformly installed inside the shell frame 21, the top end of the electric push rod 231 is connected with the fixed pressing plate 232 through a flange, the fixed pressing plate 232 is of a rectangular structure, the movable pressing plate 233 is symmetrically arranged on the outer side of the fixed pressing plate 232, the expansion link 234 is uniformly installed between the movable pressing plate 233 and the fixed pressing plate 232, and the inner side surfaces of the movable pressing plate 233 and the fixed pressing plate 232 are tightly attached to the heating carbon strip 224.
The electrifying unit 24 comprises a transverse plate 241, an electric slider 242, a moving plate 243, an electrifying assembly 244 and a pressing roller 245, the transverse plate 241 is symmetrically installed in the shell frame 21, the electric slider 242 is installed on the transverse plate 241, the moving plate 243 is installed between the outer sides of the electric sliders 242, the electrifying assembly 244 is installed in the middle of the moving plate 243, the pressing roller 245 is symmetrically installed on the moving plate 243, a guide groove is formed between the pressing roller 245 and the electrifying assembly 244, and the heating carbon strips 224 are located in the guide groove.
The electrifying assembly 244 comprises a connecting frame 2441, a pressing plate 2442, a partition 2443, a guide rod 2444, a pressing block 2445, a telescopic spring 2446 and an iron sheet 2447, the connecting frame 2441 is installed between the moving plates 243, the middle of the connecting frame 2441 is of a hollow structure, through grooves are symmetrically installed on the connecting frame 2441, the pressing plate 2442 is connected in the through grooves in a sliding fit mode, the partition 2443 is installed in the middle of the connecting frame 2441, a through hole is formed in the middle of the partition 2443, the guide rod 2444 is connected in the through hole in a sliding fit mode, the pressing block 2445 is installed at one end of the guide rod 2444, the pressing block 2445 is of a trapezoidal structure, the outer side face of the pressing block 2445 is tightly attached to the pressing plate 2442, the telescopic spring 2446 is arranged on the guide rod 2444 between the partition 2443 and the pressing block 2445, an electrifying coil is arranged on the outer side of the other end of the guide rod 2444, and the iron sheet 2447 is installed inside the connecting frame 2441.
The upper end face of the pressing plate 2442 is an arc-shaped face, the pressing plate 2442 is made of a conductive material, the pressing plate 2442 is electrically connected with the electricity connection frame 25, a conductive copper sheet is uniformly arranged on the concave face in the pressing plate 2442, the contact efficiency between the conductive copper sheet and the heating carbon strip 224 can be effectively increased, and the phenomenon of poor conductivity is avoided.
Comparative example 1:
in the comparative example, the traditional graphite film preparation process is adopted, the prepared polyimide PI film is carbonized by heating from room temperature to 1300 ℃ in a vacuum state, and the temperature rise procedure of the carbonization is as follows: raising the temperature from room temperature to 600 ℃ at a heating rate of 20 ℃/min, preserving the heat of 1 h, and then continuing raising the temperature to 1300 ℃ according to the original heating rate; and (3) transferring the cooled carbonized polyimide PI film into a graphite furnace after carbonization is finished, and heating the film from room temperature to 2800 ℃ under argon gas for graphitization, wherein the graphitization heating procedure is as follows: the temperature of the polyimide PI film is raised to 1600 ℃ from room temperature at the heating rate of 20 ℃/min, and the temperature is maintained at 5 h and then raised to 2800 ℃ at the original rate.
Example 2:
in this embodiment, a graphite film is prepared by using a rapid high-temperature heat treatment technology, the cooled carbonized polyimide PI film in embodiment 1 is transferred to a heated carbon strip 224 after vacuum carbonization, and is graphitized by heating from room temperature to 2800 ℃ under argon for 1min, and maintaining the temperature for 20 min.
Example 3:
in this embodiment, a graphite film is prepared by using a rapid high-temperature heat treatment technology, the cooled carbonized polyimide PI film in embodiment 1 is transferred to a heated carbon strip 224 after vacuum carbonization, and is graphitized by heating from room temperature to 2800 ℃ under argon for 1min, and maintaining the temperature for 30 min.
Example 4:
in this embodiment, a graphite film is prepared by using a rapid high-temperature heat treatment technology, the cooled carbonized polyimide PI film in embodiment 1 is transferred to a heated carbon strip 224 after vacuum carbonization, and is graphitized by heating from room temperature to 3000 ℃ under argon for 1min, and maintaining the temperature for 20 min.
