CN113999526A - Polyimide film having improved thermal conductivity and method for preparing the same - Google Patents
Polyimide film having improved thermal conductivity and method for preparing the same Download PDFInfo
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- CN113999526A CN113999526A CN202111309968.9A CN202111309968A CN113999526A CN 113999526 A CN113999526 A CN 113999526A CN 202111309968 A CN202111309968 A CN 202111309968A CN 113999526 A CN113999526 A CN 113999526A
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims description 9
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 25
- 239000000178 monomer Substances 0.000 claims abstract description 22
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 11
- 150000004985 diamines Chemical class 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 23
- 238000011049 filling Methods 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000010954 inorganic particle Substances 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 8
- 238000005576 amination reaction Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 3
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 16
- 239000007788 liquid Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a polyimide film with improved thermal conductivity and a preparation method thereof, relating to the technical field of polyimide films, and the polyimide film comprises a diamine monomer, an acid dianhydride monomer, an imidization solution, graphene, a dehydrating agent, a catalyst, rare earth oxide and aluminum nitride, wherein the aluminum nitride doped with the rare earth oxide has low dielectric loss, meanwhile, the graphene and aluminum nitride have higher heat-conducting property, rare earth oxide, graphene and aluminum nitride are added into the polyimide film, can obviously reduce the dielectric loss of the polyimide film, obviously improve the heat-conducting property of the polyimide film, and then, half amount of heat-conducting slurry is uniformly wrapped on the surface of the polyimide film, so that the polyimide film with unqualified quality can be subjected to secondary processing treatment, the product percent of pass can reach one hundred percent, and unqualified products are avoided.
Description
Technical Field
The invention relates to the technical field of polyimide films, in particular to a polyimide film with improved thermal conductivity and a preparation method thereof.
Background
Polyimide is one of organic polymer materials with the best comprehensive performance, has the advantages of high temperature resistance of more than 400 ℃, long-term use range of-200-300 ℃, high insulating property and the like, and is widely applied to the fields of aerospace, aviation, microelectronics, nano, liquid crystal, separation membranes, laser and the like.
The polyimide film that traditional mode obtained through the method of adulterating heat conduction filler in the resin has been difficult to satisfy electronic product's heat dissipation requirement, and the practicality is poor, and secondly, all heat conduction fillers mix in the inside of film, when film heat conduction quality not reach standard, can't carry out secondary operation, cause the raw materials extravagant, increased the loss of enterprise.
Disclosure of Invention
The invention aims to: to solve the problems of poor thermal conductivity and inconvenience in secondary processing, a polyimide film having improved thermal conductivity and a method for preparing the same are provided.
In order to achieve the purpose, the invention provides the following technical scheme: a polyimide film having improved thermal conductivity, comprising a diamine monomer, an acid dianhydride monomer, an imidization solution, graphene, a dehydrating agent, a catalyst, a rare earth oxide, and aluminum nitride; the thickness of the polyimide film is 40-60 μm, the elongation at break is 70-130%, the elastic modulus is 2.7-4.0GPa, and the thermal expansion coefficient is 16-32 ppm/K.
Preferably, the imidization solution includes a filler, which is at least one inorganic particle of calcium hydrogen phosphate, calcium, and potassium.
By adopting the technical scheme: inorganic particles are introduced, so that the film is convenient to roll, and the winding performance of the film is improved.
Preferably, the filling amount of the graphene, the rare earth oxide and the aluminum nitride is controlled to be 5-25 wt%.
By adopting the technical scheme: the filling amount is strictly controlled, and the problem that the heat-conducting property of the film is improved to a limited extent when the filling amount of the heat-conducting filler is too low is avoided; when the filling amount of the heat-conducting filler is too high, the mechanical property of the film is influenced to a certain extent.
Preferably, the average particle diameter D50 of the aluminum nitride and the graphene is 2.5 to 20 μm.
