CN118085758A - High-heat-conductivity insulating adhesive film and preparation method thereof - Google Patents
High-heat-conductivity insulating adhesive film and preparation method thereof Download PDFInfo
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- CN118085758A CN118085758A CN202410329259.4A CN202410329259A CN118085758A CN 118085758 A CN118085758 A CN 118085758A CN 202410329259 A CN202410329259 A CN 202410329259A CN 118085758 A CN118085758 A CN 118085758A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 79
- 239000002313 adhesive film Substances 0.000 title claims abstract description 54
- 239000000945 filler Substances 0.000 claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 52
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 52
- 239000011159 matrix material Substances 0.000 claims abstract description 44
- 239000012790 adhesive layer Substances 0.000 claims abstract description 40
- 239000003822 epoxy resin Substances 0.000 claims abstract description 33
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 33
- 150000002148 esters Chemical class 0.000 claims abstract description 30
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 26
- 239000004917 carbon fiber Substances 0.000 claims abstract description 26
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 23
- 239000010426 asphalt Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 238000002156 mixing Methods 0.000 claims description 40
- 239000011231 conductive filler Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 24
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
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- 229920002379 silicone rubber Polymers 0.000 description 4
- 239000004945 silicone rubber Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
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- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
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- 125000004185 ester group Chemical group 0.000 description 1
- GADHUKQASVRNQF-UHFFFAOYSA-N ethyl 2-(2,4-dihydroxyphenyl)acetate Chemical group CCOC(=O)CC1=CC=C(O)C=C1O GADHUKQASVRNQF-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The application relates to the technical field of electronic packaging, and particularly discloses a high-heat-conductivity insulating adhesive film and a preparation method thereof. The high-heat-conductivity insulating adhesive film comprises a base material and an insulating adhesive layer arranged on any side of the base material, wherein the insulating adhesive layer comprises the following raw materials in parts by weight: 30-40 parts of multifunctional epoxy resin, 20-40 parts of phenolic resin, 30-40 parts of active ester, 8-16 parts of silane cross-linking agent, 10-20 parts of solvent, 80-90 parts of modified silicon filler and 80-100 parts of heat conducting filler, wherein the heat conducting filler comprises aluminum nitride, carbon nano tubes, asphalt-based carbon fibers and an insulating high polymer matrix. The high-heat-conductivity insulating adhesive film has the advantages of excellent insulativity and high heat conductivity; in addition, the preparation method provided by the application has the advantages of improving the thermal conductivity of the insulating adhesive film and optimizing the adhesive force of the insulating adhesive film.
Description
Technical Field
The application relates to the technical field of electronic packaging, in particular to a high-heat-conductivity insulating adhesive film and a preparation method thereof.
Background
The insulating adhesive film is a material widely applied in the electronic industry, and particularly plays important roles in insulation, protection, fixation and the like in the field of electronic packaging. Along with the rapid development of electronic and electric technology, the volumes of various electronic components and equipment are continuously reduced, the integration density is continuously improved, the power density of unit area is remarkably increased, the heat generation is more concentrated, and the requirements on packaging materials are also higher and higher. The performance of the insulating adhesive film as an important packaging material directly affects the reliability, stability and working efficiency of the electronic device.
The insulating adhesive film is prepared by mixing raw materials such as epoxy resin, active ester, polyacrylate, organic silicon and the like with fillers such as heat-conducting ceramic split bodies and the like, coating the mixture on base materials such as PET, PI, glass fiber cloth and the like, and drying the mixture.
Aiming at the related technology, the inventor finds that the insulating adhesive film on the market at present mainly comprises two materials, namely polyacrylate and silicone rubber made of organic silicon, wherein the polyacrylate is a monomer with unsaturated double bonds, and the monomer can be subjected to free radical polymerization reaction under the action of a catalyst to form a self-adhesive polymer, so that a relatively firm adhesive force can be formed under the action of a small amount, the film can be conveniently adhered, but the heat resistance and the heat conductivity are low; silicone rubber has excellent high temperature resistance, thermal oxidative aging resistance and excellent insulating property, but the thermal conductivity of the silicone rubber raw material silicone is only 0.2W/(m·k), the heat transfer efficiency is very low, the silicone is a nonpolar polymer, the intermolecular force is low, the bonding force is low, and especially when the heat conducting filler is highly filled, the bonding force of the silicone rubber can be further reduced or even lose viscosity, which is unfavorable for preparing the heat conducting insulating adhesive film with high reliability, so that the finally prepared insulating adhesive film has poor thermal conductivity and cannot effectively conduct heat away from a heating source, thereby limiting the performance and reliability of electronic equipment.
