CN115520862B - Preparation method of artificial high-thermal-conductivity ultrathin graphite film - Google Patents
Preparation method of artificial high-thermal-conductivity ultrathin graphite film Download PDFInfo
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- CN115520862B CN115520862B CN202211234245.1A CN202211234245A CN115520862B CN 115520862 B CN115520862 B CN 115520862B CN 202211234245 A CN202211234245 A CN 202211234245A CN 115520862 B CN115520862 B CN 115520862B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 53
- 239000010439 graphite Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 124
- 229920001721 polyimide Polymers 0.000 claims abstract description 100
- 239000004642 Polyimide Substances 0.000 claims abstract description 97
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005087 graphitization Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000000197 pyrolysis Methods 0.000 claims abstract description 8
- 230000000630 rising effect Effects 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims description 62
- 229910052799 carbon Inorganic materials 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 230000006835 compression Effects 0.000 claims description 9
- 238000007906 compression Methods 0.000 claims description 9
- 239000004020 conductor Substances 0.000 claims description 8
- 238000005192 partition Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 230000005611 electricity Effects 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002105 nanoparticle Substances 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 229910052786 argon Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241000826860 Trapezium Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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Abstract
The invention relates to a preparation method of an artificial high heat conduction 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 pyrolysis treatment at 1000-1500 ℃, and carrying out graphitization treatment on the polyimide PI film after carbonization treatment, wherein a rapid high-temperature heat treatment device is adopted in the graphitization treatment process, and the temperature rising rate of the rapid high-temperature heat treatment device is 10 3 ～10 4 The temperature of heat treatment is 2500-3500 ℃ at the temperature of/min, and the thickness of the graphitized polyimide PI film is 20-50 mu m. The graphite film prepared by the invention has ultrathin thickness, good softness and extremely large heat conductivity coefficient.
Description
Technical Field
The invention relates to the field of preparation of high-heat-conductivity ultrathin graphite films, in particular to a preparation method of an artificial high-heat-conductivity ultrathin graphite film.
Background
The high heat conduction graphite film is a novel heat conduction and heat dissipation material, and the laminated structure can be suitable for uniform heat conduction and heat transfer on the surface, has the advantages of light weight, low density, high specific heat capacity, long-term reliability and the like, and is one of the necessary parts for solving the heat dissipation problem of electronic products (or batteries). The natural graphite film has a heat conductivity coefficient of 300-750W/m.K, a thickness of more than 50 mu m, is fragile and can not be bent and processed; the graphene heat dissipation film has higher heat conductivity coefficient, but is expensive and unfavorable for 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. The graphite film with high heat conductivity coefficient obtained by carbonizing and graphitizing the high-orientation Polyimide (PI) film serving as a precursor is a main direction of the artificial high-heat-conductivity graphite film. The heat conductivity coefficient of the high heat conductivity graphite film is 700-1900W/mK, which is much higher than the heat conductivity of copper (380W/mK) and aluminum (200W/mK), and the density of the artificial high heat conductive graphite film is about 1.0-2.0 g/cm 3 And is also much lower than the metals copper and aluminum. In addition, the artificial high-heat-conductivity graphite film with high heat conductivity and light weight can meet various special design requirements of electronic products in high integration, high density and light weight, has a market scale of over one hundred billion and has a wide application prospect.
The manufacturers of the artificial high-heat-conductivity graphite film mainly take foreign enterprises (such as DuPont, korean SKC, japanese Kaneka and the like) as main raw materials, and the technical level of domestic graphite film products and imported films still have a large gap, and the main reasons are that: (1) Polyimide (PI) has low in-plane orientation (less than 25%) and high thermal expansion coefficient (40 to 55X 10) -6 /K), resulting in lower interlayer thermal conductivity and overall thermal conductivity of the graphite film; (2) The graphitization process of the graphite film is complicated, the temperature rise is slow and the energy consumption is high, so that the uniformity of the graphite film is poor, defects are many, and the like, so that the thermal conductivity of the film is low. At present, carbonization and graphitization treatment of polyimide films for artificial high-heat-conductivity graphite films at home and abroad have accumulated a certain theoretical basis, and an industrial production technology of carbonization and graphitization of oriented polyimide films is formed. In addition, the graphite material has anisotropic performance due to the special lamellar 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 thermal conductivity between layers is a research hot spot of current researchers.
