CN113912883A - Moisture-proof heat-conducting insulating film and preparation method thereof - Google Patents
Moisture-proof heat-conducting insulating film and preparation method thereof Download PDFInfo
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- CN113912883A CN113912883A CN202111256061.0A CN202111256061A CN113912883A CN 113912883 A CN113912883 A CN 113912883A CN 202111256061 A CN202111256061 A CN 202111256061A CN 113912883 A CN113912883 A CN 113912883A
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- 238000002360 preparation method Methods 0.000 title description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims abstract description 49
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 37
- 229920000642 polymer Polymers 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000004642 Polyimide Substances 0.000 claims abstract description 10
- 229920001721 polyimide Polymers 0.000 claims abstract description 10
- 230000007547 defect Effects 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 9
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- 239000012188 paraffin wax Substances 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 26
- 239000012153 distilled water Substances 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229940075507 glyceryl monostearate Drugs 0.000 claims description 15
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- 238000001125 extrusion Methods 0.000 claims description 14
- 238000003682 fluorination reaction Methods 0.000 claims description 14
- 238000004108 freeze drying Methods 0.000 claims description 14
- 239000000155 melt Substances 0.000 claims description 14
- 230000007935 neutral effect Effects 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 14
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 13
- 239000002033 PVDF binder Substances 0.000 claims description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 13
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 12
- 239000000194 fatty acid Substances 0.000 claims description 12
- 229930195729 fatty acid Natural products 0.000 claims description 12
- 150000004665 fatty acids Chemical class 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- VIFIHLXNOOCGLJ-UHFFFAOYSA-N trichloro(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CC[Si](Cl)(Cl)Cl VIFIHLXNOOCGLJ-UHFFFAOYSA-N 0.000 claims description 9
- 229920002472 Starch Polymers 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- 239000008107 starch Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000002800 charge carrier Substances 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract description 2
- 230000006798 recombination Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 17
- 238000005245 sintering Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 238000010030 laminating Methods 0.000 description 5
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 description 4
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/0007—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality
- B32B37/003—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality to avoid air inclusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- 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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/16—Ethene-propene or ethene-propene-diene copolymers
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- 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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- 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
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- 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
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- Formation Of Insulating Films (AREA)
Abstract
The invention belongs to the technical field of films, and particularly relates to a moisture-proof heat-conducting insulating film which comprises: the carrier film comprises elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect2O3The insulating layer consists of insulating polymer polyimide and Al with hydrophobic modified high vacancy defect2O3GaN and glycerin monostearate, the hydrophobic membrane is prepared by coating a fluorinated liquid containing paraffin-silicon on a polytetrafluoroethylene plate, and the Al with high vacancy defect is subjected to hydrophobic modification2O3The GaN is prepared by hydrothermal reaction, calcination, high-temperature annealing and hydrophobic modification, a hydrophobic membrane prepared by coating the paraffin-silicon-containing fluorinated liquid on a polytetrafluoroethylene plate has a hydrophobic effect, and Al with high vacancy defect is subjected to hydrophobic modification2O3the/GaN can capture charge carriers in water, accelerate charge recombination, inhibit conduction, and hydrophobically modify Al with high vacancy defects2O3the/GaN can play a role in resisting moisture cooperatively with the hydrophobic film.
Description
Technical Field
The invention belongs to the technical field of films, and particularly relates to a moisture-proof heat-conducting insulating film and a preparation method thereof.
Background
With the rapid development of the electronic industry, electronic equipment devices are more and more popular, and meanwhile, the electronic equipment is smaller and smaller in size and has more and more functions. The chip or the electronic module in the electronic device is required to have powerful functions and operate at a faster and faster speed, the generated heat is more and more, the heat energy accumulated at a certain point of the chip or a certain point of the electronic module is more and more, the short, thin and light space in the electronic device cannot or is difficult to conduct heat out simply by arranging a fan, and when the chip or the electronic module is in a high-temperature environment, the working performance is reduced, and the service life is shortened.
The electrically insulating film is a thin plastic sheet that can be used in electronic components for: computers, printers, fax machines, household appliances, audio equipment, video equipment, telephones, radios, motors, generators, wires, cables, and the like, but insulation alone does not satisfy more needs, and how to attach the moisture-resistant and heat-conductive function to the insulating film is an urgent problem to be solved.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the problem of poor moisture-proof and heat-conducting performance of the conventional insulating film material.
