CN113912883B - 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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- CN113912883B CN113912883B CN202111256061.0A CN202111256061A CN113912883B CN 113912883 B CN113912883 B CN 113912883B CN 202111256061 A CN202111256061 A CN 202111256061A CN 113912883 B CN113912883 B CN 113912883B
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- 238000002360 preparation method Methods 0.000 title claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 230000007547 defect Effects 0.000 claims abstract description 63
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims abstract description 58
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 36
- 229920000642 polymer Polymers 0.000 claims abstract description 33
- 229940075507 glyceryl monostearate Drugs 0.000 claims abstract description 28
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims abstract description 28
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 18
- 239000010703 silicon Substances 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 16
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 11
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims abstract description 7
- 239000004642 Polyimide Substances 0.000 claims abstract description 6
- 229920001721 polyimide Polymers 0.000 claims abstract description 6
- 239000012188 paraffin wax Substances 0.000 claims description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 40
- 238000001035 drying Methods 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 27
- 238000005303 weighing Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 26
- 239000012153 distilled water Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 23
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 20
- 239000002033 PVDF binder Substances 0.000 claims description 20
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 20
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 20
- 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
- 238000004108 freeze drying Methods 0.000 claims description 14
- 230000007935 neutral effect Effects 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 13
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 13
- 239000000194 fatty acid Substances 0.000 claims description 13
- 229930195729 fatty acid Natural products 0.000 claims description 13
- 150000004665 fatty acids Chemical class 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000009835 boiling 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
- 238000001125 extrusion Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 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
- 238000003828 vacuum filtration Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 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
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000002788 crimping Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- 229920001600 hydrophobic polymer Polymers 0.000 claims 1
- 239000002800 charge carrier Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
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- 238000009413 insulation Methods 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 description 1
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 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
- 238000006116 polymerization reaction Methods 0.000 description 1
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- 230000006798 recombination Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- 230000001052 transient effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- B32B37/0007—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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- 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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- 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
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- 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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Abstract
The invention belongs to the technical field of films, and in particular relates to a moisture-resistant heat-conducting insulating film, which comprises the following components: a carrier film, an insulating layer formed on the carrier film, a hydrophobic film formed on the insulating layer, wherein the carrier film is prepared from ethylene propylene rubber which is an elastic polymer and Al with high vacancy defects modified by hydrophobic property 2 O 3 GaN and glyceryl monostearate, and the insulating layer is made of insulating polymer polyimide and hydrophobically modified Al with high vacancy defect 2 O 3 GaN, glyceryl monostearate, the hydrophobic film is prepared by coating fluorinated solution containing paraffin-silicon on polytetrafluoroethylene plate, and the hydrophobically modified high vacancy defect Al 2 O 3 GaN is prepared through hydrothermal reaction, calcining, high-temperature annealing and hydrophobic modification, and the hydrophobic film prepared by coating the fluorinated liquid containing paraffin-silicon on the polytetrafluoroethylene plate has hydrophobic effect and is hydrophobically modified with Al with high vacancy defect 2 O 3 GaN can capture charge carriers in water and accelerate charge recombinationInhibiting conductive, hydrophobically modified high vacancy defects Al 2 O 3 GaN can play a role in synergy with the hydrophobic film for moisture resistance.
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 increasingly popular, and meanwhile, the volume of electronic equipment is smaller and the functions are also more and more. The electronic device is required to have powerful functions of an internal chip or an electronic module, the running speed is faster and faster, more and more heat is generated due to the powerful functions, more and more heat is accumulated at a certain point of the chip or a certain point of the electronic module, and the heat cannot be conducted out by simply arranging a fan in a short, thin, light and small space of the electronic device or is difficult to conduct out the heat simply, so that the working performance of the chip or the electronic module is reduced and the working life is shortened under a high-temperature environment, and therefore, how to quickly and effectively transfer out the heat in the electronic device becomes an objective requirement.
The electric insulating film is a thin plastic sheet and can be applied to electronic elements of the following devices: computers, printers, facsimile machines, home appliances, audio equipment, video equipment, telephones, radios, engines, generators, wires, cables, etc., but insulation alone is not sufficient for more needs, and how to attach moisture and heat resistant functions to an insulating film is a problem to be solved.