Disclosure of Invention
In order to improve the heat conducting performance of the insulating adhesive film and optimize the adhesive force of the insulating adhesive film, the application provides a high-heat conducting insulating adhesive film and a preparation method thereof.
In a first aspect, the present application provides a high thermal conductive insulating film, which adopts the following technical scheme:
The high-heat-conductivity insulating adhesive film comprises a base material and insulating adhesive layers arranged on any side of the base material, wherein the insulating adhesive layers comprise the following raw materials in parts by weight: 30-40 parts of multifunctional epoxy resin, 20-40 parts of phenolic resin, 30-40 parts of active ester, 8-16 parts of silane cross-linking agent, 10-20 parts of solvent, 80-90 parts of modified silicon filler and 80-100 parts of heat conducting filler; the heat conducting filler comprises aluminum nitride, carbon nano tubes, asphalt-based carbon fibers and an insulating high polymer matrix in a mass ratio of (1-2) to (20-30).
By adopting the technical scheme, the carbon nano tube and the asphalt-based carbon fiber in the heat conduction filler are the fillers with higher heat conductivity, higher heat stability and larger specific surface area, and the contact area between the conductive filler and other raw materials of the insulating adhesive layer can be increased by the large specific surface area, so that the heat conduction efficiency is improved.
The asphalt-based carbon fiber has a fiber network structure, and can form the fiber network structure in the insulating adhesive layer, so that more paths are provided for heat conduction in the insulating adhesive layer; the carbon nano tube is of a nano-scale and has a one-dimensional structure, and can be used as a bridge for heat transfer to connect dispersed heat conducting filler particles together, so that the distribution state of the insulating adhesive layer matrix material can be changed, and more heat conduction paths are formed; the mixing of two fillers of different morphology and size can exert a positive synergistic effect, forming more heat conduction paths in the insulating polymer matrix.
Aluminum nitride has low molar mass, strong bonding and a relatively simple crystal structure, and when the insulating adhesive film is subjected to heat, the aluminum nitride can rapidly disperse and transfer the heat, so that the heat is effectively prevented from accumulating locally, and the overall heat dissipation performance of the insulating adhesive film is improved.
The insulating polymer matrix has good insulativity, is compounded with aluminum nitride, carbon nano tubes and asphalt-based carbon fibers, can form a barrier between the aluminum nitride, the carbon nano tubes and the asphalt-based carbon fibers, reduces migration of electrons, further improves insulating performance of an insulating adhesive layer, and reduces conductive influence of the aluminum nitride, the carbon nano tubes and the asphalt-based carbon fibers on the insulating adhesive layer.
The silane cross-linking agent forms a silicon-oxygen bond through condensation reaction with hydroxyl in the polymer, so that cross-linking is realized, the insulating adhesive layer has excellent cross-linking effect and water resistance, the adhesive force between the adhesive layer and a substrate can be improved, and the durability of the adhesive layer is improved.
Optionally, the preparation method of the heat conducting filler comprises the following steps:
Mixing a carbon nano tube with a fluorocarbon surfactant for surface treatment to obtain a modified carbon nano tube, wherein the dosage of the fluorocarbon surfactant is 1-2% of the mass of the carbon nano tube; mixing an insulating high polymer matrix with a matrix solvent to form matrix emulsion, wherein the dosage of the matrix solvent is 10-15% of the mass of the insulating high polymer matrix; mixing the modified carbon nano tube with aluminum nitride and asphalt-based carbon fiber, adding the mixture into the matrix emulsion, and drying, hot-pressing and crushing the mixture to obtain the heat-conducting filler.
By adopting the technical scheme, the carbon nano tube is subjected to surface active treatment when the heat conducting filler is prepared, hydrophobic groups of surfactant molecules are adsorbed on the surface of the carbon nano tube through physical action, the adsorption action can reduce the surface energy of the carbon nano tube, enhance the dispersibility of the carbon nano tube in a polymer matrix, prevent the carbon nano tube from agglomerating, effectively reduce interface thermal resistance and improve the heat conductivity of an insulating adhesive layer; the fluorocarbon surfactant has excellent chemical stability, higher resistivity and low ionic conductivity due to the fluorine atom, and can prevent current from passing through and improve the insulating performance of the insulating adhesive layer.
Optionally, the carbon nanotubes are subjected to the following pretreatment prior to mixing with the surfactant: heating the carbon nano tube to 600-800 ℃ in the atmosphere of inert gas, and treating for 1-2h at high temperature.