(II) technical scheme
In order to solve the above problems, the present invention provides a moisture-resistant heat-conductive insulating film, comprising: the carrier film is composed of elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect2O3The insulating layer consists of insulating polymer polyimide and Al with hydrophobic modified high vacancy defect2O3GaN and glycerin monostearate, the hydrophobic membrane is prepared by coating a fluorinated liquid containing paraffin-silicon on a polytetrafluoroethylene plate, and the Al with high vacancy defect is subjected to hydrophobic modification2O3the/GaN is prepared by hydrothermal reaction, calcination, high-temperature annealing and hydrophobic modification.
The invention also provides a preparation method of the moisture-proof heat-conducting insulating film, which comprises the following steps: (1) weighing Al (NO)3)3·9H2Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/L NaOH solution until pH value is about 9, stirring at 120 deg.C for 1 hr, filtering to precipitate starch powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5 deg.C/min, and annealing to obtain Al with high level defect2O3/GaN；
(2) Al with high dislocation defect2O3Dispersing GaN in water to obtain uniformly dispersed solution, adding fatty acid with more than 6 carbon atoms, stirring in water bath at constant temperature, and drying in drying oven at constant temperature to obtain lipophilic Al with high vacancy defect2O3Adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent is completely volatilized to obtain a mixture, and putting the mixture in an ammonia atmosphere for pyrolysis treatment to obtain the hydrophobically modified Al with high vacancy defects2O3/GaN；
(3) Weighing elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect2O3Mixing with GaN and glyceryl monostearateMelt-extruding the mixture from a T die using a single-shaft extruder having a diameter of 30mm and a powder sintered filter having a nominal diameter of 20 μm, molding, and continuously curling by cooling to obtain a melt-extruded carrier film having a width of 320 mm;
(4) weighing insulating polymer polyimide and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from T die with single-shaft extruder with diameter of 30mm and powder sintered filter with nominal diameter of 20 μm, making into film, cooling, and continuously curling to obtain melt-extruded insulating layer with width of 320 mm;
(5) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(6) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) and overlapping the carrier film, the insulating layer and the hydrophobic film together, and pressurizing and discharging air between the adjacent overlapped layers by using a hydraulic press to enable the lower layer and the upper layer to be tightly integrated into a whole so as to obtain the moisture-proof heat-conducting insulating film.
Preferably, Al (NO) in said step (1)3)3·9H2The mass ratio of O, distilled water and GaN is 1.76-2.46:40-50:0.3-0.5, the drying temperature is 100-2 hours, the annealing temperature is 800-900 ℃, and the annealing time is 5-8 minutes.
Preferably, Al having high vacancy defect in the step (2)2O3The mass ratio of GaN to water to fatty acid with more than 6 carbon atoms is 8-10:15-30:0.2-0.5, and the stirring temperature is 50-80 ℃.
Preferably, the elastic polymer ethylene propylene rubber and the Al with hydrophobic modified high vacancy defects in the step (3)2O3The mass ratio of GaN to glycerin monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film-making speed is 2-2.5 m/min.
Preferably, the insulating polymer polyimide in the step (4) is hydrophobically modified Al with high vacancy defect2O3The mass ratio of GaN to glycerin monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film-making speed is 2-2.5 m/min.
Preferably, the mass ratio of the paraffin wax carboxylated in the step (6), the polyvinylidene fluoride, the hexafluoropropylene, the 3-aminopropyltriethoxysilane, the ethanol, the ethyl orthosilicate, the water, the ethanol and the 1H,1H,2H, 2H-perfluorodecyl trichlorosilane is 1-3:2-5:2-5:1-3:5-8:1-2:2-4:20-25: 0.01-0.03.
Compared with the prior art, the method has the beneficial effects that:
(1) the invention provides a moisture-proof heat-conducting insulating film and a preparation method thereof.A hydrophobic film prepared by coating a fluorinated liquid containing paraffin-silicon on a polytetrafluoroethylene plate has a hydrophobic effect, and hydrophobically modified Al with high vacancy defect2O3the/GaN can capture charge carriers in water, accelerate charge recombination, inhibit conduction, and hydrophobically modify Al with high vacancy defects2O3the/GaN can play a role in resisting moisture cooperatively with the hydrophobic film.
