A modified epoxy resin with high tg, an insulating adhesive film with high shear strength and high thermal conductivity, and a preparation method thereof

Abstract

The application provides a modified epoxy resin with high Tg, a bonding insulating film with high shear strength and high thermal conductivity and a preparation method thereof, and aims at the problems that the existing thermal conductive bonding glue cannot meet the heat dissipation demand, is easy to produce bubbles and has low thermal conductivity, provides a solution for preparing the bonding insulating film by using a low-thermal-expansion diphenyl epoxy resin and a high-temperature-resistant naphthalene type epoxy resin to form a modified epoxy resin, and specifically comprises the following components in parts by weight: a naphthalene type epoxy resin 60-80 parts; a diphenyl epoxy resin 20-40 parts; a first solvent 80-120 parts; white carbon black 5-10 parts; a first defoaming agent 0.2-0.3 parts; a leveling agent 0.05-0.15 parts; a first curing agent 1-20 parts; and a first accelerator 0.5-1 part. The low-thermal-expansion diphenyl epoxy resin and the high-temperature-resistant naphthalene type epoxy resin are used, and the crosslinking degree of the epoxy resin is improved through the curing agent, so that the Tg temperature of the modified epoxy resin is greater than 300 DEG C.

Description

Technical Field

[0001] This invention relates to the field of thermally conductive adhesives, specifically to a modified epoxy resin with high Tg, an adhesive insulating film with high shear strength and high thermal conductivity, and a method for preparing the same. Background Technology

[0002] MOSFETs are common power transistors used in electronic and electrical products. These transistors generate a lot of heat and often need to be attached to heat sinks for timely heat dissipation. A common practice is to place a thermally conductive insulating sheet between the non-insulated MOSFET and the metal heat sink. This insulating sheet provides both electrical insulation and thermal conduction, and the MOSFET is then secured to the heat sink with screws. This manual screw-fixing method is inefficient and difficult to automate. The industry urgently needs an alternative method to improve assembly efficiency.

[0003] In recent years, thermosetting adhesive thermally conductive insulating films, which use silicone as the base adhesive and glass fiber or PI film as the substrate and are cured by hydrosilicone addition crosslinking, have been used on a small scale. After the MOSFET and the heat sink are initially bonded together with the thermosetting adhesive thermally conductive insulating film, they are then heated to a certain temperature, and the thermosetting adhesive insulating film will cure and bond the MOSFET and the heat sink together, thus replacing the screw fixing method.

[0004] Using this thermosetting adhesive insulating film to fix the MOSFET to the heat sink reduces assembly costs. This thermosetting adhesive insulating film contains vinyl silicone rubber and hydrogen-containing silicone oil, which undergoes addition cross-linking and curing under the action of a platinum catalyst. To prevent the thermally conductive insulating film from curing before it is attached to the MOSFET, an inhibitor is added to the formulation to inhibit the catalytic effect of the platinum catalyst. However, the storage time of the thermally conductive adhesive insulating film cannot be well controlled by the inhibitor. When the amount of inhibitor added is small, the storage time is short, and the thermally conductive adhesive insulating film has already cured before application. When the amount of inhibitor added is excessive, the platinum catalyst in the insulating film is slow to complete the catalytic cross-linking process effectively. Furthermore, the thermally conductive adhesive insulating film has a short storage time at room temperature. If it is refrigerated, it needs to be warmed up before use, which affects the efficiency of automated production.

[0005] However, existing thermally conductive adhesives on the market cannot meet heat dissipation requirements, are prone to generating bubbles, and have insufficient thermal conductivity. With the rapid development of electronic and electrical technologies, people's demand for electronic products is increasing, and the requirements for heat dissipation of electronic products are becoming more and more stringent. There is an urgent need for an adhesive insulating film with high thermal conductivity and high shear strength, and which is resistant to high temperatures and does not generate bubbles when cured at high temperatures. Summary of the Invention

[0006] In view of the aforementioned problems, this application is made to provide a high-Tg modified epoxy resin, an adhesive insulating film with high shear strength and high thermal conductivity, and a method for preparing the same, which overcomes or at least partially solves the aforementioned problems, comprising: A high-Tg modified epoxy resin, by weight, comprises: 60-80 parts of naphthalene-type epoxy resin; 20-40 parts of biphenyl epoxy resin; 80-120 parts of the first solvent; 5-10 parts of silica; First defoamer: 0.2-0.3 parts; Leveling agent 0.05–0.15 parts; 1-20 parts of the first curing agent; The first accelerator is 0.5 to 1 part.

[0007] Preferably, the naphthalene-type epoxy resin includes at least one of 1,5-naphthol diglycidyl ether, 2,7-naphthol diglycidyl ether, binaphthol diglycidyl ether, naphthol phenolic epoxy, and naphthol-biphenyl aryl epoxy. The biphenyl epoxy resin includes at least one of 4,4'-biphenyl diglycidyl ether, 3,3',5,5'-tetramethylbiphenyl diglycidyl ether, and biphenyl aralkyl groups.

