CN110540752A - Filler orientation-reinforced high-thermal-conductivity polyimide composite film and preparation method thereof - Google Patents
Filler orientation-reinforced high-thermal-conductivity polyimide composite film and preparation method thereof Download PDFInfo
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- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
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- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
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- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C08K2003/385—Binary compounds of nitrogen with boron
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- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
Abstract
The invention discloses a filler orientation reinforced high heat conduction polyimide composite film and a preparation method thereof, wherein the film is prepared by extruding polyamide acid solution containing heat conduction fillers through a long and narrow die head channel with variable diameter, spreading a film, rolling and carrying out thermal imidization; the heat-conducting filler is formed by mixing more than two fillers with different morphologies, wherein the fillers at least comprise one flaky heat-conducting filler, and the mass ratio of the flaky heat-conducting filler to the non-flaky heat-conducting filler is 1: 0.5 to 2; the preparation method comprises the steps of dispersing the heat-conducting filler in a polar solvent, generating a polyamic acid solution through the polycondensation reaction of aromatic dianhydride and aromatic diamine, extruding and spreading the polyamic acid solution through a long and narrow and variable-diameter die head channel of an extruder, removing part of the solvent in the film, carrying out calendaring and thermal imidization treatment, and cooling to obtain the high-heat-conducting polyimide film. The film prepared by the method has high heat conductivity coefficient and low thermal expansion coefficient, has short film forming period, and is widely applied to the fields of microelectronic devices, electronic packaging and aerospace.
Description
Technical Field
The invention relates to the technical field of polyimide films, in particular to a filler orientation-reinforced high-thermal-conductivity polyimide composite film and a preparation method thereof.
Background
With the upgrading and upgrading of electronic products such as smart phones and notebook computers, and the miniaturization, light weight and high integration, the electronic products gradually become bright points. The lifetime and stability of these electronic products are also receiving increasing attention, and the factors affecting lifetime and stability are mainly the heat dissipation capability of the system. At present, a heat dissipation material with high heat conductivity is an important requirement in the electronic industry, and a material with a heat conduction function becomes a key technology for solving the heat dissipation problem of an electronic product. The polyimide film is one of the currently known polymer films with the highest temperature resistance level, and the molecular chain of the polyimide film has a stable aromatic heterocyclic structure, so that the polyimide film has the characteristics of excellent oxidation resistance stability, high temperature resistance, excellent mechanical properties, high carbon density and the like, which are difficult to realize by other polymers. However, the pure polyimide film has poor thermal conductivity and the thermal conductivity is only 0.19 W.m < -1 > K < -1 >, which greatly limits the application of the pure polyimide film, so the research and development and preparation of the polyimide film with high thermal conductivity are urgent needs for solving the heat dissipation problem of the electronic industry at present.
there are two main ways to improve the thermal conductivity of the polyimide film with low thermal conductivity: one is to obtain a special physical structure by changing the structure of material molecules and chain links in the process of material synthesis and molding processing, establish channels and networks favorable for phonon transmission in the polymer, and improve the heat-conducting property, for example, some special monomers are used or the film is highly stretched and oriented, but the preparation process is complicated, the difficulty is high, the cost is high, a certain distance is left from the industrial application, and the improvement range of the heat-conducting coefficient is limited. And the other is to prepare a heat-conducting composite film by adding a high-heat-conducting inorganic filler, and introduce the high-heat-conducting inorganic filler into a polyimide matrix to achieve the purpose of increasing heat conduction, wherein in patent CN 108384235A, one of boron nitride and aluminum oxide is used as a filler to prepare the polyimide film, and the adding amount is up to 30% -60%, so that the adding of the same heat-conducting filler has great limitation on the improvement of the heat-conducting property of the polyimide film, and the adding of the same heat-conducting filler cannot be simultaneously and obviously improved in the in-plane direction and the out-of-plane direction of the film. Patent CN 105111739 a discloses a preparation method of a polyimide film with high thermal conductivity, in which nano-alumina, carbon black powder, iron oxide and the like are used as fillers to achieve the purpose of improving the thermal conductivity, but the fillers are independent from each other and have no synergistic effect, and the thermal conductivity of the film is not significantly improved.