Disclosure of Invention
(one) solving the technical problems
The invention aims to solve the problem of poor moisture and heat resistance 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: a carrier film, an insulating layer formed on the carrier film, and a hydrophobic film formed on the insulating layer, wherein the carrier film is prepared from ethylene propylene rubber which is an elastic polymer, and Al with high vacancy defects is modified by hydrophobic property 2 O 3 GaN and glyceryl monostearate, and the insulating layer is made of insulating polymer polyimide and hydrophobically modified Al with high vacancy defect 2 O 3 GaN, glyceryl monostearate, the hydrophobic film is prepared by coating fluorinated solution containing paraffin-silicon on polytetrafluoroethylene plate, and the hydrophobically modified high vacancy defect Al 2 O 3 GaN is prepared by hydrothermal reaction, calcination, high-temperature annealing and hydrophobic modification.
The invention also provides a moisture-proof heat-conducting insulation materialThe preparation method of the edge film comprises the following steps: (1) Weighing Al (NO) 3 ) 3 ·9H 2 Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/LNaOH solution to pH of about 9, stirring at 120deg.C for 1 hr, filtering to obtain precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5deg.C/min, and annealing to obtain Al with high vacancy defect 2 O 3 /GaN;
(2) Al with high vacancy defect 2 O 3 Dispersing GaN in water to obtain a solution, adding fatty acid with carbon number of 6 or more, stirring in water bath at constant temperature, and drying in a drying oven at constant temperature to obtain lipophilic high vacancy defect Al 2 O 3 GaN, adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent volatilizes completely to obtain a mixture, and placing the mixture in ammonia gas atmosphere for pyrolysis treatment to obtain hydrophobically modified high vacancy defect Al 2 O 3 /GaN;
(3) Weighing elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die, molding, and cooling to continuously curl to obtain melt-extruded carrier film with width of 320mm by using a single-shaft extruder with diameter of 30mm and powder sintering filter with nominal diameter of 20 μm;
(4) Weighing insulating polymer polyimide and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die, forming film, cooling, and continuously crimping to obtain melt extruded insulating layer with width of 320 mm;
(5) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(6) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the lower layer and the upper layer can be tightly adhered into a whole, and the moisture-proof heat-conducting insulating film is obtained.
Preferably, al (NO 3 ) 3 ·9H 2 The mass ratio of O, distilled water and GaN is 1.76-2.46:40-50:0.3-0.5, the drying temperature is 100-110 ℃, the drying time is 2-3 hours, the calcining temperature is 350-400 ℃, the calcining time is 1.5-2 hours, the annealing temperature is 800-900 ℃, and the annealing time is 5-8 minutes.
Preferably, the Al with high vacancy defect in the step (2) 2 O 3 The mass ratio of the GaN to the water to the fatty acid with the carbon number of more than 6 is 8-10:15-30:0.2-0.5, and the stirring temperature is 50-80 ℃.
Preferably, the elastomeric polymer ethylene propylene rubber in the step (3) is hydrophobically modified with high vacancy-defect Al 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film forming speed is 2-2.5m/min.
Preferably, the insulating polymer polyimide in the step (4), hydrophobically modified high vacancy-defective Al 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film forming speed is 2-2.5m/min.
Preferably, the mass ratio of carboxylated paraffin wax, polyvinylidene fluoride, hexafluoropropylene, 3-aminopropyl triethoxysilane, ethanol, ethyl orthosilicate, water, ethanol, 1H, 2H-perfluoro decyl trichlorosilane 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.
Compared with the prior art, the method has the beneficial effects that:
(1) According to the moisture-proof heat-conducting insulating film and the preparation method thereof, provided by the invention, the hydrophobic film prepared by coating the fluorinated liquid containing paraffin-silicon on the polytetrafluoroethylene plate has a hydrophobic effect, and the hydrophobic modified Al with high vacancy defects 2 O 3 GaN can capture charge carriers in water, accelerate charge recombination, inhibit conduction and hydrophobically modify Al with high vacancy defects 2 O 3 GaN can play a role in synergy with the hydrophobic film for moisture resistance.