(2) The invention provides a moisture-proof heat-conducting insulating film and a preparation method thereof.A carrier film and an insulating layer are both filled with hydrophobically modified Al with high-position defects2O3The GaN overcomes the problems of low heat conductivity coefficient and poor heat conductivity of the polymer, and the elastic ethylene propylene rubber is adopted as the carrier layer, so that the carrier layer is beneficial to better contact with the circuit device.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for preparing a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO)3)3·9H2The mass ratio of O to distilled water to GaN is 1.76:40:0.3, and Al with high dislocation defects2O3GaN, water, fatty acid with more than 6 carbon atoms in a mass ratio of 8:15:0.2, elastic polymer, and hydrophobically modified Al with high vacancy defect2O3The mass ratio of GaN to glycerin monostearate is 70:5:3, the insulating polymer and the hydrophobically modified Al with high vacancy defects2O3The mass ratio of the glycerol monostearate to the GaN is 70:5:3, and the mass ratio of the carboxylated paraffin, the polyvinylidene fluoride, the hexafluoropropylene, the 3-aminopropyltriethoxysilane, the ethanol, the ethyl orthosilicate, the water, the ethanol and the 1H,1H,2H, 2H-perfluorodecyl trichlorosilane is 1:2:2:1:5:1:2:20: 0.01.
(1) Weighing Al (NO)3)3·9H2Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/L NaOH solution until pH value is about 9, stirring at 120 deg.C for 1 hr, filtering to precipitate starch powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at a heating rate of 5 deg.C/min, annealing at 100 deg.C for 2 hr, 350 deg.C for 1.5 hr, 800 deg.C for 5min to obtain Al with high level defect2O3/GaN；
(2) Al with high dislocation defect2O3Dispersing GaN in water to obtain uniformly dispersed solution, adding fatty acid with carbon number of more than 6, stirring in water bath at constant temperatureStirring at 50 deg.C, and drying in drying oven at constant temperature to obtain lipophilic Al with high vacancy defect2O3Adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent is completely volatilized to obtain a mixture, and putting the mixture in an ammonia atmosphere for pyrolysis treatment to obtain the hydrophobically modified Al with high vacancy defects2O3/GaN；
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 μm, wherein the melt extrusion temperature is 250 ℃, the film-making speed is 2m/min, molding, and continuously curling by cooling to obtain a melt-extruded carrier film with the width of 320 mm;
(4) weighing insulating polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 μm, wherein the melt extrusion temperature is 250 ℃, the film-making speed is 2m/min, and making a film, and cooling and continuously curling to obtain a melt-extruded insulating layer with the width of 320 mm;
(5) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(6) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) and laminating the carrier film, the insulating layer and the hydrophobic film together, and pressurizing by using a hydraulic press to discharge air between the adjacent laminated layers so that the lower layer and the upper layer can be tightly combined into a whole to obtain the moisture-proof heat-conducting insulating film.
Example 2
A method for preparing a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO)3)3·9H2The mass ratio of O, distilled water and GaN is 1.78:42:0.35, and Al with high dislocation defects2O3GaN, water, fatty acid with more than 6 carbon atoms in a mass ratio of 8.5:16:0.25, elastic polymer, and hydrophobically modified Al with high vacancy defect2O3GaN, glycerin monostearate with a mass ratio of 75:6:3.5, insulating polymer, hydrophobically modified Al with high vacancy defects2O3The mass ratio of the glycerol monostearate to the GaN is 78:10:4, and the mass ratio of the carboxylated paraffin, the polyvinylidene fluoride, the hexafluoropropylene, the 3-aminopropyltriethoxysilane, the ethanol, the ethyl orthosilicate, the water, the ethanol, the 1H, the 2H-perfluorodecyl trichlorosilane is 1.2:2.2:2.2:1.2:5.2:1.2:2.5:21: 0.015.
(1) Weighing Al (NO)3)3·9H2Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/L NaOH solution until pH value is about 9, stirring at 120 deg.C for 1 hr, filtering to precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at a heating rate of 5 deg.C/min, annealing at drying temperature of 102 deg.C for 2.2 hr, 355 deg.C for 1.55 hr, 82 deg.C for 5.5 min to obtain Al with high vacancy defect2O3/GaN；
(2) Al with high dislocation defect2O3Dispersing GaN in water to obtain uniformly dispersed solution, adding fatty acid with carbon number of more than 6, stirring in water bath at constant temperature of 60 deg.CDrying at constant temperature in drying oven to prepare lipophilic Al with high vacancy defect2O3Adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent is completely volatilized to obtain a mixture, and putting the mixture in an ammonia atmosphere for pyrolysis treatment to obtain the hydrophobically modified Al with high vacancy defects2O3/GaN；
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with a diameter of 30mm and a powder sintering filter with a nominal diameter of 20 μm, wherein the melt extrusion temperature is 254 ℃, the film-making speed is 2.1m/min, molding, and continuously curling by cooling to obtain a melt-extruded carrier film with a width of 320 mm;
(4) weighing insulating polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 μm, wherein the melt extrusion temperature is 255 ℃, the film-making speed is 2.1m/min, and making a film, and cooling and continuously curling to obtain a melt-extruded insulating layer with the width of 320 mm;
(5) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(6) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) and laminating the carrier film, the insulating layer and the hydrophobic film together, and pressurizing by using a hydraulic press to discharge air between the adjacent laminated layers so that the lower layer and the upper layer can be tightly combined into a whole to obtain the moisture-proof heat-conducting insulating film.