By adopting the technical scheme, the particle size is strictly controlled, and the problem that the heat-conducting filler is not easy to disperse when the particle size is too large is avoided; when the particle size is too small, the heat-conducting filler is easy to agglomerate.
A method for preparing a polyimide film having improved thermal conductivity, comprising the steps of:
step 1: mixing rare earth oxide, graphene and aluminum nitride according to a certain proportion, then putting the mixture into a ball mill for grinding and sieving, and sintering the mixture for 2 to 3 hours at the temperature of 1900-;
step 2: adding a diamine monomer and an acid dianhydride monomer into a solvent, and mixing and stirring at-20-0 ℃ to obtain a mixed solution A, wherein the viscosity of the mixed solution A is not less than 100000 centipoises;
and step 3: dispersing the mixture obtained in the step 1 in an organic solvent to form heat-conducting slurry B;
and 4, step 4: stirring and mixing the mixed solution A obtained in the step 2 with an imidization solution for 1.5-3H, and then adding one part of heat-conducting slurry B to obtain a polyimide film intermediate;
and 5: adding a dehydrating agent and a catalyst into the polyimide film intermediate obtained in the step 4, and mixing and stirring the mixture in inert gas at the temperature of between 20 ℃ below zero and 0 ℃ to obtain polyimide film mixed solution;
step 6: defoaming, filling, film forming, drying and stripping the polyimide film mixed solution obtained in the step 5 to obtain a polyimide film preform;
and 7: uniformly and fully wrapping half of the heat-conducting slurry B left in the step (4) on the polyimide film preform, and then guiding the polyimide film preform to an imidization furnace for hot-pressing amination to obtain a polyimide film finished product with improved heat conductivity
Preferably, the film-forming carrier of the polyimide film preform in the step 5 is a cold steel belt
Through adopting above-mentioned technical scheme, with the liquid film tiling on cold steel band, make things convenient for the scraper blade to scrape and get solid polyimide film.
Preferably, the flowing direction of hot wind and hot wind during drying in the step 5 is opposite to the running direction of the polyimide film preform.
By adopting the technical scheme, the temperature of the liquid film is gradually increased during drying, the solvent is gradually volatilized, and the drying effect is improved.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the rare earth oxide-doped aluminum nitride has low dielectric loss and high heat conductivity with graphene aluminum nitride, the rare earth oxide, the graphene and the aluminum nitride are added into the polyimide film, the dielectric loss of the polyimide film can be obviously reduced, the heat conductivity of the polyimide film is obviously improved, then half of heat-conducting slurry is uniformly coated on the surface of the polyimide film, the polyimide film with unqualified quality can be subjected to secondary processing treatment, the product qualification rate reaches one hundred percent, unqualified products are avoided, the heat conductivity and the mechanical strength are also enhanced, and the windability of the film can be improved by further introducing inorganic particles into the polyimide film.
Detailed Description
Example 1:
a polyimide film having improved thermal conductivity, comprising a diamine monomer, an acid dianhydride monomer, an imidization solution, graphene, a dehydrating agent, a catalyst, a rare earth oxide, and aluminum nitride; the polyimide film had a thickness of 40 μm, an elongation at break of 70%, an elastic modulus of 2.7GPa, and a thermal expansion coefficient of 16 ppm/K.
In the present invention, the imidization solution includes a filler, and the filler is calcium hydrogen phosphate inorganic particles.
By adopting the technical scheme: inorganic particles are introduced, so that the film is convenient to roll, and the winding performance of the film is improved.
In the invention, the filling amount of the graphene, the rare earth oxide and the aluminum nitride is controlled to be 5 wt%.
By adopting the technical scheme: the filling amount is strictly controlled, and the problem that the heat-conducting property of the film is improved to a limited extent when the filling amount of the heat-conducting filler is too low is avoided; when the filling amount of the heat-conducting filler is too high, the mechanical property of the film is influenced to a certain extent.
In the present invention, the average particle diameter D50 of the aluminum nitride and graphene is 2.5 μm.