By adopting the technical scheme, impurity particles possibly exist in the carbon nano tube, the carbon nano tube is subjected to high-temperature heat treatment and purification, and the impurity particles undergo pyrolysis reaction at high temperature, so that most of impurities are eliminated, the purity of the carbon nano tube is improved, and the heat conductivity of the carbon nano tube is improved.
Optionally, the modified carbon nanotubes and aluminum nitride, pitch-based carbon fibers are subjected to the following pretreatment before being mixed and added into the matrix emulsion: mixing the modified carbon nano tube with aluminum nitride and asphalt-based carbon fiber, and grinding for 1-2h.
By adopting the technical scheme, the carbon nano tube is better coated on the surfaces of aluminum nitride and asphalt-based carbon fibers during mixing, and after the thermal compression reaction, a separated network structure can be formed in the heat-conducting filler, so that the contact area between the heat-conducting fillers is improved, and the heat conductivity of the insulating adhesive film is improved.
Optionally, the modified silicon filler comprises polymethyl vinyl siloxane and boric acid in the mass ratio of (10-15) to (1-2).
By adopting the technical scheme, the modified silicon filler is a hybrid chain organic silicon polymer formed by substituting one or more Si on a molecular chain of a siloxane polymer Si-O-Si with boron, and the Si-O: B structure can be formed by utilizing a boron electron-deficient structure and oxygen atoms on the molecular chain, so that the system can be endowed with good self-adhesiveness and heat resistance, the adhesive force of an insulating adhesive layer is effectively improved, and the situation that the adhesive force of the insulating adhesive layer is reduced due to filling of a heat conducting filler can be compensated by adding the modified silicon filler into the raw material of the insulating adhesive layer.
Optionally, the preparation method of the modified silicon filler comprises the following steps:
Mixing polymethyl vinyl siloxane and boric acid, and reacting at 170-200 ℃ for 1.5-2 hours to obtain viscous polyborosiloxane; adding white carbon black and a peroxide vulcanizing agent into the viscous polyborosiloxane for vulcanization reaction and mixing, cooling and crushing to obtain modified silicon filler, wherein the vulcanization reaction conditions are as follows: the mass ratio of the polymethyl vinyl siloxane to the white carbon black to the peroxide vulcanizing agent is (10-15) 1:1 at 150-170 ℃ under the pressure of 8-10MPa for 10-20 min.
By adopting the technical scheme, the composite of the polyborosiloxane and the white carbon black is facilitated under the condition of high-temperature vulcanization of the oxide, the prepared modified silicon filler has good bonding performance, and the product obtained by peroxide vulcanization has higher stretching, tearing and wear resistance, and particularly can show excellent performance at high temperature.
Optionally, the multifunctional epoxy resin is selected from one or more of resorcinol-formaldehyde epoxy resin, naphthalene-based epoxy resin, biphenyl epoxy resin, and phenolic epoxy resin.
By adopting the technical scheme, the resorcinol-formaldehyde epoxy resin, the naphthyl epoxy resin, the biphenyl epoxy resin and the phenolic epoxy resin have higher heat resistance, insulativity, moisture resistance and chemical stability, the performances of different multifunctional epoxy resins have certain difference, and the performances of various multifunctional epoxy resins can be complemented by compounding and using, so that the overall performance of the insulating adhesive film is improved.
Optionally, the insulating polymer matrix is vinyl resin.
By adopting the technical scheme, the vinyl resin is thermosetting resin with excellent performance, has excellent electrical insulation performance, can effectively isolate current and prevent electric shock and electric fire, and can bear severe environments such as high temperature, humidity and the like and maintain stable insulation performance.
Optionally, the active ester is selected from one or more of an anhydride-based active ester, a carboxylic acid-based active ester, and a phenolic ester-based active ester.
By adopting the technical scheme, as the active ester is an organic compound with an active function, the structure of the active ester contains ester groups, the active ester can react with other compounds through the rupture of ester bonds, functional groups of the active ester generally react with functional groups such as hydroxyl groups, amino groups and the like in a polymer in an insulating adhesive layer to form chemical bond connection, so that the crosslinking density and strength of the insulating adhesive layer are increased, and the acid anhydride active ester, the carboxylic acid active ester and the phenol ester active ester have good electrical insulation property and higher reactivity and can react with the functional groups in the polymer to form a stable crosslinking structure, so that the integral strength of the insulating adhesive layer is improved.
In a second aspect, the application provides a preparation method of a high-heat-conductivity insulating adhesive film, which adopts the following technical scheme: the preparation method of the high-heat-conductivity insulating adhesive film comprises the following steps: mixing and stirring multifunctional epoxy resin, phenolic resin, active ester, a cross-linking agent, modified silicon filler, heat-conducting filler and a solvent for 1-2 hours to prepare insulating slurry; coating the insulating slurry on a substrate to form an insulating adhesive layer; and drying, extruding to form a film and rolling the insulating adhesive layer to obtain the insulating adhesive film.