Example 5:
in this embodiment, a graphite film is prepared by using a rapid high-temperature thermal treatment technology, a polyimide PI film containing 2% carbon quantum dots is carbonized by heating from room temperature to 1300 ℃ in a vacuum state, and the temperature rise procedure of the carbonization is as follows: heating to 600 ℃ from room temperature at a heating rate of 20 ℃/min, keeping the temperature of 1 h, and then continuously heating to 1300 ℃ according to the original heating rate; and after the vacuum carbonization is finished, transferring the cooled carbonized polyimide PI film into a heating carbon strip 224, heating the temperature from room temperature to 2800 ℃ under argon gas for graphitization, wherein the heating time is 1min, and keeping the temperature for 20 min.
Comparative example 2:
in the comparative example, the conventional graphite film preparation process is adopted, and the polyimide PI film containing 2% of carbon quantum dots is carbonized by heating from room temperature to 1300 ℃ in a vacuum state, wherein the temperature rise procedure of the carbonization is as follows: raising the temperature from room temperature to 600 ℃ at a heating rate of 20 ℃/min, preserving the heat of 1 h, and then continuing raising the temperature to 1300 ℃ according to the original heating rate; and (3) transferring the cooled carbonized film into a graphite furnace after carbonization is finished, and graphitizing the carbonized film from room temperature to 2800 ℃ under argon, wherein the temperature rising procedure of graphitization is as follows: the temperature of the polyimide PI film is raised to 1600 ℃ from room temperature at the heating rate of 20 ℃/min, and the temperature is maintained at 5 h and then raised to 2800 ℃ at the original rate.
Example 6:
in this embodiment, a graphite film is prepared by using a rapid high-temperature heat treatment technology, the cooled carbonized polyimide PI film in embodiment 2 is transferred to a heated carbon strip 224 after vacuum carbonization is completed, and is graphitized by heating from room temperature to 3000 ℃ under nitrogen for 1min, and the temperature is maintained for 20 min.
FIG. 1 shows a schematic view of a
Figure DEST_PATH_IMAGE001

Claims (9)

1. A method for preparing an artificial high-thermal-conductivity ultrathin graphite film,
(1) Performing pyrolysis treatment on the polyimide PI film at 500-600 ℃;
(2) Carbonizing the polyimide PI film subjected to pyrolysis treatment at 1000-1500 ℃;
(3) Graphitizing the carbonized polyimide PI film, wherein the graphitizing process adopts a rapid high-temperature heat treatment device, and the temperature rise rate of the rapid high-temperature heat treatment device is 10 3 ~10 4 The temperature of the heat treatment is 2500-3500 ℃, and the thickness of the graphitized polyimide PI film is 20-50 mu m;
the rapid high-temperature heat treatment device comprises a plurality of support frames (1), heat treatment modules (2) and feed rollers (3), wherein the heat treatment modules (2) are arranged between the upper ends of the support frames (1), the heat treatment modules (2) are rectangular in structure, open slots are symmetrically formed in the end parts of the heat treatment modules (2), and the feed rollers (3) are symmetrically arranged in the open slots through bearings;
the heat treatment module (2) comprises a shell frame (21), a heating unit (22), a pressing unit (23), an electrifying unit (24) and an electrifying frame (25), wherein the shell frame (21) is of a rectangular hollow structure, the heating unit (22) is symmetrically arranged in the middle of the shell frame (21), the pressing unit (23) is arranged between the middle of the outer side of the heating unit (22) and the shell frame (21), the electrifying unit (24) is symmetrically arranged on the inner side wall of the shell frame (21), the electrifying unit (24) is connected with the end part of the heating unit (22), the electrifying frame (25) is symmetrically arranged in the middle of the outer side of the shell frame (21), and the electrifying frame (25) is electrically connected with the electrifying unit (24);
the method for preparing the high-heat-conductivity ultrathin graphite film by adopting the rapid high-temperature heat treatment device comprises the following steps:
s1, feeding the carbonized polyimide PI film into a heat treatment module (2) through a feed roller (3), and enabling the carbonized polyimide PI film to pass through the heat treatment module (2) under the action of a tractor;
s2, the pressing unit (23) drives the heating unit (22) to be tightly attached to the carbonized film, the heating area of the heating unit (22) is uniform, meanwhile, the pressing unit (23) can be adaptively adjusted according to the size of the carbonized polyimide PI film, and further the carbonized polyimide PI films with different sizes can be processed;
s3, the power connection frame (25) drives the power connection unit (24) to be powered on, the power connection unit (24) adopts the joule heat principle, and the power connection unit (24) after being powered on is rapidly heated to achieve graphitization treatment of the carbonized film.
