High-performance epoxy resin adhesive and preparation method thereof
By using surface-modified thermal conductivity and toughening elastomers in epoxy resin adhesives, the problems of insufficient thermal conductivity and brittleness of epoxy resin adhesives in the electronic packaging field are solved, and high-performance mechanical and thermal conductivity improvement is achieved, and widening it Application scope.
Patent Information
- Application Number
- CN202411362014.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2024-12-27
AI Technical Summary
Epoxy resin adhesives have problems such as insufficient thermal conductivity, high toxicity of flammable and combustion flue gases, as well as low brittleness and mechanical properties in the field of electronic packaging, which limits their application prospects.
Using surface-modified thermally conductive particles, such as composite particles of aluminum nitride, silicon nitride and carbon nitride, combined with toughened elastomer and reasonable particle size ratio, high-performance rings are prepared by ultrasonic dispersion and polymerization reaction. Oxygen resin adhesive enhances its thermal conductivity and mechanical properties.
It improves the thermal conductivity, mechanical properties and heat resistance stability of epoxy resin adhesives, meets the thermal management needs of electronic packaging, broadens the application range, and improves the brittleness of traditional epoxy resins.
Smart Images

Figure BDA0005065165120000071 
Figure BDA0005065165120000081
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of adhesive production, and in particular to a high-performance epoxy resin adhesive and a preparation method thereof. Background Art
[0002] As one of the three major thermosetting plastics, epoxy resin has excellent adhesion, corrosion resistance, thermal stability and low curing shrinkage. It is widely used in the manufacture of adhesives, coatings and composite materials. It has become an important material in the fields of aerospace, transportation and electronic packaging. The global market demand for epoxy resin is also growing. However, due to the high cross-linking density of the irreversible network of epoxy resin, it shows obvious brittleness and low elongation at break. It is also flammable and has high toxicity of combustion smoke, which seriously limits the application prospects of epoxy resin.
[0003] For the field of electronic packaging, epoxy resin adhesive materials not only need to have good bonding properties, but also have high requirements for the electrical insulation and thermal conductivity of the material. For epoxy resin polymers, compared with ceramics and metals, its thermal conductivity is lower and cannot meet the needs of thermal management in the field of electronic packaging. For this reason, thermal conductive fillers are needed in polymers to improve the thermal conductivity of the material. However, due to the weak interface interaction between the filler and the polymer, the thermal conductivity enhancement efficiency of the material is low. In order to achieve higher thermal conductivity, it is often necessary to add a higher proportion of filler to the matrix, which in turn leads to poor interface compatibility between the filler and the matrix, causing the filler to agglomerate in the matrix, which in turn seriously affects the processing performance and mechanical properties of the material. For this reason, it is urgent to propose an effective method to overcome this problem and solve the pain points of the application of epoxy resin in electronic packaging. Summary of the invention
[0004] The purpose of the present invention is to provide a high-performance epoxy resin adhesive and a preparation method thereof in order to solve the above-mentioned deficiencies in the prior art.
[0005] The purpose of the present invention is achieved through the following technical scheme: The present invention provides a high-performance epoxy resin adhesive, comprising the following raw materials in parts by weight: 80-100 parts of epoxy resin, 10-40 parts of thermal conductive filler, 5-20 parts of toughening elastomer, 30-55 parts of curing agent, 1-5 parts of accelerator, and 10-30 parts of diluent.
[0006] Furthermore, the epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin or novolac epoxy resin.
[0007] Furthermore, the thermally conductive filler is thermally conductive particles having acrylate double bonds obtained by surface modification, and the thermally conductive particles are at least one of aluminum nitride, silicon nitride or carbon nitride.
[0008] Furthermore, the particle size of the thermally conductive particles is 3-50 μm.
[0009] In the present invention, by introducing thermally conductive particles as thermally conductive fillers, it is helpful to improve the mechanical properties, thermal conductivity and aging resistance of the epoxy resin adhesive, but this is closely related to the degree of dispersion of the thermally conductive particles on the epoxy resin matrix. The agglomeration of thermally conductive particles will cause internal defects of the epoxy resin material to a certain extent, thereby affecting the overall performance and interface bonding ability of the material. Therefore, in order to improve the agglomeration of thermally conductive particles, on the one hand, the particle size of the thermally conductive particles is adjusted, and on the other hand, the surface of the thermally conductive particles is modified to enhance the interaction between the thermally conductive particles and the epoxy groups. As a preferred embodiment of the present invention, the thermally conductive particles are compounded by aluminum nitride, silicon nitride and carbon nitride in a mass ratio of 3-4:2:1, wherein the particle size of aluminum nitride is 20-30nm, the particle size of silicon nitride is 10nm, and the particle size of carbon nitride is 3-5nm.
[0010] Furthermore, the preparation method of the thermally conductive filler comprises the following steps:
[0011] Step A, placing the thermally conductive particles in dichloromethane for ultrasonic dispersion, adding triethylamine in an ice bath to mix evenly, then adding a mixture of 2-bromoisobutyryl bromide and dichloromethane, stirring at room temperature for 20-24 hours, and then repeatedly centrifuging and washing with acetone and ethanol, and drying to obtain solid particles;
[0012] Step B, placing the solid particles obtained in step A in cyclohexanone for ultrasonic dispersion, then adding 2,3-epoxypropyl methacrylate and 2,2-bipyridine, filling the entire reaction system with inert gas, then adding a catalyst, raising the temperature to 50±3° C. for polymerization reaction, quenching in ice water after completion, washing the product with acetone, ethanol and water for multiple times, and then centrifugally drying to obtain the thermal conductive filler.