Through adopting above-mentioned technical scheme, mix the back with the raw materials and coat and form the insulating glue layer on the substrate, help improving the adhesion of raw materials and substrate for whole insulation structure is more stable, is difficult for appearing delamination or the phenomenon that drops.
In summary, the application has the following beneficial effects:
1. According to the application, the carbon nano tube with good heat conductivity, aluminum nitride and asphalt-based carbon fiber are used as the heat conduction filler, the carbon nano tube is of a nano level, has a larger surface area, and can increase the contact area between the heat conduction filler and other raw materials of the insulating adhesive layer; the asphalt-based carbon fiber can form a fiber network structure in the insulating adhesive layer, so that a bridge is established for heat conduction in the insulating adhesive layer, and more paths are provided; the aluminum nitride has excellent heat conduction performance, and more heat conduction passages can be formed in the insulating adhesive layer by the synergistic effect of the three components, so that the heat conduction performance of the insulating adhesive layer is effectively improved.
2. According to the application, the modified silicon filler is endowed with good adhesive property by modifying the polymethyl vinyl siloxane in a mode of modifying the boron element to form the hybrid chain organosilicon polymer, so that the adhesive force of the insulating adhesive layer is effectively improved, and the effect of compensating for the reduction of the adhesive property of the insulating adhesive layer caused by filling of the heat conducting filler is achieved.
3. According to the preparation method, the carbon nanotubes in the heat conducting material are purified and subjected to surface treatment, the surface energy of the carbon nanotubes is reduced through the adsorption effect of the surfactant, the carbon nanotubes can be effectively prevented from agglomerating, and the interface thermal resistance is reduced; by purifying the carbon nanotubes, the influence of impurity particles possibly existing in the carbon nanotubes on the thermal conductivity of the carbon nanotubes is removed, and the thermal conductivity of the insulating adhesive layer is further improved.
Detailed Description
The following examples illustrate the application in further detail.
Preparation example
Preparation examples 1 to 10 of thermally conductive filler
The fluorocarbon surfactant of preparation examples 1-10 was selected from FC-209, a division of Zhonghai chemical industry, guangzhou; carbon nanotubes selected from Roen reagent 308068-56-6; asphalt-based carbon fiber, 65996-93-2, available from Hebei Feng Taiyuan energy technologies; the average particle diameter of aluminum nitride was 20. Mu.m.
Preparation example 1: the preparation method of the heat conducting filler comprises the following steps:
s1, heating the carbon nano tube to 600 ℃ in the nitrogen atmosphere, and purifying for 2 hours at a high temperature;
s2, mixing 1Kg of purified carbon nanotube with 0.01Kg of fluorocarbon surfactant for 1h to obtain a modified carbon nanotube;
s3, mixing and stirring 20Kg of insulating high polymer matrix and 2Kg of matrix solvent to form matrix emulsion, wherein the insulating high polymer matrix is vinyl resin, and the matrix solvent is methanol;
S4, mixing the modified carbon nano tube with 10Kg of aluminum nitride and 1Kg of asphalt-based carbon fiber, grinding the mixture in a ball mill at a speed of 200r/min for 2 hours, and then adding the mixture into a matrix emulsion, mixing and stirring the mixture for 4 hours to obtain a mixture;
s5, drying the mixture prepared in the step S4 in a drying oven for 3 hours, and then carrying out hot-pressing treatment on the mixture at 300 ℃ and under 15MPa, and cooling to obtain a blocky filler;
and S6, grinding the blocky filler prepared in the step S5 in a ball mill at 200r/min for 4 hours to obtain the heat-conducting filler with the average particle size of 10 mu m.
Preparation example 2: the preparation method of the heat conducting filler comprises the following steps:
s1, heating the carbon nano tube to 800 ℃ in the nitrogen atmosphere, and purifying for 1h at a high temperature;
S2, mixing 1Kg of purified carbon nanotube with 0.02Kg of fluorocarbon surfactant for 1h to obtain a modified carbon nanotube;
S3, mixing and stirring 30Kg of insulating high polymer matrix with 6Kg of matrix solvent to form matrix emulsion, wherein the insulating high polymer matrix is vinyl resin, and the matrix solvent is methanol;
S4, mixing the modified carbon nano tube with 10Kg of aluminum nitride and 2Kg of asphalt-based carbon fiber, grinding the mixture in a ball mill at a speed of 200r/min for 1h, and then adding the mixture into a matrix emulsion, mixing and stirring the mixture for 4h to obtain a mixture;
s5, drying the mixture prepared in the step S4 in a drying oven for 3 hours, and then carrying out hot-pressing treatment on the mixture at 300 ℃ and under 15MPa, and cooling to obtain a blocky filler;
And S6, grinding the blocky filler prepared in the step S5 in a ball mill at 200r/min for 4 hours to obtain the heat-conducting filler with the average particle size of 8 mu m.