The heat treatment technology of the polyimide film is key to preparing the high-heat-conductivity graphite film. The traditional heat treatment process needs to be carried out under the protection of vacuum or inert atmosphere, and mainly comprises the following three steps: (1) 550-600 ℃ heat treatment, wherein oxygen atoms are heated to CO and CO 2 Form escape; (2) Carbonizing a high-temperature PI film (1000-1500 ℃), wherein the process is N, H element and N 2 、H 2 And CH (CH) 4 The first two processes mainly proceed heteroatom abstraction; (3) High temperature graphitization treatment (2500-3000 deg.c) to make hetero atom almostAfter the carbon is removed, rearrangement occurs, and the hexagonal carbon network structure grows from disorder to regularity, so that the graphite film is obtained to improve the heat conducting property. However, the conventional heat treatment technology (particularly the high-temperature graphitization treatment in the third step) generally has the problems of slow heating rate (10-50 ℃/min) and long heat treatment time (5-10 h), so that the defects of high energy consumption, long time consumption, high cost and the like are caused, and a series of side reactions (poor uniformity, defects and the like) are easily caused in the long-time heating process, so that the defects of low axial heat conductivity after film formation and the like are caused, so that the further development and application of the high-heat-conductivity graphite film material are greatly limited, and therefore, the selection of a proper heat treatment process is important.
Disclosure of Invention
First, the technical problem to be solved
The preparation method of the artificial high-heat-conductivity ultrathin graphite film can solve the technical problems mentioned above.
(II) technical scheme
Aiming at the problems of the background technology, the invention aims to provide a preparation method of an artificial high-heat-conductivity ultrathin graphite film, and the technical scheme adopted by the invention is as follows:
the preparation method of the artificial high-heat-conductivity ultrathin graphite film comprises the following steps of:
(1) Carrying out 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 with the temperature rising rate of 10 percent 3 ～10 4 The temperature of heat treatment is 2500-3500 ℃ at the temperature of/min, 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 and are of rectangular structures, open grooves are symmetrically formed in the end parts of the heat treatment modules, and the feeding rollers are symmetrically arranged in the open grooves through bearings;
the heat treatment module comprises a shell frame, a heating unit, a compressing unit, an electrifying unit and an electricity receiving frame, wherein the shell frame is of a rectangular hollow structure, the heating unit is symmetrically installed in the middle of the shell frame, the compressing unit is installed between the middle of the outer side of the heating unit and the shell frame, the electrifying unit is symmetrically installed on the inner side wall of the shell frame, the electrifying unit is connected with the end part of the heating unit, the electricity receiving frame is symmetrically installed in the middle of the outer side of the shell frame, and the electricity receiving frame is electrically connected with the electrifying unit.
The preparation of the high-heat-conductivity ultrathin graphite film by adopting the rapid high-temperature heat treatment device comprises the following steps:
s1, enabling a carbonized polyimide PI film to enter the heat treatment module through a feeding roller, and enabling the carbonized polyimide PI film to pass through the heat treatment module under the action of a tractor;
s2, the compression unit drives the heating unit to be tightly attached to the carbonized polyimide PI film, the heating area of the heating unit is uniform, the heating rate and uniformity of the carbonized polyimide PI film are effectively improved, meanwhile, the compression unit can be adaptively adjusted according to the size of the carbonized polyimide PI film, and further the carbonized polyimide PI film with different sizes can be processed;
s3, the power-on frame drives the power-on unit to conduct power-on, the power-on unit adopts the Joule heat principle, and the power-on unit after power-on is quickly heated to form a height Wen Wenou to realize graphitization treatment of the carbonized film.
Preferably, the polyimide PI film has a thickness of 20 to 100 μm.
Preferably, the polyimide PI film is internally filled with nanoparticle filler.
Preferably, the heating carbon strip is made of flexible heat-conducting materials, and the heating carbon strip is one or more of carbon felt and carbon fiber cloth.
Preferably, the heating unit comprises a guide frame, a sliding block, a connecting spring and heating carbon strips, wherein the guide frame is uniformly arranged in the shell frame, a sliding groove is formed in the middle of the guide frame, the sliding block is connected in the sliding groove in a sliding fit mode, the connecting spring is arranged between the outer side of the sliding block and the sliding groove, and the heating carbon strips are arranged between the adjacent sliding blocks.
Preferably, the compressing unit comprises an electric push rod, a fixed pressing plate, a movable pressing plate and a telescopic rod, wherein the electric push rod is uniformly arranged in 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 arranged 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 clung to the heating carbon strips.