Example 3
A method for preparing a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO)3)3·9H2The mass ratio of O to distilled water to GaN is 2.2:48:0.45, and Al with high dislocation defects2O3GaN, water, fatty acid with more than 6 carbon atoms in a mass ratio of 9:19:0.4, elastic polymer, and hydrophobically modified Al with high vacancy defect2O3The mass ratio of GaN to glycerin monostearate is 88:12:4.8, the insulating polymer and the hydrophobically modified Al with high vacancy defects2O3The mass ratio of the glycerol monostearate to the GaN is 87:14.5:4.9, and the mass ratio of the carboxylated paraffin, the polyvinylidene fluoride, the hexafluoropropylene, the 3-aminopropyltriethoxysilane, the ethanol, the ethyl orthosilicate, the water, the ethanol, the 1H, the 2H and the 2H-perfluorodecyl trichlorosilane is 2:4:4:2:7:1.8:3:23: 0.02.
(1) Weighing Al (NO)3)3·9H2Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/LNaOH solution until the pH value is about 9, stirring at 120 ℃ for 1 hour, filtering to precipitate starch powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at a heating rate of 5 ℃/min, and finally annealing, wherein the drying temperature is set to 106 ℃, the drying time is 2.4 hours, the calcining temperature is 360 ℃, the calcining time is 1.7 hours, the annealing temperature is 890 ℃, and the annealing time is 7 minutes to obtain Al with high dislocation defects2O3/GaN；
(2) Al with high dislocation defect2O3Dispersing GaN in water to obtain uniformly dispersed solution, adding fatty acid with carbon number of more than 6, stirring in water bath at constant temperature of 70 deg.C, and drying in drying oven at constant temperature to obtain lipophilic high-altitude productBit-defective Al2O3Adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent is completely volatilized to obtain a mixture, and putting the mixture in an ammonia atmosphere for pyrolysis treatment to obtain the hydrophobically modified Al with high vacancy defects2O3/GaN；
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 μm, wherein the melt extrusion temperature is 265 ℃, the film-making speed is 2.4m/min, molding, and continuously curling by cooling to obtain a melt-extruded carrier film with the width of 320 mm;
(4) weighing insulating polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 μm, wherein the melt extrusion temperature is 265 ℃, the film-making speed is 2.4m/min, and making a film, and cooling and continuously curling to obtain a melt-extruded insulating layer with the width of 320 mm;
(5) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(6) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) and laminating the carrier film, the insulating layer and the hydrophobic film together, and pressurizing by using a hydraulic press to discharge air between the adjacent laminated layers so that the lower layer and the upper layer can be tightly combined into a whole to obtain the moisture-proof heat-conducting insulating film.
Example 4
A method for preparing a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO)3)3·9H2The mass ratio of O to distilled water to GaN is 2.46:50:0.5, and Al with high dislocation defects2O3GaN, water, fatty acid with more than 6 carbon atoms in a mass ratio of 10:30:0.5, elastic polymer, and hydrophobically modified Al with high vacancy defect2O3The mass ratio of GaN to glycerin monostearate is 90:15:5, the insulating polymer and the hydrophobically modified Al with high vacancy defects2O3The mass ratio of the glycerol monostearate to the GaN is 90:15:5, and the mass ratio of the carboxylated paraffin, the polyvinylidene fluoride, the hexafluoropropylene, the 3-aminopropyltriethoxysilane, the ethanol, the ethyl orthosilicate, the water, the ethanol, the 1H, the 2H and the 2H-perfluorodecyl trichlorosilane is 3:5:5:3:8:2:4:25: 0.03.