[0008] Preferably, the first solvent includes at least one of acetone, propylene glycol methyl ether acetate, butanone, and dimethylformamide.

[0009] Preferably, the silica includes at least one of fumed silica and precipitated silica.

[0010] Preferably, the first curing agent includes at least one of dicyandiamide and its derivatives, phenolic resin, diaminodiphenyl sulfone, diaminodiphenylamine, organic acid hydrazide, BF3 amine complex, and modified imidazole compounds.

[0011] Preferably, the first accelerator comprises at least one of 2-ethyl-4-methylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2,4,6-tris(dimethylaminomethylamine)phenol, phenyl dimethylamine, organic urea and its derivatives, benzoyl peroxide, triphenylphosphine, triphenyl phosphite, and acetylacetone metal complexes.

[0012] A method for preparing a high-Tg modified epoxy resin, comprising the following steps: Weigh out the following components according to the first specified ratio: naphthalene-type epoxy resin, biphenyl epoxy resin, solvent, silica, defoamer, leveling agent, curing agent, and accelerator. The naphthalene-type epoxy resin, the biphenyl epoxy resin, the solvent, the carbon black, the defoamer, the leveling agent, and the curing agent are mixed and stirred. Finally, the accelerator is added, and the mixture is subjected to segmented temperature-controlled stirring to obtain the target modified epoxy resin.

[0013] An adhesive insulating film with high shear strength and high thermal conductivity, comprising, by weight: 90-110 parts of modified epoxy resin; Toughening agent 1-5 parts; The second solvent is 1000-2000 parts; 1-20 parts of the second curing agent; Second accelerator: 0.1-1 part; 1800-2200 parts of thermally conductive powder; 50-70 parts of thickener; The second defoamer is 0.2 to 0.3 parts.

[0014] Preferably, the thermally conductive powder is at least one of aluminum oxide, zinc oxide, boron nitride, aluminum nitride, silicon nitride, diamond, graphene, and carbon fiber.

[0015] A method for preparing an adhesive insulating film with high shear strength and high thermal conductivity includes the following steps: Weigh the modified epoxy resin, toughening agent, solvent, curing agent, accelerator, thermally conductive powder, tackifier and defoamer according to the second specified ratio; The modified epoxy resin, the toughening agent, the solvent, the thermally conductive powder, the tackifier, the defoamer, the curing agent, and the accelerator are mixed and stirred to make the viscosity of the adhesive 10,000 to 15,000 cps; The adhesive is directly coated on both sides of the PI film surface, and then laminated with PET release film on both sides to obtain the target adhesive insulating film.

[0016] This application has the following advantages: In the embodiments of this application, addressing the technical problems of existing thermally conductive adhesives failing to meet heat dissipation requirements, easily generating bubbles, and having insufficient thermal conductivity, this application provides a solution for preparing an adhesive insulating film using a modified epoxy resin composed of low-thermal-expansion biphenyl epoxy resin and high-temperature-resistant naphthalene-type epoxy resin. Specifically, by weight, it comprises: 60-80 parts of naphthalene-type epoxy resin; 20-40 parts of biphenyl epoxy resin; 80-120 parts of a first solvent; 5-10 parts of silica; 0.2-0.3 parts of a first defoamer; 0.05-0.15 parts of a leveling agent; 1-20 parts of a first curing agent; and 0.5-1 parts of a first accelerator. By adding low-thermal-expansion biphenyl epoxy resin and high-temperature-resistant naphthalene-type epoxy resin, and by adding a curing agent to increase the crosslinking degree of the epoxy resin, the Tg temperature of the modified epoxy resin is greater than 300°C. Attached Figure Description

[0017] To more clearly illustrate the technical solution of this application, the drawings used in the description of this application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic flowchart of a method for preparing a high-Tg modified epoxy resin according to an embodiment of this application; Figure 2 This is a process flow diagram of a method for preparing an adhesive insulating film with high shear strength and high thermal conductivity, according to an embodiment of this application. Detailed Implementation

[0019] To make the objectives, features, and advantages of this application more apparent and understandable, the application will be further described in detail below with reference to the accompanying drawings and specific embodiments. Obviously, the described embodiments are only some, not all, of the embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0020] The inventors, through analysis of existing technologies, discovered that the thermal conductivity of current thermally conductive silicone adhesive insulating films is only 1.5W, which is insufficient to meet the heat dissipation requirements of heat sinks. Furthermore, heating and curing at temperatures above 170℃ easily leads to bubble formation, affecting heat dissipation. Some thermally conductive adhesive films have a maximum thermal conductivity of only around 3W. With the rapid development of electronic and electrical technologies, people's demands for electronic products are increasing, and the requirements for heat dissipation are becoming more stringent. There is an urgent need for an adhesive insulating film with high thermal conductivity and high shear strength, as well as high-temperature resistance and bubble-free high-temperature curing.