Preferably, the power-on unit comprises a transverse plate, electric sliding blocks, a moving plate, power-on components and a pinch roller, wherein the transverse plate is symmetrically arranged in the shell frame, the electric sliding blocks are arranged on the transverse plate, the moving plate is arranged between the outer sides of the electric sliding blocks, the power-on components are arranged in the middle of the moving plate, the pinch roller is symmetrically arranged on the moving plate, a guide groove is formed between the pinch roller and the power-on components, and the heating carbon strip is arranged in the guide groove.
Preferably, the circular telegram subassembly includes link, pressure strip, baffle, guide bar, briquetting, extension spring and iron sheet, install the link between the movable plate, the link middle part is hollow structure, and the symmetry is installed logical groove on the link, is connected with the pressure strip through sliding fit's mode in the logical inslot, and link mid-mounting has the baffle, and the baffle middle part is provided with the through-hole, is connected with the guide bar through sliding fit's mode in the through-hole, and the briquetting is installed to guide bar one end, and the briquetting is trapezium structure, and the briquetting lateral surface is hugged closely with the pressure strip, is provided with extension spring on the guide bar between baffle and the briquetting, and the guide bar other end outside is provided with the power-on coil, and link internally mounted has the iron sheet.
Preferably, the upper end face of the pressing plate is an arc-shaped face, the pressing plate is made of conductive materials, the pressing plate is electrically connected with the power receiving frame, and conductive copper sheets are uniformly arranged on the inner concave face of the pressing plate.
(III) beneficial effects
1. The rapid high-temperature heat treatment device provided by the invention can rapidly reach ultra-high temperature (3000 ℃ in 1 min), and is beneficial to improving the crystallinity of graphite, so that the heat conducting property of the graphite is improved.
2. The rapid high-temperature heat treatment device provided by the invention effectively improves the condition of nonuniform temperature areas of the traditional heat treatment technology, the carbonized polyimide PI film is in direct contact with the heating carbon strips, the heating areas are uniform, and the temperature rising rate and uniformity of the carbonized polyimide PI film can be effectively improved.
3. The rapid high-temperature heat treatment device provided by the invention is beneficial to reducing defects of the graphite film, improving the crystallinity of the graphite film and optimizing the interlayer spacing of the graphite film, so that the plane and radial heat conductivity of the graphite film are improved.
4. The rapid high-temperature heat treatment device provided by the invention can simplify the production process, reduce the energy consumption, be beneficial to improving the production efficiency and reduce the time and the labor cost.
5. The length and the shape of the heating carbon strip can be designed according to the heated carbonized polyimide PI film, and the length of the heating carbon strip can be changed to adapt to the carbonized polyimide PI films with different sizes, so that the continuous preparation of the high-heat-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 meet the increasingly thin requirements and trends of consumer electronic products, and realizes the localization of the high-heat-conductivity graphite film.
Drawings
The invention will be further described with reference to the drawings and examples.
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 schematic view of the cut-away structure of the present application.
Fig. 5 is a schematic cross-sectional structure of the present application.
Fig. 6 is a schematic view of the partial cross-sectional structure of fig. 5 of the present application.
FIG. 7 is a schematic 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:
the preparation method of the artificial high-heat-conductivity ultrathin graphite film comprises the following steps of:
(1) Carrying out pyrolysis treatment on the polyimide PI film at 500-600 ℃;
(2) And (3) carbonizing the polyimide PI film subjected to pyrolysis treatment from room temperature to 1300 ℃ in a vacuum state, wherein the carbonization heating program is as follows: raising the temperature from room temperature to 600 ℃ at a heating rate of 20 ℃/min, and keeping the temperature for 1 h, and then continuously raising the temperature to 1300 ℃ according to the original heating rate;
(3) Graphitizing the carbonized polyimide PI film, wherein the graphitizing treatment process adopts a rapid high-temperature heat treatment device, and the cooled carbonized polyimide PI film is transferred into the rapid high-temperature heat treatment device after vacuum carbonization, wherein the temperature rising rate of the rapid high-temperature heat treatment device is 10 3 ～10 4 Graphitization is carried out at the temperature of 2800 ℃ from room temperature under argon at the temperature of 1min, and the temperature is kept for 10 min.