(2) According to the moisture-resistant heat-conducting insulating film and the preparation method thereof provided by the invention, both the carrier film and the insulating layer are filled with the Al with the hydrophobic modified high vacancy defect 2 O 3 GaN overcomes the problems of low heat conductivity and poor heat conductivity of the polymer, and the carrier layer adopts an elastic polymer ethylene propylene rubber, which is beneficial to better contact with circuit devices.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO) 3 ) 3 ·9H 2 The mass ratio of O, distilled water and GaN is 1.76:40:0.3, and Al with high vacancy defect is prepared 2 O 3 The mass ratio of GaN, water and fatty acid with more than 6 carbon atoms is 8:15:0.2, and the elastic polymer and the Al with the hydrophobic modified high vacancy defect are prepared 2 O 3 GaN, single hardThe mass ratio of the glyceride fatty acid is 70:5:3, and the insulating polymer and the hydrophobically modified Al with high vacancy defect 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 70:5:3, and the mass ratio of the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene, 3-aminopropyl triethoxysilane, ethanol, tetraethoxysilane, water, ethanol, 1H, 2H-perfluoro decyl trichlorosilane is 1:2:2:1:5:1:2:20:0.01.
(1) Weighing Al (NO) 3 ) 3 ·9H 2 Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/LNaOH solution to pH of about 9, stirring at 120deg.C for 1 hr, filtering to obtain precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5deg.C/min, annealing, setting drying temperature to 100deg.C, drying for 2 hr, calcining at 350deg.C for 1.5 hr, annealing at 800deg.C for 5min, and obtaining Al with high vacancy defect 2 O 3 /GaN;
(2) Al with high vacancy defect 2 O 3 Dispersing GaN in water to obtain a solution, adding fatty acid with carbon number of 6 or more, stirring in water bath at 50deg.C, and drying in a drying oven at constant temperature to obtain lipophilic high vacancy defect Al 2 O 3 GaN, adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent volatilizes completely to obtain a mixture, and placing the mixture in ammonia gas atmosphere for pyrolysis treatment to obtain hydrophobically modified high vacancy defect Al 2 O 3 /GaN;
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die at 250deg.C at film-forming speed of 2m/min with a single-shaft extruder with diameter of 30mm and powder sintering filter with nominal diameter of 20 μm, molding, and cooling to continuously curl to obtain melt-extruded carrier film with width of 320 mm;
(4) Weighing insulating polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from a T die at 250 deg.C at 2m/min by using a single-shaft extruder with diameter of 30mm and a powder sintering filter with nominal diameter of 20 μm, and cooling to continuously curl to obtain melt-extruded insulating layer with width of 320 mm;
(5) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(6) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the lower layer and the upper layer can be tightly adhered together to obtain the moisture-proof heat-conducting insulating film.
Example 2
A preparation method of a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO) 3 ) 3 ·9H 2 The mass ratio of O, distilled water and GaN is 1.78:42:0.35, and Al with high vacancy defect is prepared 2 O 3 The mass ratio of GaN, water and fatty acid with more than 6 carbon atoms is 8.5:16:0.25, and the elastic polymer and the Al with high vacancy defect are modified by hydrophobic property 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 75:6:3.5, and the insulating polymerization is carried outMaterial, hydrophobically modified high vacancy defect Al 2 O 3 The mass ratio of the/GaN and the glyceryl monostearate is 78:10:4, and the mass ratio of the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene, 3-aminopropyl triethoxysilane, ethanol, tetraethoxysilane, water, ethanol, 1H, 2H-perfluoro decyl trichlorosilane is 1.2:2.2:2:1.2:5.2:1.2:2.5:21:0.015.
(1) Weighing Al (NO) 3 ) 3 ·9H 2 Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/LNaOH solution to pH of about 9, stirring at 120deg.C for 1 hr, filtering to obtain precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5deg.C/min, annealing, setting drying temperature at 102 deg.C for 2.2 hr, calcining at 355 deg.C for 1.55 hr, annealing at 82 deg.C for 5.5 min to obtain Al with high vacancy defect 2 O 3 /GaN;
(2) Al with high vacancy defect 2 O 3 Dispersing GaN in water to obtain a solution, adding fatty acid with carbon number of 6 or more, stirring in water bath at 60deg.C, and drying in a drying oven to obtain lipophilic high vacancy defect Al 2 O 3 GaN, adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent volatilizes completely to obtain a mixture, and placing the mixture in ammonia gas atmosphere for pyrolysis treatment to obtain hydrophobically modified high vacancy defect Al 2 O 3 /GaN;
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die at 254 deg.C with film forming speed of 2.1m/min by using a single shaft extruder with diameter of 30mm and powder sintering filter with nominal diameter of 20 μm, molding, and cooling to continuously curl to obtain melt-extruded carrier film with width of 320 mm;
(4) Weighing insulating polymer and hydrophobically modified Al with high vacancy defect 2 O 3 GaN/glyceryl monostearateMixing, using a single-shaft extruder with the diameter of 30mm and a powder sintering filter with the nominal diameter of 20 mu m, carrying out melt extrusion on the mixture from a T die, wherein the melt extrusion temperature is 255 ℃, the film forming speed is 2.1m/min, forming a film, and continuously curling through cooling to obtain a melt extrusion insulating layer with the width of 320 mm;
(5) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(6) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the lower layer and the upper layer can be tightly adhered together to obtain the moisture-proof heat-conducting insulating film.