The invention adds more than two fillers with different shapes into a polar solvent, mixes at least one heat-conducting filler with a sheet structure, and carries out polycondensation reaction on aromatic dianhydride and aromatic diamine in the polar solvent to generate polyamic acid, and the polyamic acid is further thermally imidized after passing through a flow channel to obtain the polyimide composite film with high heat conductivity. When the flaky fillers pass through the long and narrow flow channel, the flaky fillers are subjected to shearing action and oriented in the plane of the film, so that the in-plane high thermal conductivity is obtained, meanwhile, other non-flaky fillers form thermal conduction connection among the flaky fillers, and the thermal conduction connection is further enhanced through the calendering action, so that a thermal conduction network is perfected in the thickness direction, and the high out-plane thermal conductivity is obtained.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a filler orientation-reinforced high-thermal-conductivity polyimide composite film and a preparation method thereof.
The technical scheme for realizing the purpose of the invention is as follows:
A high heat conduction polyimide composite film with reinforced filler orientation is prepared by extruding polyamide acid solution containing heat conduction filler through a long and narrow die head channel with gradually changed cross section area, spreading a film, rolling and performing thermal imidization; the heat-conducting filler is formed by mixing more than two fillers with different morphologies, wherein the fillers at least comprise one flaky heat-conducting filler, and the mass ratio of the flaky heat-conducting filler to the non-flaky heat-conducting filler is 1: 0.5-2.
the heat-conducting filler is at least two of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, iron oxide, silicon carbide, copper particles, silver particles, carbon nano tubes, graphene, flaky carbon powder and graphite, and at least comprises one flaky heat-conducting filler.
the thickness of the film is 25-150um, and the solid content is 15% -30%.
a preparation method of a filler orientation reinforced high-thermal-conductivity polyimide composite film comprises the following steps:
(1) Mixing more than two heat-conducting fillers with different morphologies, wherein the heat-conducting fillers at least comprise one flaky heat-conducting filler, adding a polar solvent containing a dispersing agent, uniformly dispersing, and then adding aromatic diamine to completely dissolve the aromatic diamine in the solvent to obtain a uniformly mixed system;
(2) Adding aromatic dianhydride into the mixed system obtained in the step (1) in batches, stirring for full reaction after adding the aromatic dianhydride, and defoaming to obtain a polyamic acid solution;
(3) Adding the defoamed polyamic acid solution into a feed hopper, extruding and spreading a film through a long and narrow die head channel with gradually changed cross-sectional area, removing part of solvent in the film to obtain a polyamic acid gel film with certain self-supporting property, obtaining a glue film with preset thickness through a calender, performing thermal imidization treatment, allowing the flaky filler to be subjected to shearing action to be oriented in the plane of the film when passing through the die head channel, forming heat conduction connection between the flaky fillers by the non-flaky filler, and cooling to obtain the high-heat-conductivity polyimide film.
the aromatic dianhydride is one or more of pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride, 4,4' -oxydiphthalic anhydride, 3 ', 4,4' -biphenyl tetracarboxylic dianhydride and bisphenol A dianhydride.
the aromatic diamine is one or more of diaminodiphenyl ether (ODA), p-phenylenediamine (p-PDA) and TAB.
The polar solvent is one of N, N-Dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP).
a die head for preparing a filler orientation-enhanced high-thermal-conductivity polyimide composite film is provided with a long and narrow die head channel with gradually changed cross-sectional area.
The cross section of the die head channel is rectangular, and the cross section area is gradually reduced along the extrusion direction.
The invention provides a filler orientation reinforced high-thermal conductivity polyimide composite film and a preparation method thereof, wherein the preparation principle of the film is as follows: the heat-conducting filler is effectively dispersed in a polar solvent, polyamide acid is generated through the polycondensation reaction of aromatic dianhydride and aromatic diamine, the polyamide acid solution is extruded through a section of long and narrow extrusion channel and a rectangular section die head, and the sheet heat-conducting filler is subjected to shearing action to generate film in-plane orientation when passing through a long and narrow flow channel, so that in-plane high heat conductivity is obtained; other non-flaky fillers form heat conduction connection among the flaky fillers, and the heat conduction connection is further enhanced through the calendering effect, so that a more compact heat conduction network is formed in the thickness direction of the film, high out-of-plane heat conduction is obtained, namely, the heat conduction in the plane of the film is enhanced through the orientation of the flaky fillers, and the heat conduction in the thickness direction of the film is enhanced through the cooperation of the non-flaky heat conduction fillers, so that the high heat conduction polyimide composite film is prepared.