The rapid high-temperature heat treatment device comprises a plurality of support frames 1, heat treatment modules 2 and feeding 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 of rectangular structures, open grooves are symmetrically formed in the end parts of the heat treatment modules 2, and the feeding rollers 3 are symmetrically arranged in the open grooves 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 electricity receiving 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 electricity receiving frame 25 is symmetrically arranged in the middle of the outer side of the shell frame 21, and the electricity receiving frame 25 is electrically connected with the electrifying unit 24.
The preparation of the high-heat-conductivity ultrathin graphite film by adopting the rapid high-temperature heat treatment device comprises the following steps:
s1, enabling a carbonized polyimide PI film to enter the heat treatment module 2 through a feeding 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 compression unit 23 drives the heating unit 22 to be clung to the carbonized polyimide PI film, the heating area of the heating unit 22 is uniform, the heating rate and uniformity of the carbonized polyimide PI film are effectively improved, meanwhile, the compression unit 23 can be adaptively adjusted according to the size of the carbonized polyimide PI film, and further the carbonized polyimide PI film with different sizes can be processed;
s3, the power-on frame 25 drives the power-on unit 24 to conduct power-on, the power-on unit 24 adopts the Joule heat principle, and the power-on unit 24 after power-on is quickly heated to form a height Wen Wenou to realize graphitization treatment of the carbonized film.
The polyimide PI film thickness is 20-100 mu m.
The polyimide PI film is internally filled with nano particle filler, the nano particle filler is added in the PI film preparation process, and the content of the nano particle filler can be 0.01% -20% of one or more combinations.
The nanoparticle filler can be one or a combination of a plurality of carbon materials, metal simple substances or alloy materials and inorganic nonmetallic materials. 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 nonmetallic 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, sliding blocks 222, connecting springs 223 and heating carbon strips 224, wherein the guide frame 221 is uniformly arranged in the shell frame 21, a sliding groove is formed in the middle of the guide frame 221, the sliding blocks 222 are connected in the sliding groove in a sliding fit mode, the connecting springs 223 are arranged between the outer sides of the sliding blocks 222 and the sliding grooves, and the heating carbon strips 224 are arranged between the adjacent sliding blocks 222.
The heating carbon strips 224 are made of flexible heat-conducting materials, the heating carbon strips 224 are one or more of carbon felts and carbon fiber cloths, and the carbon felts are one or more of polyacrylonitrile-based carbon felts, asphalt-based carbon felts or adhesive-based carbon felts.
As known from the joule's theorem, the amount of heat generated by a current passing through a conductor is proportional to the square of the current intensity, inversely proportional to the resistance of the conductor, and proportional to the time of energization, and when a current passes through the heated carbon strip 224, the heated carbon strip 224 rapidly generates a large amount of heat. The heating rate can be adjusted by adjusting the current, and the heating rate can reach 10 3 ～10 4 The temperature reduction rate is up to 10 ℃ per minute 4 The temperature/min can effectively reduce the energy consumption.
The compressing unit 23 comprises an electric push rod 231, a fixed pressing plate 232, a movable pressing plate 233 and a telescopic rod, wherein the electric push rod 231 is uniformly arranged in the shell frame 21, the fixed pressing plate 232 is connected to the top end of the electric push rod 231 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 telescopic rod is uniformly arranged between the movable pressing plate 233 and the fixed pressing plate 232, and the inner side faces of the movable pressing plate 233 and the fixed pressing plate 232 are tightly attached to the heating carbon strips 224.
The electrifying unit 24 comprises a transverse plate 241, electric sliding blocks 242, a moving plate 243, electrifying components 244 and pressing rollers 245, wherein the transverse plate 241 is symmetrically arranged in the shell frame 21, the electric sliding blocks 242 are arranged on the transverse plate 241, the moving plate 243 is arranged between the outer sides of the electric sliding blocks 242, the electrifying components 244 are arranged in the middle of the moving plate 243, the pressing rollers 245 are symmetrically arranged on the moving plate 243, guide grooves are formed between the pressing rollers 245 and the electrifying components 244, and the heating carbon strips 224 are positioned in the guide grooves.
The power-on 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, wherein the connecting frame 2441 is installed between the moving plates 243, the middle part 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 part of the connecting frame 2441, a through hole is formed in the middle part of the partition 2443, the guide rod 2444 is connected in the through hole in a sliding fit mode, one end of the guide rod 2444 is provided with the pressing block 2445, the outer side surface 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, the power-on coil is arranged on the outer side of the other end of the guide rod 2444, and the iron sheet 2447 is installed in 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 conductive materials, the pressing plate 2442 is electrically connected with the power connection frame 25, conductive copper sheets are uniformly arranged on the concave face in the pressing plate 2442, the contact efficiency between the conductive copper sheets and the heating carbon strips 224 can be effectively increased, and poor conduction is avoided.