Example 3
A preparation method of a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO) 3 ) 3 ·9H 2 The mass ratio of O, distilled water and GaN is 2.2:48:0.45, and Al with high vacancy defect is prepared 2 O 3 The mass ratio of GaN, water and fatty acid with more than 6 carbon atoms is 9:19:0.4, and the elastic polymer and the Al with high vacancy defect are modified by hydrophobic property 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 88:12:4.8, and the insulating polymer and the hydrophobic modified high vacancy defect are formedAl of (2) 2 O 3 The mass ratio of/GaN to glycerol monostearate is 87:14.5:4.9, and the mass ratio of carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene, 3-aminopropyl triethoxysilane, ethanol, ethyl orthosilicate, water, ethanol, 1H, 2H-perfluoro decyl trichlorosilane is 2:4:4:2:7:1.8:3:23:0.02.
(1) Weighing Al (NO) 3 ) 3 ·9H 2 Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/LNaOH solution to pH of about 9, stirring at 120deg.C for 1 hr, filtering to obtain precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5deg.C/min, annealing, setting drying temperature at 106 deg.C for 2.4 hr, calcining at 360 deg.C for 1.7 hr, annealing at 890 deg.C for 7 min to obtain Al with high vacancy defect 2 O 3 /GaN;
(2) Al with high vacancy defect 2 O 3 Dispersing GaN in water to obtain a solution, adding fatty acid with carbon number of 6 or more, stirring in water bath at 70deg.C, and drying in a drying oven at constant temperature to obtain lipophilic high vacancy defect Al 2 O 3 GaN, adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent volatilizes completely to obtain a mixture, and placing the mixture in ammonia gas atmosphere for pyrolysis treatment to obtain hydrophobically modified high vacancy defect Al 2 O 3 /GaN;
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from a T die at 265 deg.C by using a single-shaft extruder with diameter of 30mm and a powder sintering filter with nominal diameter of 20 μm, molding at 2.4m/min, and continuously crimping by cooling to obtain a melt-extruded carrier film with width of 320 mm;
(4) Weighing insulating polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, extruding with single shaft of 30mm diameterMelt-extruding the mixture from a T die at 265 ℃ and film-forming speed of 2.4m/min, and continuously curling after cooling to obtain a melt-extruded insulating layer with width of 320 mm;
(5) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(6) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the lower layer and the upper layer can be tightly adhered together to obtain the moisture-proof heat-conducting insulating film.
Example 4
A preparation method of a moisture-resistant heat-conducting insulating film comprises the following steps:
the material ratio is as follows: al (NO) 3 ) 3 ·9H 2 The mass ratio of O, distilled water and GaN is 2.46:50:0.5, and Al with high vacancy defect is prepared 2 O 3 GaN, water, fatty acid with more than 6 carbon atoms in a mass ratio of 10:30:0.5, elastic polymer, hydrophobically modified Al with high vacancy defect 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 90:15:5, and the insulating polymer and the hydrophobically modified Al with high vacancy defects 2 O 3 GaN, monostearinThe mass ratio of the glyceride is 90:15:5, and the mass ratio of carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene, 3-aminopropyl triethoxysilane, ethanol, ethyl orthosilicate, water, ethanol, 1H, 2H-perfluoro decyl trichlorosilane is 3:5:5:3:8:2:4:25:0.03.