Preparation example 3: the preparation of the heat conductive filler is different from preparation example 1 in that the carbon nanotube is not subjected to the high temperature purification treatment of step S1, and the other steps are the same as preparation example 1.
Preparation example 4: the preparation of the heat conductive filler is different from preparation example 1 in that the purified carbon nanotube is not subjected to the fluorocarbon surface activation treatment of step S2, and the other steps are the same as preparation example 1.
Preparation example 5: the preparation of the heat conductive filler was different from preparation example 1 in that the modified carbon nanotube and pitch-based carbon fiber were mixed and added to the matrix emulsion without grinding treatment, and the other steps were the same as preparation example 1.
Preparation example 6: the preparation of the heat conductive filler is different from that of preparation example 1 in that polyvinyl chloride is used as the insulating polymer matrix, and other steps are the same as those of preparation example 1.
Preparation example 7: the preparation method of the heat conducting filler comprises the following steps:
s1, mixing 62.6Kg of insulating high polymer with 6.2Kg of matrix solvent, stirring to form matrix emulsion, wherein the matrix of the insulating high polymer is vinyl resin, and the matrix solvent is methanol;
S2, mixing 6.3Kg of carbon nanotubes with 4.7Kg of asphalt-based carbon fibers, and then adding the mixture into the matrix emulsion, mixing and stirring for 4 hours to obtain a mixture;
S3, drying the mixture prepared in the step S2 in a drying oven for 3 hours, and then carrying out hot-pressing treatment on the mixture at 300 ℃ and 15MPa, and cooling to obtain a blocky filler;
s4, grinding the blocky filler prepared in the step S3 in a ball mill at 200r/min for 4 hours, and obtaining the heat-conducting filler with the average particle size of 18 mu m.
Preparation example 8: the preparation of the heat conductive filler was different from preparation example 7 in that no carbon nanotube was added, and the other steps were the same as preparation example 7.
Preparation example 9: the heat conductive filler was prepared in the same manner as in preparation example 7 except that the pitch-based carbon fiber was not added.
Preparation example 10: the preparation of the heat conductive filler was different from that of preparation example 7 in that aluminum nitride was not added, and the other steps were the same as those of preparation example 7.
Preparation examples 11 to 15 of modified silicon fillers
The polymethylvinylsiloxane of preparation examples 11-15 was selected from Dongjue silicone (Nanjing) Inc., 110-2; boric acid, which is selected from novel composite materials of esteem, 10043-35-3; white carbon black selected from XHG-200 of Zhejiang New England Ind; peroxide vulcanizing agent selected from Ackersinobell, 14-40B-pd.
Preparation example 11: the preparation method of the modified silicon filler comprises the following steps:
S1, mixing 62Kg of polymethylvinylsiloxane and 6.2Kg of boric acid, and reacting at 200 ℃ for 1.5 hours to obtain viscous polyborosiloxane;
S2, adding 6.2Kg of white carbon black and 6.2Kg of peroxide vulcanizing agent into the viscous polyborosylsiloxane obtained in the step S1, mixing for 10min at 170 ℃ under the pressure of 8MPa, cooling and crushing to obtain the modified silicon filler.
Preparation example 12: the preparation method of the modified silicon filler comprises the following steps:
S1, mixing 70.5Kg of polymethylvinylsiloxane and 9.4Kg of boric acid, and reacting at 170 ℃ for 2 hours to obtain viscous polyborosiloxane;
s2, adding 4.8Kg of white carbon black and 4.8Kg of peroxide vulcanizing agent into the viscous polyborosylsiloxane obtained in the step S1, mixing for 20min at 150 ℃ under the pressure of 10MPa, cooling and crushing to obtain the modified silicon filler.
Preparation example 13: the difference from preparation example 10 is that no white carbon black was added in step S2, and the other steps are the same as in preparation example 10.
Preparation example 14: the difference from preparation example 10 is that no peroxide curing agent was added in step S2, and the rest of the steps were the same as preparation example 10.
Preparation example 15: the difference from preparation example 10 is that white carbon black and a peroxide vulcanizing agent are not added in step S2, and the rest of the steps are the same as those of preparation example 10.