Comparative example 1:
in the comparative example, a traditional graphite film preparation process is adopted, and the polyimide PI film prepared is carbonized from room temperature to 1300 ℃ in a vacuum state, and the carbonization temperature-raising program is as follows: raising the temperature from room temperature to 600 ℃ at a heating rate of 20 ℃/min, and keeping the temperature for 1 h, and then continuously raising the temperature to 1300 ℃ according to the original heating rate; transferring the cooled carbonized polyimide PI film into a graphite furnace after carbonization, and heating to 2800 ℃ from room temperature under argon to graphitize, wherein the graphitization heating program is as follows: the carbonized polyimide PI film is heated to 1600 ℃ from room temperature at a heating rate of 20 ℃/min, and is heated to 2800 ℃ at the original rate after heat preservation of 5 h.
Example 2:
in this example, a graphite film was prepared by a rapid thermal treatment technique, and after the vacuum carbonization in example 1 was completed, the cooled carbonized polyimide PI film was transferred to a heated carbon strip 224, and graphitized by heating from room temperature to 2800 ℃ under argon for a heating time of 1min, and then heat was preserved for 20 min.
Example 3:
in this example, a graphite film was prepared by a rapid thermal treatment technique, and after the vacuum carbonization in example 1 was completed, the cooled carbonized polyimide PI film was transferred to a heated carbon strip 224, and graphitized by heating from room temperature to 2800 ℃ under argon for a heating time of 1min, and then heat was preserved for 30 min.
Example 4:
in this example, a graphite film was prepared by a rapid thermal treatment technique, and after the vacuum carbonization in example 1 was completed, the cooled carbonized polyimide PI film was transferred to a heated carbon strip 224, and graphitized by heating from room temperature to 3000 ℃ under argon for 1min, and then heat was preserved for 20 min.
Example 5:
in the embodiment, a graphite film is prepared by adopting a rapid high-temperature heat treatment technology, and a polyimide PI film containing 2% of carbon quantum dots is carbonized from room temperature to 1300 ℃ in a vacuum state, wherein the carbonization temperature-raising program is as follows: raising the temperature from room temperature to 600 ℃ at a heating rate of 20 ℃/min, and keeping the temperature for 1 h, and then continuously raising the temperature to 1300 ℃ according to the original heating rate; after the vacuum carbonization is completed, the cooled carbonized polyimide PI film is transferred to a heating carbon strip 224, and graphitized is carried out by heating from room temperature to 2800 ℃ under argon, wherein the heating time is 1min, and the temperature is kept for 20 min.
Comparative example 2:
in the comparative example, a traditional graphite film preparation process is adopted, and a polyimide PI film containing 2% of carbon quantum dots is carbonized in a vacuum state from room temperature to 1300 ℃, and the carbonization temperature-rise program is as follows: raising the temperature from room temperature to 600 ℃ at a heating rate of 20 ℃/min, and keeping the temperature for 1 h, and then continuously raising the temperature to 1300 ℃ according to the original heating rate; transferring the cooled carbonized film into a graphite furnace after carbonization is completed, and heating the cooled carbonized film to 2800 ℃ from room temperature under argon to graphitize, wherein the graphitization heating program is as follows: the carbonized polyimide PI film is heated to 1600 ℃ from room temperature at a heating rate of 20 ℃/min, and is heated to 2800 ℃ at the original rate after heat preservation of 5 h.
Example 6:
in this example, a graphite film was prepared by a rapid thermal treatment technique, and after the vacuum carbonization in example 2 was completed, the cooled carbonized polyimide PI film was transferred to a heated carbon strip 224, and graphitized by heating from room temperature to 3000 ℃ under nitrogen for a heating time of 1min and heat preservation for 20 min.