the invention has the beneficial effects that:
(1) The heat-conducting fillers with different shapes are adopted, one of the heat-conducting fillers is limited to be a flaky filler, and an uninterrupted heat-conducting network is formed by the mutual contact of the flaky heat-conducting filler and the non-flaky heat-conducting filler, so that the heat-conducting property of the film is effectively improved;
(2) the method adopts a slender and variable-diameter die head, when PAA flows through a die head channel, the flaky fillers are subjected to shearing action to generate orientation in the plane of the film when passing through a long and narrow flow channel, so that in-plane high thermal conductivity is obtained, meanwhile, other non-flaky fillers form thermal conductivity connection among the flaky fillers, and the thermal conductivity connection is further increased through the calendering action, so that a good thermal conductivity network is formed in the thickness direction, high out-of-plane thermal conductivity is obtained, the overall thermal conductivity of the film is improved, and the thermal expansion coefficient of the film is reduced.
drawings
FIG. 1 is a schematic view of a process for producing a polyimide film;
FIG. 2 is a schematic structural view of a filler in a cross section of a film;
FIG. 3 is a schematic view of a die channel;
Fig. 1 and 3 show a schematic diagram of the process equipment flow and die channel for making thin films.
Detailed Description
The invention is further described below by way of examples, but is not limited thereto.
As shown in fig. 3, a die for preparing a filler orientation-reinforced high thermal conductivity polyimide composite film is provided with a long and narrow die channel with gradually changed cross-sectional area.
The cross section of the die head channel is rectangular, and the cross section area is gradually reduced along the extrusion direction.
the composite films of the following examples were prepared by the process shown in fig. 1, and the cross-sectional structure of the prepared composite films is shown in fig. 2.
Example 1
The embodiment provides a filler orientation-reinforced high-thermal-conductivity polyimide composite film, which is prepared from the following raw materials in parts by mass: 10 parts of heat-conducting filler, 2 parts of dispersant, 50 parts of aromatic dianhydride, 45 parts of aromatic diamine and 400 parts of DMAC; wherein the heat-conducting filler is a mixture of spherical alumina and flaky boron nitride, and the mass ratio of the alumina to the boron nitride is 1: 1; the aromatic dianhydride is pyromellitic dianhydride (PMDA), and the aromatic diamine is diaminodiphenyl ether (ODA); the preparation method of the film comprises the following steps:
(1) Dispersing 10 parts by mass of spherical alumina and flaky boron nitride mixed filler in 400 parts by mass of DMAC (dimethylacetamide) containing 2 parts by mass of polyvinylpyrrolidone (PVP) and carrying out ultrasonic treatment for 2 hours, then adding 45 parts by mass of ODA, and mechanically stirring until the ODA is completely dissolved in a solvent to obtain a uniform mixed system;
(2) Sequentially adding 50 parts by mass of PMDA into the mixed system prepared in the step (1) for 3 times, after all the PMDA are added, mechanically stirring and reacting for 4 hours, standing for 1 hour, and performing self defoaming to obtain a polyamic acid solution;
(3) Adding the defoamed polyamic acid solution into a feed hopper, extruding the polyamic acid solution through a long and narrow extruder die head channel with gradually reduced cross-sectional area, controlling the thickness of a film by using a scraper, so that the polyamic acid solution forms a film on a steel belt, heating to remove part of a solvent in the film, obtaining a PAA gel film with certain self-supporting property, obtaining a glue film with a preset thickness by using a calender, performing thermal imidization by using a heating process according to the gradient of 80 ℃/1h + 100 ℃/1h + 150 ℃/40min + 230 ℃/1h + 300 ℃/1h + 350 ℃/0.5h, and naturally cooling after imidization is completed to obtain the high-thermal conductivity polyimide film.
According to test detection, the polyimide film prepared in the embodiment has the in-plane thermal conductivity coefficient of 3.06 W.m < -1 >. K < -1 > and the out-of-plane thermal conductivity coefficient of 0.65 W.m < -1 >. K < -1 >.