2. The preparation method of the artificial high-thermal-conductivity ultrathin graphite film as claimed in claim 1, characterized in that: the thickness of the polyimide PI film is 20-100 mu m.
3. The preparation method of the artificial high-thermal-conductivity ultrathin graphite film according to claim 1, characterized by comprising the following steps: and nano particle fillers are filled in the polyimide PI film.
4. The preparation method of the artificial high-thermal-conductivity ultrathin graphite film according to claim 1, characterized by comprising the following steps: heating unit (22) include leading truck (221), slider (222), coupling spring (223) and heating carbon strip (224), leading truck (221) is evenly installed to casing frame (21) inside, and leading truck (221) middle part is provided with the spout, is connected with slider (222) through sliding fit's mode in the spout, installs coupling spring (223) between slider (222) outside and the spout, installs heating carbon strip (224) between adjacent slider (222).
5. The preparation method of the artificial high-thermal-conductivity ultrathin graphite film according to claim 4, characterized by comprising the following steps: the heating carbon strips (224) are made of flexible heat conducting materials, and the heating carbon strips (224) are one or more of carbon felts and carbon fiber cloth.
6. The preparation method of the artificial high-thermal-conductivity ultrathin graphite film according to claim 5, characterized by comprising the following steps: compress tightly unit (23) and include electric putter (231), fixed pressing plate (232), remove clamp plate (233) and telescopic link (234), casing frame (21) inside evenly installs electric putter (231), and flange joint has fixed pressing plate (232) on the top of electric putter (231), and fixed pressing plate (232) are the rectangle structure, and fixed pressing plate (232) outside symmetry is provided with and removes clamp plate (233), evenly installs telescopic link (234) between removal clamp plate (233) and fixed pressing plate (232), and removal clamp plate (233) and fixed pressing plate (232) medial surface hug closely with heating carbon strip (224).
7. The preparation method of the artificial high-thermal-conductivity ultrathin graphite film according to claim 6, characterized by comprising the following steps: the power-on unit (24) comprises a transverse plate (241), an electric slider (242), a moving plate (243), a power-on assembly (244) and a pressing roller (245), the transverse plate (241) is symmetrically installed inside the shell frame (21), the electric slider (242) is installed on the transverse plate (241), the moving plate (243) is installed between the outer sides of the electric slider (242), the power-on assembly (244) is installed in the middle of the moving plate (243), the pressing roller (245) is symmetrically installed on the moving plate (243), a guide groove is formed between the pressing roller (245) and the power-on assembly (244), and the heating carbon strip (224) is located inside the guide groove.
8. The method for preparing the artificial high-thermal-conductivity ultrathin graphite film according to claim 7, characterized by comprising the following steps: the power-on assembly (244) comprises a connecting frame (2441), a pressing plate (2442), a partition plate (2443), a guide rod (2444), a pressing block (2445), a telescopic spring (2446) and an iron sheet (2447), the connecting frame (2441) is installed between the moving plates (243), the middle of the connecting frame (2441) is of a hollow structure, a through groove is symmetrically installed on the connecting frame (2441), the pressing plate (2442) is connected in the through groove in a sliding fit mode, the partition plate (2443) is installed in the middle of the connecting frame (2441), a through hole is formed in the middle of the partition plate (2443), the guide rod (2444) is connected in the through hole in a sliding fit mode, the pressing block (2445) is installed at one end of the guide rod (2444), the pressing block (2445) is of a trapezoidal structure, the outer side face of the pressing block (2445) and the pressing plate (2442), the telescopic spring (2446) is arranged on the guide rod (2444) between the partition plate (2443) and the pressing block (2445), a coil is arranged on the outer side of the other end of the guide rod (44), and the iron sheet (2447) is installed inside the connecting frame (2441).
9. The method for preparing the artificial high-thermal-conductivity ultrathin graphite film according to claim 8 is characterized in that: the upper end face of the pressing plate (2442) is an arc-shaped face, the pressing plate (2442) is made of a conductive material, the pressing plate (2442) is electrically connected with the electric connection rack (25), and conductive copper sheets are uniformly arranged on the concave face of the pressing plate (2442).
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