[0021] One embodiment of this application provides a high-Tg modified epoxy resin, comprising, by weight parts: 60-80 parts of naphthalene-type epoxy resin; 20-40 parts of biphenyl epoxy resin; 80-120 parts of the first solvent; 5-10 parts of silica; First defoamer: 0.2-0.3 parts; Leveling agent 0.05–0.15 parts; 1-20 parts of the first curing agent; The first accelerator is 0.5 to 1 part.

[0022] In the embodiments of this application, addressing the technical problems of existing thermally conductive adhesives failing to meet heat dissipation requirements, easily generating bubbles, and having insufficient thermal conductivity, this application provides a solution for preparing an adhesive insulating film using a modified epoxy resin composed of low-thermal-expansion biphenyl epoxy resin and high-temperature-resistant naphthalene-type epoxy resin. Specifically, by weight, it comprises: 60-80 parts of naphthalene-type epoxy resin; 20-40 parts of biphenyl epoxy resin; 80-120 parts of a first solvent; 5-10 parts of silica; 0.2-0.3 parts of a first defoamer; 0.05-0.15 parts of a leveling agent; 1-20 parts of a first curing agent; and 0.5-1 parts of a first accelerator. By adding low-thermal-expansion biphenyl epoxy resin and high-temperature-resistant naphthalene-type epoxy resin, and by adding a curing agent to increase the crosslinking degree of the epoxy resin, the Tg temperature of the modified epoxy resin is greater than 300°C.

[0023] The following will further describe a high-Tg modified epoxy resin in this exemplary embodiment.

[0024] In one embodiment of this application, the naphthalene-type epoxy resin includes at least one of 1,5-naphthol diglycidyl ether, 2,7-naphthol diglycidyl ether, binaphthol diglycidyl ether, naphthol phenolic epoxy, and naphthol-biphenyl aryl epoxy. The biphenyl epoxy resin includes at least one of 4,4'-biphenyl diglycidyl ether, 3,3',5,5'-tetramethylbiphenyl diglycidyl ether, and biphenyl aralkyl groups.

[0025] It should be noted that the naphthalene-type epoxy resin contains a naphthalene skeleton with a fused ring structure, which can improve the crosslinking density and segment rigidity of the cured resin through its rigid large π-conjugated system, thereby effectively increasing the glass transition temperature and heat resistance of the resin system while reducing water absorption. The biphenyl epoxy resin contains a freely rotatable biphenyl structure, which provides moderate rigidity while imparting good orientation and liquid crystal order to the molecular chains, promoting the formation of anisotropic network structures during curing, thereby significantly reducing the coefficient of thermal expansion of the resin system and improving its melt flowability.

[0026] Naphthalene-based epoxy resins focus on maximizing the system's heat resistance and hydrophobicity, establishing a solid foundation for high Tg and low moisture absorption; biphenyl epoxy resins focus on optimizing the system's toughness, internal stress, and dielectric properties, improving processability. When combined, these two materials significantly improve the heat resistance, dimensional stability, resistance to humid heat aging, mechanical properties, and dielectric properties of the modified epoxy resin cured product while maintaining a high glass transition temperature and without sacrificing processability.

[0027] In one specific implementation, 4,4'-biphenyl diglycidyl ether and naphthol-biphenyl aryl epoxide are selected in a mass ratio of 3:7.

[0028] In one embodiment of this application, the first solvent includes at least one selected from acetone, propylene glycol methyl ether acetate, methyl ethyl ketone (MEK), and dimethylformamide. The solvent is used to dissolve and dilute the naphthalene-type epoxy resin, the biphenyl epoxy resin, and other components to adjust the solid content and viscosity of the composition to meet the operational requirements of coating, impregnation, or spraying processes, while simultaneously promoting uniform mixing of the components at the molecular level. The preferred solvent in this application is MEK.

[0029] In one embodiment of this application, the silica includes at least one of fumed silica and precipitated silica. As a thixotropic agent and nano-reinforcing filler, silica has a surface rich in silanol groups, which can form a reversible physical cross-linking network in the resin matrix through hydrogen bonding. This imparts excellent anti-sagging properties to the composition, reduces volume shrinkage during curing, and improves the mechanical strength and heat and oxygen aging resistance of the cured product. Preferably, this application uses fumed silica with a particle size of 14 nm and a specific surface area of ​​150 m². 2 / g.

[0030] In one embodiment of this application, the first curing agent includes at least one selected from dicyandiamide and its derivatives, phenolic resin, diaminodiphenyl sulfone, diaminodiphenylamine, organic acid hydrazide, BF3 amine complex, and modified imidazole compounds. The curing agent is used to undergo a ring-opening crosslinking reaction with the epoxy groups in the naphthalene-type epoxy resin and biphenyl epoxy resin to construct a three-dimensional network structure with high crosslinking density. Preferably, the curing agent is a mixture of m-phenylenediamine and diaminodiphenyl sulfone in a 1:5 ratio.