(1) Weighing Al (NO) 3 ) 3 ·9H 2 Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/LNaOH solution to pH of about 9, stirring at 120deg.C for 1 hr, filtering to obtain precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5deg.C/min, annealing, setting drying temperature at 110deg.C for 2-3 hr, calcining at 400deg.C for 2 hr, annealing at 900deg.C for 8 min to obtain Al with high vacancy defect 2 O 3 /GaN;
(2) Al with high vacancy defect 2 O 3 Dispersing GaN in water to obtain a solution, adding fatty acid with carbon number of 6 or more, stirring in water bath at 80deg.C, and drying in a drying oven to obtain lipophilic high vacancy defect Al 2 O 3 GaN, adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent volatilizes completely to obtain a mixture, and placing the mixture in ammonia gas atmosphere for pyrolysis treatment to obtain hydrophobically modified high vacancy defect Al 2 O 3 /GaN;
(3) Weighing elastic polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die at 270 deg.C with a film forming speed of 2.5m/min by using a single-shaft extruder with diameter of 30mm and a powder sintering filter with nominal diameter of 20 μm, molding, and continuously crimping by cooling to obtain a melt-extruded carrier film with width of 320 mm;
(4) Weighing insulating polymer and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, sintering and filtering powder with diameter of 30mm and nominal diameter of 20 μmA device for melt-extruding the mixture from a T die, wherein the melt-extruding temperature is 270 ℃, the film-forming speed is 2.5m/min, and the film-forming is continuously curled by cooling to obtain a melt-extruded insulating layer with the width of 320 mm;
(5) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(6) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the lower layer and the upper layer can be tightly adhered together to obtain the moisture-proof heat-conducting insulating film.
Comparative example 1
A preparation method of a heat-conducting insulating film comprises the following steps:
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 elastic polymer and glyceryl monostearate, mixing, melt extruding the mixture from T die at 250deg.C with film forming speed of 2m/min by using a single-shaft extruder with diameter of 30mm and powder sintering filter with nominal diameter of 20 μm, molding, and cooling to continuously curl to obtain melt-extruded carrier film with width of 320 mm;
(2) Weighing insulating polymer and glyceryl monostearate, mixing, melt extruding the mixture from a T die at 250 ℃ at a film forming speed of 2m/min by using a single-shaft extruder with a diameter of 30mm and a powder sintering filter with a nominal diameter of 20 mu m, and continuously curling after cooling to obtain a melt extruded insulating layer with a width of 320 mm;
(3) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(4) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(5) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the lower layer and the upper layer can be tightly adhered together to obtain the moisture-proof heat-conducting insulating film.
Insulating thermal conductivity testing was performed on the film samples in examples and comparative examples: the breakdown field intensity is measured by using a BTF-038-50kV voltage breakdown experiment instrument, and the adopted test standard is GB/T1408.1-2006; the test standard of the DRL-III heat conductivity coefficient tester for thermal conductivity test is ASTMD5470-2006, the test method is a transient plane heat source method, and the test result of the insulation heat conductivity is shown in the following table 1.
TABLE 1
As can be seen from Table 1, the film samples of examples 1 to 4 were higher in breakdown field strength and thermal conductivity than those of the film sample of comparative example because the film material of comparative example 1 was free of Al added with hydrophobically modified high vacancy defects 2 O 3 GaN, poor heat conduction and insulation, shows that 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 angle of the insulating film samples in examples 1 to 4 was greater than that of the insulating film sample in comparative example 1, indicating that the insulating film samples prepared according to the present invention had 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 characteristics 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 disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (7)
1. The preparation method of the moisture-resistant heat-conducting insulating film is characterized by comprising the following steps of:
(1) Weighing Al (NO) 3 ) 3 ·9H 2 Dissolving O in distilled water, adding GaN, mixing under continuous stirring, dripping 1mol/L NaOH solution to pH 9, stirring at 120deg.C for 1 hr, filtering to obtain precipitate powder, washing with distilled water for 5 times, drying, calcining the obtained solid powder at heating rate of 5deg.C/min, and annealing to obtain Al with high vacancy defect 2 O 3 /GaN;