Example 2
The embodiment provides a filler orientation-reinforced high-thermal-conductivity polyimide composite film, which is prepared from the following raw materials in parts by mass: 12 parts of heat-conducting filler, 3 parts of dispersing agent, 75 parts of aromatic dianhydride, 45 parts of aromatic diamine and 400 parts of polar solvent; wherein the filler is a mixture of spherical alumina and flaky boron nitride, and the mass ratio of the alumina to the boron nitride is 1: 1; the aromatic dianhydride is Benzophenone Tetracarboxylic Dianhydride (BTDA), and the aromatic diamine is diaminodiphenyl ether (ODA); the preparation method of the film comprises the following steps:
(1) Dispersing 12 parts by mass of spherical alumina and flaky boron nitride mixed filler in 400 parts by mass of DMAC (dimethylacetamide) containing 3 parts by mass of scorotuocilok 7117w, carrying out ultrasonic treatment for 2 hours, adding 45 parts by mass of ODA, and mechanically stirring until the ODA is completely dissolved in a solvent to obtain a uniform mixed system;
(2) Sequentially adding 75 parts by mass of BTDA into the mixed system prepared in the step (1) for 3 times, after all BTDA are added, mechanically stirring and reacting for 4 hours, standing for 1 hour, and performing self-defoaming to obtain a polyamic acid solution;
(3) Adding the defoamed polyamic acid solution into a feed hopper, extruding the polyamic acid solution through a long and narrow extruder die head channel with gradually reduced cross-sectional area, controlling the thickness of a film by using a scraper, so that the polyamic acid solution forms a film on a steel belt, heating to remove part of a solvent in the film, obtaining a PAA gel film with certain self-supporting property, obtaining a glue film with a preset thickness by using a calender, performing thermal imidization by using a heating process according to the gradient of 80 ℃/1h + 100 ℃/1h + 150 ℃/1h + 230 ℃/1h + 300 ℃/1h + 350 ℃/0.5h, and naturally cooling after imidization is completed to obtain the high-thermal conductivity polyimide film.
according to test detection, the polyimide film prepared in the embodiment has the in-plane thermal conductivity coefficient of 2.85 W.m < -1 >. K < -1 > and the out-of-plane thermal conductivity coefficient of 0.73 W.m < -1 >. K < -1 >.
Example 3
The embodiment provides a filler orientation-reinforced high-thermal-conductivity polyimide composite film, which is prepared from the following raw materials in parts by mass: 12 parts of heat-conducting filler, 3 parts of dispersant, 60 parts of aromatic dianhydride, 46 parts of aromatic diamine and 430 parts of polar solvent; wherein the filler is a mixture of flaky aluminum nitride and spherical alumina, and the mass ratio of the aluminum nitride to the alumina is 1: 1; the aromatic dianhydride is pyromellitic dianhydride (PMDA), the aromatic diamine is diaminodiphenyl ether (ODA) and p-phenylenediamine (p-PDA), and the molar ratio of ODA to PDA is 7: 3; the preparation method of the film comprises the following steps:
(1) dispersing 12 parts by mass of flaky aluminum nitride and spherical alumina mixed filler in 430 parts by mass of DMAC (dimethylacetamide) containing 3 parts by mass of PVP (polyvinyl pyrrolidone) dispersant, carrying out ultrasonic treatment for 2 hours, adding 46 parts by mass of ODA and PDA mixture, and mechanically stirring until the ODA and the PDA are completely dissolved in a solvent to obtain a uniform mixed system;
(2) Sequentially adding 60 parts by mass of PMDA into the mixed system prepared in the step (1) for 3 times, after all the PMDA are added, mechanically stirring and reacting for 4 hours, standing for 1 hour, and performing self defoaming to obtain a polyamic acid solution;
(3) adding the defoamed polyamic acid solution into a feed hopper, extruding the polyamic acid solution through a long and narrow extruder die head channel with gradually reduced cross-sectional area, controlling the thickness of a film by using a scraper, so that the polyamic acid solution forms a film on a steel belt, heating to remove part of a solvent in the film, obtaining a PAA gel film with certain self-supporting property, obtaining a glue film with a preset thickness by using a calender, performing thermal imidization by using a heating process according to the gradient of 80 ℃/1h + 100 ℃/1h + 150 ℃/40min + 230 ℃/1h + 300 ℃/1h + 350 ℃/0.5h, and naturally cooling after imidization is completed to obtain the high-thermal conductivity polyimide film.
according to test detection, the polyimide film prepared in the embodiment has the in-plane thermal conductivity coefficient of 3.19 W.m < -1 > K < -1 > and the out-of-plane thermal conductivity coefficient of 0.84 W.m < -1 > K < -1 >.