[0031] In one embodiment of this application, the first accelerator includes at least one selected from 2-ethyl-4-methylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2,4,6-tris(dimethylaminomethylamine)phenol, phenyl dimethylamine, organic urea and its derivatives, benzoyl peroxide, triphenylphosphine, triphenyl phosphite, and acetylacetone metal complexes. The accelerator catalyzes the curing reaction between the first curing agent and the epoxy resin, lowers the activation energy of the reaction, thereby effectively shortening the curing time or lowering the curing temperature, while promoting a more complete and uniform crosslinking reaction, avoiding uneven local crosslinking density. The accelerator is preferably phenyl dimethylamine.

[0032] In one embodiment of this application, the first defoamer includes at least one of polyether-based defoamers, natural oils, higher alcohols, silicone defoamers, polyether-modified silicone, and polysiloxane defoamers. The defoamer can eliminate air bubbles entrained or generated during resin blending, stirring, and dispersion, preventing air bubbles from remaining after curing and forming surface defects such as pinholes, pits, or craters, thereby ensuring the density and dielectric reliability of the cured product. In this embodiment, the defoamer is preferably a polyether-modified silicone defoamer.

[0033] In one embodiment of this application, the leveling agent includes at least one of polymethylphenylsiloxane, polydimethylsiloxane, polyether polyester modified organosiloxane, alkyl modified organosiloxane, end-group modified organosilicon, reactive leveling agent, acrylic leveling agent, and fluorinated leveling agent. The defoamer reduces the surface tension of the resin composition, enhances its wetting ability to the substrate or reinforcing material, and promotes uniform spreading of the resin before curing, thereby obtaining a smooth, continuous, and well-gloss cured surface. In this embodiment, an alkyl modified organosiloxane is preferred.

[0034] Reference Figure 1 This paper illustrates a method for preparing a high-Tg modified epoxy resin, comprising the following steps: S110. Weigh out naphthalene-type epoxy resin, biphenyl epoxy resin, solvent, fumed silica, defoamer, leveling agent, curing agent and accelerator according to the first specified ratio; S120. Mix and stir the naphthalene-type epoxy resin, the biphenyl epoxy resin, the solvent, the carbon black, the defoamer, the leveling agent, and the curing agent; S130. Finally, the accelerator is added, and the mixture is subjected to segmented temperature-controlled stirring to obtain the target modified epoxy resin.

[0035] In one embodiment of the present invention, the specific process of "weighing naphthalene-type epoxy resin, biphenyl epoxy resin, solvent, fumed silica, defoamer, leveling agent, curing agent and accelerator according to the first specified ratio" in step S110 can be further described in conjunction with the following description.

[0036] As an example, weigh out 70 kg of naphthalene-type epoxy resin, 30 kg of biphenyl epoxy resin, 100 kg of the first solvent, 7 kg of silica, 0.25 kg of the first defoamer, 0.1 kg of leveling agent, 15 kg of the first curing agent, and 0.6 kg of the first accelerator.

[0037] In one embodiment of the present invention, the specific process of "mixing and stirring the naphthalene-type epoxy resin, the biphenyl epoxy resin, the solvent, the carbon black, the defoamer, the leveling agent and the curing agent" in step S120 can be further described in conjunction with the following description.

[0038] As an example, 70 kg of naphthalene-type epoxy resin, 30 kg of biphenyl epoxy resin and 100 kg of solvent are first dissolved in a planetary mixer at a speed of 30 r / min for 20 to 30 min, and then the speed is increased to 50 r / min for 120 to 150 min.

[0039] Then add 7 kg of silica, stir at 30 r / min for 10-20 min, then increase the speed to 50 r / min and stir for 20-30 min.

[0040] Add 0.25 kg of defoamer and 0.1 kg of leveling agent and mix with a planetary mixer at 30 r / min for 30-40 min.

[0041] Add another 15 kg of curing agent, rotate at 30 r / min, stir for 10-20 min, and keep the temperature at 20-30℃ by circulating cooling water to avoid premature reaction due to excessive temperature.

[0042] In one embodiment of the present invention, the specific process of step S130, "finally adding the accelerator, performing segmented temperature-controlled stirring treatment on the mixture to obtain the target modified epoxy resin," can be further described in conjunction with the following description.

[0043] As an example, 0.6 kg of accelerator was added at the end, and the stirring speed was 30 r / min for 10–20 min. After stirring evenly, the temperature was raised to 120–150 °C, and the stirring speed was 30 r / min for 120–150 min to initiate crosslinking and allow the solvent and water to evaporate completely. The temperature was then raised to 180–220 °C, and the stirring speed was 30 r / min for 240–260 min to initiate deep crosslinking and form network crosslinks. Finally, the temperature was raised to 240–250 °C, and the stirring speed was 30 r / min for 60–80 min to initiate post-curing crosslinking and increase the Tg temperature of the modified epoxy resin. The modified epoxy resin was then cooled to room temperature for later use.

[0044] One embodiment of this application provides an adhesive insulating film with high shear strength and high thermal conductivity, comprising, by weight: 90-110 parts of modified epoxy resin; Toughening agent 1-5 parts; The second solvent is 1000-2000 parts; 1-20 parts of the second curing agent; Second accelerator: 0.1-1 part; 1800-2200 parts of thermally conductive powder; 50-70 parts of thickener; The second defoamer is 0.2 to 0.3 parts.