TABLE 1
| Thickness of (L) | Planar thermal conductivity | Radial thermal conductivity | |
| Comparative example 1 | 40 μm | 1100 W/m·K | 380 W/m·K |
| Example 1 | 40 μm | 1400 W/m·K | 500 W/m·K |
| Example 2 | 40 μm | 1480 W/m·K | 580 W/m·K |
| Example 3 | 40 μm | 1550 W/m·K | 600 W/m·K |
| Example 4 | 40 μm | 1580 W/m·K | 620 W/m·K |
| Comparative example 2 | 50 μm | 1200 W/m·K | 450 W/m·K |
| Example 5 | 50 μm | 1680 W/m·K | 750 W/m·K |
| Example 6 | 50 μm | 1800 W/m·K | 800 W/m·K |
Claims (5)
1. A preparation method of an artificial high-heat-conductivity ultrathin graphite film is characterized in that,
(1) Carrying out 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 with the temperature rising rate of 10 percent 3 ～10 4 The temperature of heat treatment is 2500-3500 ℃ at the temperature of/min, 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 feeding 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 of rectangular structures, open grooves are symmetrically formed in the end parts of the heat treatment modules (2), and the feeding rollers (3) are symmetrically arranged in the open grooves through bearings;
the heat treatment module (2) comprises a shell frame (21), a heating unit (22), a compressing unit (23), an electrifying unit (24) and an electric connection 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 compressing 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 electric connection frame (25) is symmetrically arranged in the middle of the outer side of the shell frame (21), and the electric connection frame (25) is electrically connected with the electrifying unit (24);
the heating unit (22) comprises a guide frame (221), sliding blocks (222), connecting springs (223) and heating carbon strips (224), wherein the guide frame (221) is uniformly arranged in the shell frame (21), sliding grooves are formed in the middle of the guide frame (221), the sliding blocks (222) are connected in the sliding grooves in a sliding fit mode, the connecting springs (223) are arranged between the outer sides of the sliding blocks (222) and the sliding grooves, and the heating carbon strips (224) are arranged between the adjacent sliding blocks (222);
the power-on unit (24) comprises a transverse plate (241), electric sliding blocks (242), moving plates (243), power-on components (244) and compression rollers (245), wherein the transverse plate (241) is symmetrically arranged in the shell frame (21), the electric sliding blocks (242) are arranged on the transverse plate (241), the moving plates (243) are arranged between the outer sides of the electric sliding blocks (242), the power-on components (244) are arranged in the middle of the moving plates (243), the compression rollers (245) are symmetrically arranged on the moving plates (243), guide grooves are formed between the compression rollers (245) and the power-on components (244), and the heating carbon strips (224) are arranged in the guide grooves;
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 iron sheets (2447), wherein the connecting frame (2441) is installed between the moving plates (243), the middle part 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 plate (2443) is installed in the middle of the connecting frame (2441), through holes are formed in the middle of the partition plate (2443), the guide rod (2444) is connected in the through holes 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 trapezoid structure, the outer side surface 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 plate (2443) and the pressing block (2445), a power-on coil is arranged on the outer side of the other end of the guide rod (2444), and the inner part of the connecting frame (2441) is installed with the iron sheets (2447).
The preparation of the high-heat-conductivity ultrathin graphite film by adopting the rapid high-temperature heat treatment device comprises the following steps:
s1, enabling a carbonized polyimide PI film to enter the heat treatment module (2) through a feeding 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 compression 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, and meanwhile, the compression unit (23) can be adaptively adjusted according to the size of the carbonized polyimide PI film, so that the carbonized polyimide PI film with different sizes can be processed;
s3, the power-on frame (25) drives the power-on unit (24) to conduct electricity, the power-on unit (24) adopts a Joule heat principle, and the power-on unit (24) after power-on is quickly heated to realize graphitization treatment of the carbonized film.
2. The method for preparing the artificial high-thermal-conductivity ultrathin graphite film, as claimed in claim 1, is characterized in that: the polyimide PI film is internally filled with nanoparticle filler.
3. The method for preparing the artificial high-thermal-conductivity ultrathin graphite film, as claimed in claim 1, is characterized in that: 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 cloths.
4. The method for preparing the artificial high-thermal-conductivity ultrathin graphite film, as claimed in claim 1, is characterized in that: the compressing unit (23) comprises an electric push rod (231), a fixed pressing plate (232), a movable pressing plate (233) and a telescopic rod, wherein the electric push rod (231) is uniformly arranged 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 telescopic rod is uniformly arranged between the movable pressing plate (233) and the fixed pressing plate (232), and the inner side faces of the movable pressing plate (233) and the fixed pressing plate (232) are tightly attached to the heating carbon strips (224).
5. The method for preparing the artificial high-thermal-conductivity ultrathin graphite film, as claimed in claim 1, 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 conductive materials, the pressing plate (2442) is electrically connected with the power-on frame (25), and conductive copper sheets are uniformly arranged on the inner concave face of the pressing plate (2442).
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