Examples
Example 1: the high-heat-conductivity insulating adhesive film comprises a base material and an insulating adhesive layer arranged on one side of the base material, wherein the multifunctional epoxy resin in the raw material of the insulating adhesive layer is resorcinol type epoxy resin, and is selected from gold-made chemical industry, 1564513; the phenolic resin is selected from the chemical engineering of Jinan Nuo, 9003-35-4; the active ester is carboxylic acid active ester selected from Guangzhou and pharmaceutical technology, 2592-19-0; the silane cross-linking agent is selected from Xuan new material technology, 550.
The high-heat-conductivity insulating adhesive film is prepared by the following method:
S1, mixing and stirring 30Kg of multifunctional epoxy resin, 30Kg of phenolic resin, 30Kg of active ester, 8Kg of cross-linking agent, 80Kg of modified silicon filler prepared in preparation example 10, 80Kg of heat-conducting filler prepared in preparation example 1 and 10Kg of solvent for 2 hours;
S2, coating the material mixed in the step S1 on a substrate to form an insulating adhesive layer, wherein the substrate is a PET release film with the thickness of 150 mu m;
s3, drying the insulating adhesive layer at 80 ℃ for 10min, and extruding the prepared insulating adhesive layer to form a film and rolling by using a calender to obtain the high-heat-conductivity insulating adhesive film with the thickness of 0.3 mm.
Example 2: a high thermal conductivity insulating film was different from example 1 in that step S1 was a mixture of 40Kg of a multifunctional epoxy resin, 20Kg of a phenol resin, 40Kg of an active ester, 16Kg of a crosslinking agent, 90Kg of a modified silica filler prepared in preparation example 11, 100Kg of a thermal conductive filler prepared in preparation example 2 and 20Kg of a solvent, and stirred for 2 hours, and the other steps were the same as in example 1.
Example 3: the difference between the insulating film with high heat conductivity and the insulating film of example 1 is that the heat conductive filler used was prepared in preparation example 3, and the other steps were the same as those of example 1.
Example 4: the difference between the insulating film with high heat conductivity and the insulating film of example 1 is that the heat conductive filler used was prepared in preparation example 4, and the other steps were the same as those of example 1.
Example 5: the difference between the insulating film with high heat conductivity and the insulating film of example 1 is that the heat conductive filler used was prepared in preparation example 5, and the other steps were the same as those of example 1.
Example 6: the difference between the insulating film with high heat conductivity and the insulating film of example 1 is that the heat conductive filler used was prepared in preparation example 7, and the other steps were the same as those of example 1.
Example 7: the difference between the insulating film with high heat conductivity and the insulating film of example 1 is that the heat conductive filler used was prepared in preparation example 6, and the other steps were the same as those of example 1.
Example 8: the high thermal conductivity insulating film was different from example 1 in that the modified silica filler used was prepared in preparation example 13, and the other steps were the same as in example 1.
Example 9: the high thermal conductivity insulating film was different from example 1 in that the modified silica filler used was prepared in preparation example 14, and the other steps were the same as in example 1.
Example 10: the high thermal conductivity insulating film was different from example 1 in that the modified silica filler used was prepared in preparation example 15, and the other steps were the same as in example 1.
Example 11: a high heat conduction insulating adhesive film is different from the embodiment 1 in that the multifunctional epoxy resin is resorcinol-based epoxy resin and naphthyl-based epoxy resin with the mass ratio of 1:1, and the naphthyl-based epoxy resin is 27610-48-6 of Wohamik biological medicine technology Co.
Example 12: the high heat conduction insulating adhesive film is different from the embodiment 1 in that the active ester is carboxylic acid active ester and phenol ester active ester with the mass ratio of 1:1, the phenol ester active ester is 2, 4-dihydroxyphenylacetic acid ethyl ester, and the rest steps are the same as the embodiment 1.
Comparative example
Comparative example 1: the high thermal conductive insulating film was different from example 1 in that the thermal conductive filler and the modified silicon filler were not added, and the other steps were the same as in example 1.
Comparative example 2: the difference between the high thermal conductive insulating film and the embodiment 1 is that no thermal conductive filler is added, and the rest steps are the same as those of the embodiment 1.
Comparative example 3: the high thermal conductivity insulating film was different from example 1 in that no modified silica filler was added, and the rest of the steps were the same as those of example 1.
Comparative example 4: the difference between the insulating film with high thermal conductivity and example 6 is that the heat conductive filler used was prepared in preparation example 8, and the other steps were the same as those in example 1.
Comparative example 5: the difference between the insulating film with high thermal conductivity and example 6 is that the heat conductive filler used was prepared in preparation example 9, and the other steps were the same as those in example 1.