[0045] In the embodiments of this application, by modifying epoxy resin, adding toughening agents to improve flexibility and avoid embrittlement after long-term aging, and adding tackifiers to improve bonding strength, a thermosetting adhesive insulating film based on epoxy resin with high thermal conductivity, high shear strength and excellent pressure resistance is provided.

[0046] The following will further describe an adhesive insulating film with high shear strength and high thermal conductivity in this exemplary embodiment.

[0047] In one embodiment of this application, the toughening agent includes at least one of vinyl acetate emulsion, phenolic resin, nitrile rubber, acrylate rubber, polyvinyl butyral, polyvinyl acetate, and polyurethane. The toughening agent prevents the adhesive insulating film from developing microcracks or interfacial peeling due to excessive embrittlement during long-term thermo-oxidative aging or thermal shock, thereby improving impact resistance and peel strength while maintaining a high glass transition temperature. In this embodiment, the toughening agent is preferably phenolic resin.

[0048] In one embodiment of this application, the second solvent includes at least one of acetone, propylene glycol methyl ether acetate, butanone, and dimethylformamide, preferably butanone.

[0049] In one embodiment of this application, the thermally conductive powder is aluminum oxide, zinc oxide, boron nitride, aluminum nitride, silicon nitride, diamond, graphene, and carbon fiber, etc. The thermally conductive powder is uniformly dispersed in a modified epoxy resin matrix to form a thermally conductive network or pathway, rapidly conducting heat generated by electronic components or heat-generating interfaces to the heat dissipation structure, providing the adhesive insulating film with a high thermal conductivity, while avoiding a decrease in electrical insulation performance due to excessive filling. In this embodiment, the aluminum nitride is preferably of at least one particle size D50 of 0.5µm, 2µm, 5µm, 10µm, and 20µm (already hydrolysis-resistant, 0.5µm:2µm:5µm:10µm:20µm = 2:6:3:7:4).

[0050] In one embodiment of this application, the second curing agent includes at least one of dicyandiamide and its derivatives, phenolic resin, diaminodiphenyl sulfone, diaminodiphenylamine, organic acid hydrazide, BF3 amine complex, and modified imidazole compounds, preferably a mixture of m-phenylenediamine and diaminodiphenyl sulfone (1:5).

[0051] In one embodiment of this application, the second promoter is selected from at least one of 2-ethyl-4-methylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2,4,6-tris(dimethylaminomethylamine)phenol, phenyl dimethylamine, organic urea and its derivatives, benzoyl peroxide, triphenylphosphine, triphenyl phosphite, and acetylacetone metal complexes, preferably phenyl dimethylamine.

[0052] In one embodiment of this application, the tackifier is one or more of vinyl-based or hydrogen-containing compounds, which enhances the interfacial adhesion between the thermosetting adhesive insulating film and the polyimide film, and is preferably a vinyl-based tackifier.

[0053] In one embodiment of this application, the second defoamer is selected from at least one of polyether defoamers, natural oils, higher alcohols, silicone defoamers, polyether-modified silicone, and polysiloxane defoamers, preferably a polyether-modified silicone defoamer.

[0054] Reference Figure 2 This paper illustrates a method for preparing an adhesive insulating film with high shear strength and high thermal conductivity, comprising the following steps: S210. Weigh the modified epoxy resin, toughening agent, solvent, curing agent, accelerator, thermally conductive powder, tackifier and defoamer according to the second specified ratio; S220. The modified epoxy resin, the toughening agent, the solvent, the thermally conductive powder, the tackifier, the defoamer, the curing agent and the accelerator are mixed and stirred to make the viscosity of the adhesive 10000-15000cps. S230. Apply the adhesive material directly to the surface of the PI film on both sides, and then laminate it with a PET release film on both sides to obtain the target adhesive insulating film.

[0055] In one embodiment of the present invention, the specific process of "weighing modified epoxy resin, toughening agent, solvent, curing agent, accelerator, thermally conductive powder, tackifier and defoamer according to the second specified ratio" in step S210 can be further described in conjunction with the following description.

[0056] As an example, weigh out 100 kg of modified epoxy resin, 2 kg of toughening agent, 100 kg of second solvent, 2000 kg of thermally conductive powder, 1000 kg of second solvent, 0.25 kg of second defoamer, 60 kg of tackifier, 15 kg of second curing agent and 0.6 kg of second accelerator.

[0057] In one embodiment of the present invention, the specific process of step S220, which involves "mixing and stirring the modified epoxy resin, the toughening agent, the solvent, the thermally conductive powder, the tackifier, the defoamer, the curing agent, and the accelerator to make the viscosity of the adhesive material 10,000 to 15,000 cps", can be further described in conjunction with the following description.

[0058] As an example, 100 kg of modified epoxy resin, 2 kg of toughening agent and 100 kg of solvent are first dissolved in a planetary mixer at a speed of 30 r / min for 20 to 30 min, and then the speed is increased to 50 r / min for 120 to 150 min.