By adopting the technical scheme, the particle size is strictly controlled, and the problem that the heat-conducting filler is not easy to disperse when the particle size is too large is avoided; when the particle size is too small, the heat-conducting filler is easy to agglomerate.
A method for preparing a polyimide film having improved thermal conductivity, comprising the steps of:
step 1: mixing rare earth oxide, graphene and aluminum nitride according to a certain proportion, then putting the mixture into a ball mill for grinding and sieving, and sintering the mixture for 3 hours at the temperature of 1900 ℃ in an inert gas environment to obtain a mixture;
step 2: adding a diamine monomer and an acid dianhydride monomer into a solvent, and mixing and stirring at-20 ℃ to obtain a mixed solution A, wherein the viscosity of the mixed solution A is not less than 100000 centipoises;
and step 3: dispersing the mixture obtained in the step 1 in an organic solvent to form heat-conducting slurry B;
and 4, step 4: stirring and mixing the mixed solution A obtained in the step 2 with an imidization solution for 1.5H, and then adding one part of heat-conducting slurry B to obtain a polyimide film intermediate;
and 5: adding a dehydrating agent and a catalyst into the polyimide film intermediate obtained in the step 4, and mixing and stirring the mixture in inert gas at the temperature of minus 20 ℃ to obtain polyimide film mixed solution;
step 6: defoaming, filling, film forming, drying and stripping the polyimide film mixed solution obtained in the step 5 to obtain a polyimide film preform;
and 7: uniformly and fully wrapping half of the heat-conducting slurry B left in the step (4) on the polyimide film preform, and then guiding the polyimide film preform to an imidization furnace for hot-pressing amination to obtain a polyimide film finished product with improved heat conductivity
In the invention, the film forming carrier of the polyimide film preform in the step 5 is a cold steel belt
Through adopting above-mentioned technical scheme, with the liquid film tiling on cold steel band, make things convenient for the scraper blade to scrape and get solid polyimide film.
In the invention, the flow direction of hot wind and hot wind is opposite to the running direction of the polyimide film preform during drying in the step 5.
By adopting the technical scheme, the temperature of the liquid film is gradually increased during drying, the solvent is gradually volatilized, and the drying effect is improved.
Example 2:
a polyimide film having improved thermal conductivity, comprising a diamine monomer, an acid dianhydride monomer, an imidization solution, graphene, a dehydrating agent, a catalyst, a rare earth oxide, and aluminum nitride; the polyimide film had a thickness of 50 μm, an elongation at break of 100%, an elastic modulus of 3.3GPa, and a thermal expansion coefficient of 26 ppm/K.
In the present invention, the imidization solution includes a filler, which is calcium inorganic particles.
By adopting the technical scheme: inorganic particles are introduced, so that the film is convenient to roll, and the winding performance of the film is improved.
In the invention, the filling amount of the graphene, the rare earth oxide and the aluminum nitride is controlled at 15 wt%.
By adopting the technical scheme: the filling amount is strictly controlled, and the problem that the heat-conducting property of the film is improved to a limited extent when the filling amount of the heat-conducting filler is too low is avoided; when the filling amount of the heat-conducting filler is too high, the mechanical property of the film is influenced to a certain extent.
In the present invention, the average particle diameter D50 of the aluminum nitride and graphene is 12 μm.
By adopting the technical scheme, the particle size is strictly controlled, and the problem that the heat-conducting filler is not easy to disperse when the particle size is too large is avoided; when the particle size is too small, the heat-conducting filler is easy to agglomerate.