Example 4
the embodiment provides a filler orientation-reinforced high-thermal-conductivity polyimide composite film, which is prepared from the following raw materials in parts by mass: 22 parts of heat-conducting filler, 5 parts of dispersing agent, 80 parts of aromatic dianhydride, 45 parts of aromatic diamine and 550 parts of polar solvent; wherein the filler is a mixture of tetrapod-shaped zinc oxide and flaky boron nitride, and the mass ratio of the zinc oxide to the boron nitride is 1: 1; the aromatic dianhydride is Benzophenone Tetracarboxylic Dianhydride (BTDA), the aromatic diamine is diaminodiphenyl ether (ODA) and p-phenylenediamine (p-PDA), and the mol ratio of ODA to PDA is 3: 7; the preparation method of the film comprises the following steps:
(1) Dispersing 22 parts by mass of a tetrapod-like zinc oxide and flaky boron nitride mixed filler in 550 parts by mass of NMP containing 5 parts by mass of siloco silok 7117w, performing ultrasonic treatment for 2 hours, adding 45 parts by mass of a mixture of ODA and PDA, and mechanically stirring until the ODA and the PDA are completely dissolved in a solvent;
(2) sequentially adding 80 parts by mass of PMDA into the mixed system prepared in the step (1) for 3 times, after all the PMDA are added, mechanically stirring and reacting for 4 hours, standing for 1 hour, and performing self defoaming to obtain a polyamic acid solution;
(3) Adding the defoamed polyamic acid solution into a feed hopper, extruding the polyamic acid solution through a long and narrow extruder die head channel with gradually reduced cross-sectional area, controlling the thickness of a film by using a scraper, so that the polyamic acid solution forms a film on a steel belt, heating to remove part of a solvent in the film, obtaining a PAA gel film with certain self-supporting property, obtaining a glue film with a preset thickness by using a calender, performing thermal imidization by using a heating process according to the gradient of 80 ℃/1h + 100 ℃/1h + 150 ℃/40min + 230 ℃/1h + 300 ℃/1h + 350 ℃/0.5h, and naturally cooling after imidization is completed to obtain the high-thermal conductivity polyimide film.
according to test detection, the polyimide film prepared in the embodiment has the in-plane thermal conductivity coefficient of 3.45 W.m < -1 >. K < -1 > and the out-of-plane thermal conductivity coefficient of 0.64 W.m < -1 >. K < -1 >.
Example 5
the embodiment provides a filler orientation-reinforced high-thermal-conductivity polyimide composite film, which is prepared from the following raw materials in parts by mass: 22 parts of heat-conducting filler, 5 parts of dispersing agent, 60 parts of aromatic dianhydride, 46 parts of aromatic diamine and 430 parts of polar solvent; wherein the filler is a mixture of flaky aluminum nitride, spherical alumina and flaky boron nitride, and the mass ratio of the aluminum nitride to the alumina to the boron nitride is 0.5: 2: 0.5; the aromatic dianhydride is pyromellitic dianhydride (PMDA), the aromatic diamine is diaminodiphenyl ether (ODA) and p-phenylenediamine (p-PDA), and the molar ratio of ODA to p-PDA is 7: 3; the preparation method of the film comprises the following steps:
(1) Dispersing 22 parts by mass of a mixed filler of flake aluminum nitride, spherical aluminum oxide and flake boron nitride in 430 parts by mass of NMP containing 5 parts by mass of PVP for 2 hours by ultrasonic treatment, adding 46 parts by mass of a mixture of ODA and p-PDA, and mechanically stirring until the ODA and the PDA are completely dissolved in a solvent to obtain a uniform mixed system;
(2) Sequentially adding 60 parts by mass of PMDA into the system for 3 times, after all the PMDA is added, mechanically stirring and reacting for 4 hours, standing for 1 hour, and performing self-defoaming to obtain a polyamic acid solution;
(3) Adding the defoamed polyamic acid solution into a feed hopper, extruding the polyamic acid solution through a long and narrow extruder die head channel with gradually reduced cross-sectional area, controlling the thickness of a film by using a scraper, so that the polyamic acid solution forms a film on a steel belt, heating to remove part of a solvent in the film, obtaining a PAA gel film with certain self-supporting property, obtaining a glue film with a preset thickness by using a calender, performing thermal imidization by using a heating process according to the gradient of 80 ℃/1h + 100 ℃/1h + 150 ℃/40min + 230 ℃/1h + 300 ℃/1h + 350 ℃/0.5h, and naturally cooling after imidization is completed to obtain the high-thermal conductivity polyimide film.