[0059] Add 2000 kg of thermally conductive powder and 1000 kg of solvent, stir at 30 r / min for 10-20 min, then increase the speed to 50 r / min and stir for 20-30 min.

[0060] Add 0.25 kg of defoamer, 60 kg of tackifier and 15 kg of curing agent to a planetary mixer and mix at 30 r / min for 30 to 40 minutes. Keep the temperature at 20 to 30°C by circulating cooling water to prevent premature reaction due to excessive temperature.

[0061] Add 0.6 kg of accelerator, rotate at 30 r / min, stir for 10-20 min, keep the temperature at 20-30℃ with cooling water to avoid premature reaction due to excessive temperature. After stirring evenly, test the viscosity of the rubber compound to be 10000-15000 cps. Filter the stirred rubber compound and set aside for use.

[0062] In one embodiment of the present invention, the specific process of step S230, "applying the adhesive to the surface of the PI film on both sides and then laminating a PET release film on both sides to obtain the target adhesive insulating film," can be further described in conjunction with the following description.

[0063] As an example, the adhesive is finally poured into the trough and directly coated on both sides of the PI film (corona value ≥3KV), with a line speed of 1.5~2min / m, a time of 10~20min, a temperature of 80~120℃, and a double-sided PET release film is laminated to form a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02mm.

[0064] The PI film has a thickness of 25–100 μm, and a 25 μm PI film is selected.

[0065] The PET film is 25-100µm, and 50µm and 25µm PET release films are used in combination.

[0066] The mesh size of the filter screen is 100 to 500 mesh, and a 200 mesh filter screen is selected.

[0067] The following are specific embodiments. Example 1 First, dissolve 70 kg of naphthol-biphenyl aryl epoxy, 30 kg of 4,4'-biphenyl diglycidyl ether, and 100 kg of butanone in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 7 kg of fumed silica and stir at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Then add 0.25 kg of polyether-modified silicone defoamer and 0.1 kg of alkyl-modified silicone siloxane and stir at 30 rpm for 35 min. Finally, add 2.5 kg of m-phenylenediamine and 12.5 kg of diaminodiphenyl sulfone and stir at 30 rpm for 15 min. Maintain the temperature at 20–30 °C by circulating cooling water to avoid… Excessive temperature can lead to premature reaction. Finally, add 0.6 kg of phenyl dimethylamine, stir at 30 rpm for 15 min, and after uniform stirring, raise the temperature to 120℃, stir at 30 rpm for 130 min for initial crosslinking, allowing the solvent and moisture to evaporate completely. Raise the temperature to 200℃, stir at 30 rpm for 250 min for deep crosslinking, forming network crosslinks. Finally, raise the temperature to 245℃, stir at 30 rpm for 70 min for post-curing crosslinking, increasing the Tg temperature of the modified epoxy resin. Cool the modified epoxy resin to room temperature before use.

[0068] First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0069] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0070] Example 2: Modified resin is the same as in Example 1 First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 1800 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0071] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0072] Example 3 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2200 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0073] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0074] Example 4 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 1.5 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0075] The thermally conductive adhesive insulating films were characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1. Example 5 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 2.5 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0076] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0077] Example 6 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.33 kg of m-phenylenediamine, and 11.67 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. To prevent premature reaction due to excessive heat, add 0.6 kg of phenyl dimethylamine, stir at 30 r / min for 15 min, and maintain a temperature of 20-30℃ with cooling water to avoid premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and directly coat it on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0078] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0079] Example 7 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.67 kg of m-phenylenediamine, and 13.33 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. To prevent premature reaction due to excessive heat, add 0.6 kg of phenyl dimethylamine, stir at 30 r / min for 15 min, and maintain a temperature of 20-30℃ with cooling water to avoid premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and directly coat it on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0080] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0081] Example 8 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.5 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2 ± 0.02 mm. Store in a freezer at 0-8℃.

[0082] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0083] Example 9 Modified Resin Example 1 First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat leads to premature reaction; add 0.7 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction due to excessive heat. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV), with a linear speed of 1.6 min / m and a time of 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0084] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0085] Comparative Example 1: Other Resin Modifications First, dissolve 70 kg of linear phenolic polyglycidyl ether, 30 kg of 4,4'-biphenyl diglycidyl ether, and 100 kg of butanone in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 7 kg of fumed silica and stir at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Then add 0.25 kg of polyether-modified silicone defoamer and 0.1 kg of alkyl-modified silicone siloxane and stir at 30 rpm for 35 min. Finally, add 2.5 kg of m-phenylenediamine and 12.5 kg of diaminodiphenyl sulfone and stir at 30 rpm for 15 min. Maintain the temperature at 20–30°C by circulating cooling water to avoid… Excessive temperature can lead to premature reaction. Finally, add 0.6 kg of phenyl dimethylamine, stir at 30 rpm for 15 min, and after uniform stirring, raise the temperature to 120℃, stir at 30 rpm for 130 min for initial crosslinking, allowing the solvent and moisture to evaporate completely. Raise the temperature to 200℃, stir at 30 rpm for 250 min for deep crosslinking, forming network crosslinks. Finally, raise the temperature to 245℃, stir at 30 rpm for 70 min for post-curing crosslinking, increasing the Tg temperature of the modified epoxy resin. Cool the modified epoxy resin to room temperature before use.