(1) Weighing Al (NO)3)3·9H2Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/L NaOH solution until pH value is about 9, stirring at 120 deg.C for 1 hr, filtering to precipitate starch powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at a heating rate of 5 deg.C/min, annealing at drying temperature of 110 deg.C for 2-3 hr, 400 deg.C for 2 hr, 900 deg.C for 8 min to obtain Al with high level defect2O3/GaN；
(2) Al with high dislocation defect2O3Dispersing GaN in water to obtain uniformly dispersed solution, adding fatty acid with more than 6 carbon atoms, stirring in water bath at 80 deg.C, and drying in drying oven at constant temperature to obtain lipophilic Al with high vacancy defect2O3GaN, plusAdding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent is completely volatilized to obtain a mixture, and putting the mixture in an ammonia atmosphere for pyrolysis treatment to obtain the hydrophobically modified Al with high vacancy defects2O3/GaN；
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with a diameter of 30mm and a powder sintering filter with a nominal diameter of 20 μm, wherein the melt extrusion temperature is 270 ℃, the film-making speed is 2.5m/min, molding, and continuously curling by cooling to obtain a melt-extruded carrier film with a width of 320 mm;
(4) weighing insulating polymer and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 μm, wherein the melt extrusion temperature is 270 ℃, the film-making speed is 2.5m/min, and making a film, and cooling and continuously curling to obtain a melt-extruded insulating layer with the width of 320 mm;
(5) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(6) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) and laminating the carrier film, the insulating layer and the hydrophobic film together, and pressurizing by using a hydraulic press to discharge air between the adjacent laminated layers so that the lower layer and the upper layer can be tightly combined into a whole to obtain the moisture-proof heat-conducting insulating film.
Comparative example 1
A method for preparing a thermally conductive insulating film, comprising the steps of:
the material ratio is as follows: the mass ratio of the elastic polymer to the glyceryl monostearate is 70:3, and the mass ratio of the insulating polymer to the glyceryl monostearate is 70: 3.
(1) Weighing an elastic polymer and glyceryl monostearate, mixing, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 mu m, wherein the melt extrusion temperature is 250 ℃, the film making speed is 2m/min, molding, and continuously curling by cooling to obtain a melt-extruded carrier film with the width of 320 mm;
(2) weighing an insulating polymer and glyceryl monostearate, mixing, melt-extruding the mixture from a T die by using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 mu m, wherein the melt extrusion temperature is 250 ℃, the film-making speed is 2m/min, and making a film, and cooling and continuously curling to obtain a melt-extruded insulating layer with the width of 320 mm;
(3) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(4) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(5) and laminating the carrier film, the insulating layer and the hydrophobic film together, and pressurizing by using a hydraulic press to discharge air between the adjacent laminated layers so that the lower layer and the upper layer can be tightly combined into a whole to obtain the moisture-proof heat-conducting insulating film.
The film samples in the examples and comparative examples were subjected to an insulation heat conduction test: the breakdown field strength is measured by using a BTF-038-50kV voltage breakdown tester, and the adopted test standard is GB/T1408.1-2006; the DRL-III thermal conductivity coefficient tester for the thermal conductivity test has the test standard of ASTM D5470-2006 and the test method of the transient plane heat source method, and the test results of the insulating and thermal conductivity are shown in the following table 1.
TABLE 1
As can be seen from Table 1, the breakdown field strength and the thermal conductivity of the film samples of examples 1 to 4 were higher than those of the film sample of comparative example because the film material of comparative example 1 had no hydrophobically modified high-vacancy defect Al added2O3And the film sample prepared by the invention has excellent heat conduction and insulation properties.
The insulating films prepared in examples 1 to 4 and comparative example 1 were subjected to a hydrophobic property test after being immersed in an aqueous solution at 20 ℃ for 2 hours, and the test results are shown in table 2.
TABLE 2
As can be seen from Table 2, the water contact angles of the insulation film samples of examples 1-4 were larger than that of the insulation film sample of comparative example 1, indicating that the insulation film samples prepared according to the present invention have good moisture resistance.
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.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A moisture-resistant heat-conductive insulating film, comprising: the carrier film is composed of elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect2O3The insulating layer consists of insulating polymer polyimide and Al with hydrophobic modified high vacancy defect2O3GaN and glycerin monostearate, the hydrophobic membrane is prepared by coating a fluorinated liquid containing paraffin-silicon on a polytetrafluoroethylene plate, and the Al with high vacancy defect is subjected to hydrophobic modification2O3the/GaN is prepared by hydrothermal reaction, calcination, high-temperature annealing and hydrophobic modification.