A method for preparing a polyimide film having improved thermal conductivity, comprising the steps of:
step 1: mixing rare earth oxide, graphene and aluminum nitride according to a certain proportion, then putting the mixture into a ball mill for grinding and sieving, and sintering the mixture for 2.5 hours at 1950 ℃ in an inert gas environment to obtain a mixture;
step 2: adding a diamine monomer and an acid dianhydride monomer into a solvent, and mixing and stirring at-10 ℃ to obtain a mixed solution A, wherein the viscosity of the mixed solution A is not less than 100000 centipoises;
and step 3: dispersing the mixture obtained in the step 1 in an organic solvent to form heat-conducting slurry B;
and 4, step 4: stirring and mixing the mixed solution A obtained in the step 2 with an imidization solution for 2.3H, and then adding one of two parts of heat-conducting slurry B to obtain a polyimide film intermediate;
and 5: adding a dehydrating agent and a catalyst into the polyimide film intermediate obtained in the step 4, and mixing and stirring the mixture in inert gas at the temperature of minus 10 ℃ to obtain polyimide film mixed solution;
step 6: defoaming, filling, film forming, drying and stripping the polyimide film mixed solution obtained in the step 5 to obtain a polyimide film preform;
and 7: uniformly and fully wrapping half of the heat-conducting slurry B left in the step (4) on the polyimide film preform, and then guiding the polyimide film preform to an imidization furnace for hot-pressing amination to obtain a polyimide film finished product with improved heat conductivity
In the invention, the film forming carrier of the polyimide film preform in the step 5 is a cold steel belt
Through adopting above-mentioned technical scheme, with the liquid film tiling on cold steel band, make things convenient for the scraper blade to scrape and get solid polyimide film.
In the invention, the flow direction of hot wind and hot wind is opposite to the running direction of the polyimide film preform during drying in the step 5.
By adopting the technical scheme, the temperature of the liquid film is gradually increased during drying, the solvent is gradually volatilized, and the drying effect is improved.
Example 3:
a polyimide film having improved thermal conductivity, comprising a diamine monomer, an acid dianhydride monomer, an imidization solution, graphene, a dehydrating agent, a catalyst, a rare earth oxide, and aluminum nitride; the polyimide film had a thickness of 60 μm, an elongation at break of 130%, an elastic modulus of 4.0GPa, and a thermal expansion coefficient of 32 ppm/K.
In the present invention, the imidization solution includes a filler, and the filler is potassium inorganic particles.
By adopting the technical scheme: inorganic particles are introduced, so that the film is convenient to roll, and the winding performance of the film is improved.
In the invention, the filling amount of the graphene, the rare earth oxide and the aluminum nitride is controlled at 25 wt%.
By adopting the technical scheme: the filling amount is strictly controlled, and the problem that the heat-conducting property of the film is improved to a limited extent when the filling amount of the heat-conducting filler is too low is avoided; when the filling amount of the heat-conducting filler is too high, the mechanical property of the film is influenced to a certain extent.
In the present invention, the average particle diameter D50 of the aluminum nitride and graphene is 20 μm.
By adopting the technical scheme, the particle size is strictly controlled, and the problem that the heat-conducting filler is not easy to disperse when the particle size is too large is avoided; when the particle size is too small, the heat-conducting filler is easy to agglomerate.
A method for preparing a polyimide film having improved thermal conductivity, comprising the steps of:
step 1: mixing rare earth oxide, graphene and aluminum nitride according to a certain proportion, then putting the mixture into a ball mill for grinding and sieving, and sintering the mixture for 2 hours at the temperature of 2000 ℃ in an inert gas environment to obtain a mixture;
step 2: adding a diamine monomer and an acid dianhydride monomer into a solvent, and mixing and stirring at 0 ℃ to obtain a mixed solution A, wherein the viscosity of the mixed solution A is not less than 100000 centipoises;
and step 3: dispersing the mixture obtained in the step 1 in an organic solvent to form heat-conducting slurry B;
and 4, step 4: stirring and mixing the mixed solution A obtained in the step 2 with an imidization solution for 1.5-3H, and then adding one part of heat-conducting slurry B to obtain a polyimide film intermediate;
and 5: adding a dehydrating agent and a catalyst into the polyimide film intermediate obtained in the step 4, and mixing and stirring in inert gas at 0 ℃ to obtain polyimide film mixed solution;
step 6: defoaming, filling, film forming, drying and stripping the polyimide film mixed solution obtained in the step 5 to obtain a polyimide film preform;
and 7: uniformly and fully wrapping half of the heat-conducting slurry B left in the step (4) on the polyimide film preform, and then guiding the polyimide film preform to an imidization furnace for hot-pressing amination to obtain a polyimide film finished product with improved heat conductivity
In the invention, the film forming carrier of the polyimide film preform in the step 5 is a cold steel belt
Through adopting above-mentioned technical scheme, with the liquid film tiling on cold steel band, make things convenient for the scraper blade to scrape and get solid polyimide film.