[0086] First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0087] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0088] Comparative Example 2: Epoxy resins in other proportions First, dissolve 65 kg of naphthol-biphenyl aryl epoxy, 35 kg of 4,4'-biphenyl diglycidyl ether, and 100 kg of butanone in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 7 kg of fumed silica and stir at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Then add 0.25 kg of polyether-modified silicone defoamer and 0.1 kg of alkyl-modified silicone siloxane and stir at 30 rpm for 35 min. Finally, add 2.5 kg of m-phenylenediamine and 12.5 kg of diaminodiphenyl sulfone and stir at 30 rpm for 15 min. Maintain the temperature at 20–30°C by circulating cooling water to avoid… Excessive temperature can lead to premature reaction. Finally, add 0.6 kg of phenyl dimethylamine, stir at 30 rpm for 15 min, and after uniform stirring, raise the temperature to 120℃, stir at 30 rpm for 130 min for initial crosslinking, allowing the solvent and moisture to evaporate completely. Raise the temperature to 200℃, stir at 30 rpm for 250 min for deep crosslinking, forming network crosslinks. Finally, raise the temperature to 245℃, stir at 30 rpm for 70 min for post-curing crosslinking, increasing the Tg temperature of the modified epoxy resin. Cool the modified epoxy resin to room temperature before use.

[0089] First, dissolve 100 kg of modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0090] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0091] Comparative Example 3: Conventional Epoxy Resin First, dissolve 100 kg of acrylate-modified epoxy resin, 2 kg of phenolic resin, and 100 kg of methyl ethyl ketone (MEK) in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of MEK, stirring at 30 rpm for 15 min, then increase the speed to 50 rpm for 25 min. Finally, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2.5 kg of m-phenylenediamine, and 12.5 kg of diaminodiphenyl sulfone (DPS) in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent overheating. Excessive heat can cause premature reaction. Add 0.6 kg of phenyl dimethylamine, rotate at 30 r / min, stir for 15 min, and maintain the temperature at 20-30℃ with cooling water to prevent premature reaction. After stirring evenly, test the viscosity of the adhesive to be 10000-15000 cps. Filter the stirred adhesive through a 200-mesh filter and set aside. Finally, pour the adhesive into a material tank and coat it directly on both sides onto a 25 μm PI film (corona value 4KV). The linear speed is 1.6 min / m, and the time is 15 min. The oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃. Double-sided lamination with 25 μm and 50 μm PET release films produces a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02 mm. Store in a freezer at 0-8℃.

[0092] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0093] Comparative Example 4: Organosilicon Resin First, dissolve 102 kg of silicone resin and 100 kg of xylene in a planetary mixer at 30 rpm for 25 min, then increase the speed to 50 rpm for 130 min. Next, add 2000 kg of aluminum nitride (0.5 μm:2 μm:5 μm:10 μm:20 μm = 2:6:3:7:4) and 1000 kg of xylene, stirring at 30 rpm for 15 min, then at 50 rpm for 25 min. Then, add 0.25 kg of polyether-modified silicone defoamer, 60 kg of vinyl tackifier, 2 kg of inhibitor (acetylenecyclohexanol), and 15 kg of hydrogen-containing silicone oil (0.36 g of hydrogen-containing silicone oil), stirring in the planetary mixer at 30 rpm for 35 min, maintaining a temperature of 20–30 °C with cooling water to prevent premature reaction due to excessive temperature. Finally, add 0.6 kg of catalyst (2000 ppm), stirring at 30 rpm. Mixing time is 15 minutes, cooling water is circulated to maintain temperature at 20-30℃ to avoid premature reaction due to excessive temperature. After mixing evenly, the viscosity of the adhesive is tested to be 10000-15000cps. The mixed adhesive is filtered through a 200-mesh filter and set aside for later use. Finally, the adhesive is poured into a material tank and directly coated on both sides onto a 25µm PI film (corona value 4KV). The linear speed is 1.6min / m, the time is 15 minutes, and the oven temperatures are 80℃, 90℃, 100℃, 110℃, 120℃, 110℃, 100℃, 90℃, and 80℃ respectively. Double-sided lamination with 25µm and 50µm PET release films is performed to form a thermally conductive adhesive insulating film with a total thickness of 0.2±0.02mm. It is then stored in a freezer at a temperature of 0-8℃.

[0094] The thermally conductive adhesive insulating film was characterized by thermal resistance, breakdown voltage, thermal conductivity, shear strength, and torsional value. The results are shown in Table 1.