Comparative example 6: the difference between the insulating film with high thermal conductivity and example 6 is that the heat conductive filler used was prepared in preparation example 10, and the other steps were the same as those in example 1.
Comparative example 7: the preparation method of the insulating heat-conducting adhesive film comprises the following steps:
S1, adding 10Kg of epoxy resin, 1Kg of bisphenol A resin, 5Kg of flexible resin and 3Kg of dimethylformamide into a container, uniformly mixing, stirring for 4 hours, adding 0.01Kg of dimethyl dipropyl sulfone, uniformly mixing, stirring for 4 hours, adding 2Kg of nitrile rubber, uniformly mixing, adding 30Kg of aluminum oxide and 20Kg of silicon dioxide, and uniformly mixing to obtain an insulating heat-conducting material;
s2, coating the insulating heat-conducting material on a release carrier, baking for 4 minutes at 120 ℃ after 2-4 minutes of treatment in a self-leveling section, and then heating to 170 ℃ and baking for 5 minutes again to obtain the insulating heat-conducting adhesive film finished product.
Performance test
Performance tests of thermal conductivity, peel strength, volume resistivity and bending resistance were performed on the insulating films prepared in examples 1 to 12 and comparative examples 1 to 7 and the test results were recorded in table 1, and the test methods were as follows:
The thermal conductivity is measured by referring to GB/T2588-2008 standard;
peel strength was tested against the requirements specified in GB/T2792-2014;
The volume resistivity is detected by referring to GB/T15662-1995, and the humidity of a test environment is 85%;
the bending resistance is tested with reference to the requirements specified in IEC-62899-202-5:2018 material conductive ink mechanical bending test of printed conductive layers on insulating substrates.
Table 1 table for performance test data of high thermal conductive insulating film
As can be seen from the detection data of examples 1-12 and comparative examples 1-7, the thermal conductivity of the insulating adhesive film in the application exceeds 7.66W/m.K, the thermal conductivity of the traditional insulating adhesive film is 4.56W/m.K, the thermal conductivity of the insulating adhesive film in the application is improved by 68% or more compared with that of the traditional insulating adhesive film, and the adhesive property and bending resistance of the insulating adhesive film in the application are improved compared with those of the traditional insulating adhesive film, so that the insulating adhesive film has excellent thermal conductivity and adhesive property, and is beneficial to obtaining more excellent performance in the field of electronic packaging.
From the test data of examples 1-6 and comparative examples 2-3, it can be seen that the addition of the heat conductive filler effectively improves the heat conductivity of the insulating film, the addition of the modified silicon filler effectively improves the adhesive property of the insulating film, and the addition of the modified silicon filler improves the resistivity of the insulating film, thereby compensating for the influence of the addition of the heat conductive filler on the insulating property of the insulating film. Impurities are contained in the unpurified carbon nanotubes, so that the self thermal resistance of the heat conducting filler is improved, and the heat conductivity of the insulating adhesive film is adversely affected; the thermal resistance of the carbon nano tube is obviously improved after fluorocarbon surface treatment, because the surface energy of the carbon nano tube is reduced due to the surface treatment, the dispersibility of the carbon nano tube in the heat conducting filler is enhanced, the carbon nano tube is prevented from agglomerating, the interface thermal resistance is effectively reduced, and the thermal conductivity of the insulating adhesive film is improved; grinding is favorable for better coating the carbon nano tubes on the surface of the asphalt-based carbon fiber during mixing, so that the contact area between the heat conducting fillers is effectively increased, and the heat conductivity of the insulating adhesive film is improved.
As can be seen from the test data of example 6 and comparative examples 4-6, the mixed use of aluminum nitride, carbon nanotubes and pitch-based carbon fibers better improved the thermal conductivity of the insulating film, because both carbon nanotubes and pitch-based carbon fibers have higher thermal conductivity and larger specific surface area, aluminum nitride has excellent thermal conductivity, carbon nanotubes can establish more bridges in the fiber network structure of pitch-based fibers to connect the dispersed thermally conductive filler particles together, and more thermally conductive paths are formed in the thermally conductive filler, and the single use effect is not as good as the mixed use effect.
From the examination data of example 1 and example 7, it can be seen that the use of thermosetting resin as the insulating polymer matrix is better in bending resistance than the use of plastic as the insulating polymer matrix, contributing to the maintenance of good mechanical properties of the insulating film.