According to test detection, the polyimide film prepared in the embodiment has the in-plane thermal conductivity coefficient of 4.05 W.m < -1 > K < -1 > and the out-of-plane thermal conductivity coefficient of 0.97 W.m < -1 > K < -1 >.
Claims (9)
1. a high heat conduction polyimide composite film with reinforced filler orientation is characterized in that the film is prepared by extruding, film paving, rolling and thermal imidization of polyamide acid solution containing heat conduction filler through a long and narrow die head channel with gradually changed cross section area; the heat-conducting filler is formed by mixing more than two fillers with different morphologies, wherein the fillers at least comprise one flaky heat-conducting filler, and the mass ratio of the flaky heat-conducting filler to the non-flaky heat-conducting filler is 1: 0.5-2.
2. The filler orientation-enhanced high thermal conductivity polyimide composite film according to claim 1, wherein the film thickness is 25-150um, and the solid content of the polyamic acid solution is 15% -30%.
3. The filler-oriented reinforced high-thermal-conductivity polyimide composite film according to claim 1, wherein the thermal-conductivity filler is at least two of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, iron oxide, silicon carbide, copper particles, silver particles, carbon nanotubes, graphene, flaky carbon powder and graphite, and at least comprises one flaky thermal-conductivity filler.
4. a preparation method of a filler orientation reinforced high-thermal-conductivity polyimide composite film is characterized by comprising the following steps:
(1) Mixing more than two heat-conducting fillers with different morphologies, wherein the heat-conducting fillers at least comprise one flaky heat-conducting filler, adding a polar solvent containing a dispersing agent for uniform dispersion, and then adding aromatic diamine to completely dissolve the aromatic diamine in the solvent to obtain a uniform mixed system;
(2) adding aromatic dianhydride into the mixed system obtained in the step (1) in batches, stirring for full reaction after adding the aromatic dianhydride, and defoaming to obtain a polyamic acid solution;
(3) Adding the defoamed polyamic acid solution into a feed hopper, extruding and spreading a film through a long and narrow extruder die head channel with gradually changed cross-sectional area, removing part of solvent in the film to obtain a polyamic acid gel film with certain self-supporting property, obtaining a glue film with preset thickness through a calender, allowing the flaky filler to be subjected to shearing action to be oriented in the plane of the film when the flaky filler passes through the die head channel, forming heat-conducting connection between the flaky fillers, and performing thermal imidization to obtain the high-heat-conductivity polyimide film.
5. The method for preparing the filler orientation-reinforced high thermal conductivity polyimide composite film according to claim 4, wherein the aromatic dianhydride is one or more of pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride, 4,4' -oxydiphthalic anhydride, 3 ', 4,4' -biphenyltetracarboxylic dianhydride, and bisphenol A dianhydride.
6. The method as claimed in claim 4, wherein the aromatic diamine is one or more selected from diaminodiphenyl ether, p-phenylenediamine and TAB.
7. the method for preparing the filler orientation-enhanced high thermal conductivity polyimide composite film according to claim 4, wherein the polar solvent is one of N, N-dimethylacetamide and N-methylpyrrolidone.
8. the die head for preparing the filler orientation-reinforced high-thermal-conductivity polyimide composite film is characterized in that the die head is provided with a long and narrow die head channel with gradually changed cross-sectional area.
9. The die for preparing the filler orientation-reinforced high thermal conductivity polyimide composite film according to claim 8, wherein the cross section of the die channel is rectangular, and the cross section area of the die channel is gradually reduced along the extrusion direction.
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| CN115216151B (en) * | 2022-08-16 | 2024-03-15 | 江西理工大学 | Construction method of polyimide film heat conduction channel |
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| CN115873285B (en) * | 2022-12-26 | 2024-04-19 | 蜂巢能源科技(上饶)有限公司 | Polyimide film and preparation method thereof |
| CN116496528B (en) * | 2023-06-25 | 2023-09-22 | 苏州尊尔光电科技有限公司 | High-strength heat-conducting composite polyimide film and preparation method thereof |
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