(2) Al with high vacancy defect 2 O 3 Dispersing GaN in water to obtain a solution, adding fatty acid with carbon number of 6 or more, stirring in water bath at constant temperature, and drying in a drying oven at constant temperature to obtain lipophilic high vacancy defect Al 2 O 3 GaN, adding siloxane coupling agent and organic solvent, mixing, stirring and hydrolyzing until the organic solvent volatilizes completely to obtain a mixture, and placing the mixture in ammonia gas atmosphere for pyrolysis treatment to obtain hydrophobically modified high vacancy defect Al 2 O 3 /GaN;
(3) Weighing elastic polymer ethylene propylene rubber and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die, molding, and cooling to continuously curl to obtain melt-extruded carrier film with width of 320mm by using a single-shaft extruder with diameter of 30mm and powder sintering filter with nominal diameter of 20 μm;
(4) Weighing insulating polymer polyimide and hydrophobically modified Al with high vacancy defect 2 O 3 Mixing GaN and glyceryl monostearate, melt extruding the mixture from T die, forming film, cooling, and continuously crimping to obtain melt extruded insulating layer with width of 320 mm;
(5) Dispersing paraffin into concentrated nitric acid, performing ultrasonic treatment for 1h, performing suction filtration, washing until filtrate is neutral, freeze-drying, sealing and preserving for standby, placing the treated paraffin into mixed acid with the volume ratio of concentrated sulfuric acid to concentrated nitric acid of 1:3, boiling for 1h, performing vacuum filtration, washing the paraffin to be neutral by using secondary distilled water, and performing freeze-drying for standby to obtain carboxylated paraffin;
(6) Weighing carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane, adding the carboxylated paraffin, polyvinylidene fluoride, hexafluoropropylene and 3-aminopropyl triethoxysilane into an ethanol solution, stirring for 5 minutes at the rotation speed of 60 revolutions per minute, adding tetraethoxysilane, water and ethanol, mixing and stirring for 15 minutes, repeatedly washing with deionized water, drying at the temperature of 60 ℃, finally, placing the modified paraffin into a container, adding 1H, 2H-perfluoro decyl trichlorosilane, placing the container into a vacuum furnace, placing the container at the temperature of 100 ℃ for 24 hours to obtain paraffin-silicon-containing fluorinated solution, and coating the paraffin-silicon-containing fluorinated solution on a polytetrafluoroethylene plate to prepare a hydrophobic membrane;
(7) The carrier film, the insulating layer and the hydrophobic film are stacked together, and air between each adjacent stacked layers is discharged under pressure by a hydraulic press, so that the carrier film, the insulating layer and the hydrophobic film can be tightly adhered together to obtain the moisture-proof heat-conducting insulating film.
2. The method for producing a moisture-resistant, heat-conductive, insulating film according to claim 1, wherein Al (NO 3 ) 3 ·9H 2 The mass ratio of O, distilled water and GaN is 1.76-2.46:40-50:0.3-0.5, the drying temperature is 100-110 ℃, the drying time is 2-3 hours, the calcining temperature is 350-400 ℃, the calcining time is 1.5-2 hours, the annealing temperature is 800-900 ℃, and the annealing time is 5-8 minutes.
3. The method for producing a moisture-resistant heat-conductive insulating film according to claim 1, wherein Al having a high vacancy defect in the step (2) 2 O 3 The mass ratio of the GaN to the water to the fatty acid with the carbon number of more than 6 is 8-10:15-30:0.2-0.5, and the stirring temperature is 50-80 ℃.
4. The method for preparing a moisture-resistant heat-conductive insulating film according to claim 1, wherein the elastic polymer ethylene propylene rubber and the hydrophobic polymer in the step (3)Water modified high vacancy defect Al 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film forming speed is 2-2.5m/min.
5. A method for producing a moisture-resistant heat-conductive insulating film according to claim 1, wherein said insulating polymer polyimide, hydrophobically modified high vacancy-defect Al in step (4) 2 O 3 The mass ratio of the GaN to the glyceryl monostearate is 70-90:5-15:3-5, the melt extrusion temperature is 250-270 ℃, and the film forming speed is 2-2.5m/min.
6. The method for producing a moisture-resistant, heat-conductive, insulating film according to claim 1, wherein the mass ratio of carboxylated paraffin wax, polyvinylidene fluoride, hexafluoropropylene, 3-aminopropyl triethoxysilane, ethanol solution, ethyl orthosilicate, water, ethanol, 1h,2 h-perfluorodecyl trichlorosilane 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.
7. A moisture-resistant heat-conductive insulating film prepared by the preparation method according to any one of claims 1 to 6.
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