2. The method for preparing the moisture-resistant heat-conductive insulating film according to claim 1, comprising the steps of:
(1) weighing Al (NO)3)3·9H2Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/L NaOH solution until pH value is about 9, stirring at 120 deg.CAfter 1 hour, filtering and precipitating starch powder, washing the starch powder for 5 times by using distilled water, drying the starch powder, calcining the obtained solid powder at the heating rate of 5 ℃/min, and finally annealing to obtain Al with high-altitude defects2O3/GaN；
(2) Al with high dislocation defect2O3Dispersing GaN in water to obtain uniformly dispersed solution, adding fatty acid with more than 6 carbon atoms, stirring in water bath at constant temperature, and drying in drying oven at constant temperature to obtain lipophilic Al with high vacancy defect2O3Adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent is completely volatilized to obtain a mixture, and putting the mixture in an ammonia atmosphere for pyrolysis treatment to obtain the hydrophobically modified Al with high vacancy defects2O3/GaN；
(3) Weighing elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die with single-shaft extruder with diameter of 30mm and powder sintered filter with nominal diameter of 20 μm, molding, cooling, and continuously curling to obtain melt-extruded carrier membrane with width of 320 mm;
(4) weighing insulating polymer polyimide and hydrophobically modified Al with high vacancy defect2O3Mixing GaN and glyceryl monostearate, melt-extruding the mixture from T die with single-shaft extruder with diameter of 30mm and powder sintered filter with nominal diameter of 20 μm, making into film, cooling, and continuously curling to obtain melt-extruded insulating layer with width of 320 mm;
(5) dispersing paraffin in concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until the filtrate is neutral, performing freeze drying, sealing, storing for later use, boiling the treated paraffin in a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3 for 1h, performing suction filtration under reduced pressure, cleaning the paraffin to be neutral by using secondary distilled water, and performing freeze drying for later use to obtain carboxylated paraffin;
(6) at room temperature, adding carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyltriethoxysilane into an ethanol solution, stirring for 5 minutes at the rotating speed of 60 revolutions per minute, then adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, then repeatedly washing with deionized water, then drying at 60 ℃, finally putting the modified paraffin into a container, adding 1H,1H,2H, 2H-perfluorodecyl trichlorosilane, putting the container into a vacuum furnace, standing for 24 hours at 100 ℃ to obtain a fluorination liquid containing paraffin-silicon, and coating the fluorination liquid containing paraffin-silicon on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) and overlapping the carrier film, the insulating layer and the hydrophobic film together, and pressurizing and discharging air between the adjacent overlapped layers by using a hydraulic press to enable the lower layer and the upper layer to be tightly integrated into a whole so as to obtain the moisture-proof heat-conducting insulating film.
3. The method for preparing the moisture-resistant heat-conductive insulating film according to claim 2, wherein Al (NO) is added in the step (1)3)3·9H2The mass ratio of O, distilled water and GaN is 1.76-2.46:40-50:0.3-0.5, the drying temperature is 100-.
4. The method for preparing the moisture-resistant heat-conductive insulating film according to claim 2, wherein Al having high vacancy defect in the step (2)2O3The mass ratio of GaN to water to fatty acid with more than 6 carbon atoms is 8-10:15-30:0.2-0.5, and the stirring temperature is 50-80 ℃.
5. The method for preparing the moisture-resistant heat-conductive insulating film according to claim 2, wherein the elastic polymer ethylene propylene rubber and the hydrophobically modified Al with high vacancy defect in the step (3)2O3The mass ratio of GaN to glycerin monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film-making speed is 2-2.5 m/min.
6. The method for preparing the moisture-resistant heat-conductive insulating film according to claim 2, wherein the insulating polymer polyimide and the hydrophobic modification in the step (4) are selected from polyimide, and polyimide, hydrophobic modification, polyimide, and polyimideAl with high vacancy defect2O3The mass ratio of GaN to glycerin monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film-making speed is 2-2.5 m/min.
7. The method for preparing the moisture-resistant heat-conductive insulating film according to claim 2, wherein the mass ratio of the carboxylated paraffin wax, the polyvinylidene fluoride, the hexafluoropropylene, the 3-aminopropyltriethoxysilane, the ethanol, the ethyl orthosilicate, the water, the ethanol, the 1H, the 2H-perfluorodecyltrichlorosilane in the step (6) is 1-3:2-5:2-5:1-3:5-8:1-2:2-4:20-25: 0.01-0.03.
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