In the invention, the flow direction of hot wind and hot wind is opposite to the running direction of the polyimide film preform during drying in the step 5.
By adopting the technical scheme, the temperature of the liquid film is gradually increased during drying, the solvent is gradually volatilized, and the drying effect is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. A polyimide film having improved thermal conductivity, characterized in that: the catalyst comprises diamine monomer, acid dianhydride monomer, imidization solution, graphene, dehydrating agent, catalyst, rare earth oxide and aluminum nitride; the thickness of the polyimide film is 40-60 μm, the elongation at break is 70-130%, the elastic modulus is 2.7-4.0GPa, and the thermal expansion coefficient is 16-32 ppm/K.
2. The polyimide film with improved thermal conductivity according to claim 1, characterized in that: the imidization solution includes a filler, which is at least one inorganic particle of calcium hydrogen phosphate, calcium, and potassium.
3. The polyimide film having improved thermal conductivity according to claim 1, wherein: the filling amount of the graphene, the rare earth oxide and the aluminum nitride is controlled to be 5-25 wt%.
4. The polyimide film having improved thermal conductivity according to claim 1, wherein: the average grain diameter D50 of the aluminum nitride and the graphene is 2.5-20 μm.
5. The method for preparing a polyimide film having improved thermal conductivity according to claim 1, comprising the steps of:
step 1: mixing rare earth oxide, graphene and aluminum nitride according to a certain proportion, then putting the mixture into a ball mill for grinding and sieving, and sintering the mixture for 2 to 3 hours at the temperature of 1900-;
step 2: adding a diamine monomer and an acid dianhydride monomer into a solvent, and mixing and stirring at-20-0 ℃ to obtain a mixed solution A, wherein the viscosity of the mixed solution A is not less than 100000 centipoises;
and step 3: dispersing the mixture obtained in the step 1 in an organic solvent to form heat-conducting slurry B;
and 4, step 4: stirring and mixing the mixed solution A obtained in the step 2 with an imidization solution for 1.5-3H, and then adding one part of heat-conducting slurry B to obtain a polyimide film intermediate;
and 5: adding a dehydrating agent and a catalyst into the polyimide film intermediate obtained in the step 4, and mixing and stirring the mixture in inert gas at the temperature of between 20 ℃ below zero and 0 ℃ to obtain polyimide film mixed solution;
step 6: defoaming, filling, film forming, drying and stripping the polyimide film mixed solution obtained in the step 5 to obtain a polyimide film preform;
and 7: and (4) uniformly and fully wrapping the half of the heat-conducting slurry B left in the step (4) on the polyimide film preform, and then guiding the polyimide film preform to an imidization furnace for hot-pressing amination to obtain a polyimide film finished product with improved heat conductivity.
6. The polyimide film having improved thermal conductivity according to claim 5, wherein: and 5, the film forming carrier of the polyimide film preform in the step 5 is a cold steel belt.
7. The polyimide film having improved thermal conductivity according to claim 5, wherein: and 5, the flowing direction of hot wind and hot wind is opposite to the running direction of the polyimide film preform during drying.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194062A (en) * | 2013-03-29 | 2013-07-10 | 株洲时代电气绝缘有限责任公司 | Polyimide film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194062A (en) * | 2013-03-29 | 2013-07-10 | 株洲时代电气绝缘有限责任公司 | Polyimide film and preparation method thereof |
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