[0095] Performance tests of high shear strength thermally conductive adhesive insulating film: Thermal conductivity was tested according to ISO 22007-2; Tg was tested according to GB / T19466.2-2004; The breakdown voltage was tested according to ASTM D149; Shear strength was tested according to ASTM D1002 at 200℃ for 30 minutes. Torque values ​​are tested internally, with a pressure of 50-80 psi for 30 seconds and a temperature of 200℃ for 30 minutes.

[0096] Table 1 Note: Comparative Example 3: Shear strength temperature 120℃ x 30 min, torque value pressure 50-80 psi, holding pressure for 30 s, temperature 120℃ x 30 min.

[0097] As can be seen from Table 1, the thermally conductive adhesive insulating film of the present invention not only has excellent shear strength, high thermal conductivity, good heat resistance, and torque value that meets the client's requirements, but also cures at high temperature without bubbles.

[0098] Although preferred embodiments of the present application have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of the embodiments of the present application.

[0099] Finally, it should be noted that in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or terminal device that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or terminal device. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or terminal device that includes said element.

[0100] The above provides a detailed description of a high-Tg modified epoxy resin, an adhesive insulating film with high shear strength and high thermal conductivity, and its preparation method. Specific examples have been used to illustrate the principles and implementation methods of this application. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of this application. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the ideas of this application. Therefore, the content of this specification should not be construed as a limitation of this application.

Claims

1. A high-Tg modified epoxy resin, characterized in that, By weight, including: 60-80 parts of naphthalene-type epoxy resin; 20-40 parts of biphenyl epoxy resin; 80-120 parts of the first solvent; 5-10 parts of silica; First defoamer: 0.2-0.3 parts; Leveling agent 0.05–0.15 parts; 1-20 parts of the first curing agent; The first accelerator is 0.5 to 1 part.

2. The high Tg modified epoxy resin according to claim 1, characterized in that, The naphthalene-type epoxy resin includes at least one of 1,5-naphthol diglycidyl ether, 2,7-naphthol diglycidyl ether, binaphthol diglycidyl ether, naphthol phenolic epoxy, and naphthol-biphenyl aryl epoxy. The biphenyl epoxy resin includes at least one of 4,4'-biphenyl diglycidyl ether, 3,3',5,5'-tetramethylbiphenyl diglycidyl ether, and biphenyl aralkyl groups.

3. The high Tg modified epoxy resin according to claim 1, characterized in that, The first solvent includes at least one of acetone, propylene glycol methyl ether acetate, butanone, and dimethylformamide.

4. The high Tg modified epoxy resin according to claim 1, characterized in that, The silica includes at least one of fumed silica and precipitated silica.

5. The high Tg modified epoxy resin according to claim 1, characterized in that, The first curing agent includes at least one of dicyandiamide and its derivatives, phenolic resin, diaminodiphenyl sulfone, diaminodiphenylamine, organic acid hydrazide, BF3 amine complex, and modified imidazole compounds.

6. The high Tg modified epoxy resin according to claim 1, characterized in that, The first accelerator includes at least one of 2-ethyl-4-methylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethylimidazole, 2,4,6-tris(dimethylaminomethylamine)phenol, phenyl dimethylamine, organic urea and its derivatives, benzoyl peroxide, triphenylphosphine, triphenyl phosphite and acetylacetone metal complexes.

7. A method for preparing a high-Tg modified epoxy resin, characterized in that, Including the following steps: Weigh out the following components according to the first specified ratio: naphthalene-type epoxy resin, biphenyl epoxy resin, solvent, silica, defoamer, leveling agent, curing agent, and accelerator. The naphthalene-type epoxy resin, the biphenyl epoxy resin, the solvent, the carbon black, the defoamer, the leveling agent, and the curing agent are mixed and stirred. Finally, the accelerator is added, and the mixture is subjected to segmented temperature-controlled stirring to obtain the target modified epoxy resin.

8. An adhesive insulating film with high shear strength and high thermal conductivity, characterized in that, By weight, including: 90-110 parts of modified epoxy resin; Toughening agent 1-5 parts; The second solvent is 1000-2000 parts; 1-20 parts of the second curing agent; Second accelerator: 0.1-1 part; 1800-2200 parts of thermally conductive powder; 50-70 parts of thickener; The second defoamer is 0.2 to 0.3 parts.

9. The adhesive insulating film with high shear strength and high thermal conductivity according to claim 8, characterized in that, The thermally conductive powder is at least one of aluminum oxide, zinc oxide, boron nitride, aluminum nitride, silicon nitride, diamond, graphene, and carbon fiber.

10. A method for preparing an adhesive insulating film with high shear strength and high thermal conductivity, characterized in that, Including the following steps: Weigh the modified epoxy resin, toughening agent, solvent, curing agent, accelerator, thermally conductive powder, tackifier and defoamer according to the second specified ratio; The modified epoxy resin, the toughening agent, the solvent, the thermally conductive powder, the tackifier, the defoamer, the curing agent, and the accelerator are mixed and stirred to make the viscosity of the adhesive 10,000 to 15,000 cps; The adhesive is directly coated on both sides of the PI film surface, and then laminated with PET release film on both sides to obtain the target adhesive insulating film.

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