From the test data of examples 8 to 10 and comparative example 3, it can be seen that the addition of the modified silica filler effectively improves the adhesive strength of the insulating film. The bending strength of the insulating adhesive film without adding the white carbon black is obviously reduced, the addition of the white carbon black is beneficial to improving the mechanical property and the bonding strength of the insulating adhesive film, and the insulating adhesive film obtained by peroxide vulcanization has better bonding strength and bending resistance.
As can be seen from the detection data of examples 11-12, the cross-linking density and strength of the insulating adhesive film are improved by mixing a plurality of multifunctional epoxy resins or a plurality of active esters, so that the insulating adhesive film has better bending resistance and effectively improves the mechanical property of the insulating adhesive film.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The high-heat-conductivity insulating adhesive film is characterized by comprising a base material and an insulating adhesive layer arranged on any side of the base material, wherein the insulating adhesive layer comprises the following raw materials in parts by weight: 30-40 parts of multifunctional epoxy resin, 20-40 parts of phenolic resin, 30-40 parts of active ester, 8-16 parts of silane cross-linking agent, 10-20 parts of solvent, 80-90 parts of modified silicon filler and 80-100 parts of heat conducting filler;
The heat conducting filler comprises aluminum nitride, carbon nano tubes, asphalt-based carbon fibers and an insulating high polymer matrix in a mass ratio of (1-2) to (20-30).
2. The high-heat-conductivity insulating adhesive film according to claim 1, wherein the preparation method of the heat-conductivity filler comprises the following steps:
mixing a carbon nano tube with a fluorocarbon surfactant for surface treatment to obtain a modified carbon nano tube, wherein the dosage of the fluorocarbon surfactant is 1-2% of the mass of the carbon nano tube;
mixing an insulating high polymer matrix with a matrix solvent to form matrix emulsion, wherein the dosage of the matrix solvent is 10-20% of the mass of the insulating high polymer matrix;
Mixing the modified carbon nano tube with asphalt-based carbon fiber and aluminum nitride, adding the mixture into the matrix emulsion, and drying, hot-pressing and crushing the mixture to obtain the heat-conducting filler.
3. The method for preparing the heat conductive filler of the high heat conductive insulating adhesive film according to claim 2, wherein the carbon nanotubes are subjected to the following pretreatment before being mixed with the fluorocarbon surfactant: heating the carbon nano tube to 600-800 ℃ in the atmosphere of inert gas, and treating for 1-2h at high temperature.
4. The method for preparing the heat conductive filler of the high heat conductive insulating adhesive film according to claim 2, wherein the following pretreatment is performed before the modified carbon nanotubes, the asphalt-based carbon fibers and the aluminum nitride are mixed and added into the matrix emulsion: mixing the modified carbon nano tube with asphalt-based carbon fiber and aluminum nitride, and grinding for 1-2h.
5. The high thermal conductivity insulating film according to claim 1, wherein: the modified silicon filler comprises (1-2) polymethyl vinyl siloxane and boric acid in a mass ratio of (10-15).
6. The high thermal conductivity insulating film according to claim 5, wherein the preparation method of the modified silicon filler comprises the following steps:
Mixing polymethyl vinyl siloxane and boric acid, and reacting at 170-200 ℃ for 1.5-2 hours to obtain viscous polyborosiloxane;
adding white carbon black and a peroxide vulcanizing agent into the viscous polyborosiloxane for vulcanization reaction and mixing, cooling and crushing to obtain modified silicon filler, wherein the vulcanization reaction conditions are as follows: the mass ratio of the polymethyl vinyl siloxane to the white carbon black to the peroxide vulcanizing agent is (10-15) 1:1 at 150-170 ℃ under the pressure of 8-10MPa for 10-20 min.
7. The high thermal conductivity insulating film according to claim 1, wherein: the multifunctional epoxy resin is selected from one or more of resorcinol-type epoxy resin, resorcinol-formaldehyde-type epoxy resin, naphthalene-based epoxy resin, biphenyl epoxy resin and phenolic epoxy resin.
8. The high thermal conductivity insulating film according to claim 1, wherein: the insulating high polymer matrix is vinyl resin.
9. The high thermal conductivity insulating film according to claim 1, wherein: the active ester is selected from one or more of anhydride active ester, carboxylic acid active ester and phenol ester active ester.
10. The method for preparing the high-heat-conductivity insulating adhesive film according to any one of claims 1 to 9, which is characterized by comprising the following steps:
Mixing and stirring multifunctional epoxy resin, phenolic resin, active ester, silane cross-linking agent, modified silicon filler, heat-conducting filler and solvent for 1-2h to prepare insulating slurry;
coating the insulating slurry on a substrate to form an insulating adhesive layer;
and drying, extruding to form a film and rolling the insulating adhesive layer to obtain the insulating adhesive film.
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