[0013] Furthermore, the preparation method of the toughened elastomer comprises the following steps: (1) placing hydrogenated hydroxyl-terminated polybutadiene and hydroxyl-terminated polybutadiene diol in a reaction container and stirring them uniformly, then adding toluene diisocyanate, an organic tin catalyst and dichloromethane thereto, dispersing them uniformly under ultrasonic conditions, and stirring at room temperature for 2-3 hours; (2) adding polyisobutylene succinic anhydride and an antioxidant to the mixture obtained in step (1), heating and stirring until the solvent evaporates to obtain a homogeneous mixed liquid, and finally curing by vacuum heating to obtain the toughened elastomer.
[0014] Furthermore, in step (1), the molar ratio of the hydroxyl groups contained in the hydrogenated hydroxyl-terminated polybutadiene to the hydroxyl-terminated polybutadiene diol is 1:1.
[0015] Furthermore, the curing agent is an acid anhydride curing agent; and the accelerator is at least one of DMP-30, tetraethylenetriamine or benzyldimethylamine.
[0016] Furthermore, the diluent is at least one of benzyl glycidyl ether, n-butyl glycidyl ether or ethylene glycol diglycidyl ether.
[0017] The present invention also provides a method for preparing the above-mentioned high-performance epoxy resin adhesive, comprising the following steps: fully mixing the epoxy resin, thermal conductive filler and diluent and heating them to 80-90°C, adding a toughening elastomer thereto and continuing to heat to 130-150°C and fully mixing, then cooling to 60-80°C, adding a curing agent and an accelerator thereto and stirring evenly, thereby obtaining the high-performance epoxy resin adhesive.
[0018] The beneficial effects of the present invention are as follows: (1) the high-performance epoxy resin adhesive provided by the present invention has good bonding strength, mechanical properties, thermal conductivity and heat resistance stability, which can meet the thermal management requirements of the adhesive in electronic packaging, further broadening the application scope of the epoxy resin adhesive, and the epoxy resin adhesive has a fast curing speed and good processing characteristics;
[0019] (2) The present invention can evenly disperse aluminum nitride, aluminum nitride and / or carbon nitride in an epoxy resin matrix by combining aluminum nitride with a reasonable particle size, and combine the surface modification of the thermally conductive particles so that the surface-treated thermally conductive particles and the epoxy resin matrix form a cross-linked structure, which significantly enhances the interfacial interaction between the thermally conductive filler and the epoxy resin matrix. The two have a relatively stable interaction, and a part of the stress is transferred from the epoxy resin matrix to the thermally conductive particles, which is beneficial to the improvement of stress transfer, mechanical properties and thermal stability, thereby making the epoxy resin adhesive have higher bonding strength and mechanical properties;
[0020] (3) The elastomer obtained by the polymerization reaction of hydrogenated hydroxy-terminated polybutadiene and hydroxy-terminated polybutadiene diol in the present invention has good compatibility with the epoxy resin matrix. The low modulus elastomer obtained by the above preparation method is used for toughening modification of epoxy resin, and the polar groups such as carboxyl and hydroxyl groups on its surface generate intermolecular forces with the epoxy resin, which can be beneficial to the compatibility of the toughened elastomer in the epoxy resin matrix, thereby helping to improve the mechanical properties of the epoxy resin and improve the brittleness problem of traditional epoxy resin. DETAILED DESCRIPTION
[0021] In order to facilitate the understanding of those skilled in the art, the present invention is further described below in conjunction with embodiments, and the contents mentioned in the implementation modes are not intended to limit the present invention.
[0022] Example 1
[0023] The present embodiment provides a high-performance epoxy resin adhesive, comprising the following raw materials in parts by weight: 85 parts of epoxy resin, 12 parts of thermal conductive filler, 8 parts of toughening elastomer, 40 parts of curing agent, 2 parts of accelerator, and 12 parts of diluent.
[0024] Furthermore, the epoxy resin is bisphenol A epoxy resin E51.
[0025] Furthermore, the thermally conductive filler is a thermally conductive particle having acrylate double bonds obtained by surface modification, and the thermally conductive particles are compounded by aluminum nitride, silicon nitride and carbon nitride in a mass ratio of 4:2:1, wherein the particle size of aluminum nitride is 30nm, the particle size of silicon nitride is 10nm, and the particle size of carbon nitride is 5nm.
[0026] Furthermore, the preparation method of the thermally conductive filler comprises the following steps:
[0027] Step A, placing the thermal conductive particles in dichloromethane at a mass volume ratio of 1:7 for ultrasonic dispersion for 10 minutes, adding triethylamine under ice bath conditions and mixing evenly (the volume ratio of triethylamine to dichloromethane is 1:10), then adding a mixed solution of 2-bromoisobutyryl bromide and dichloromethane in an equal volume to triethylamine (the volume ratio of 2-bromoisobutyryl bromide to dichloromethane is 1:5), stirring at room temperature for 20 hours, and then repeatedly centrifuging and washing with acetone and ethanol, and drying to obtain solid particles;
[0028] Step B, placing the solid particles obtained in step A in cyclohexanone at a mass volume ratio of 1:20 for ultrasonic dispersion for 30 minutes, then adding 2,3-epoxypropyl methacrylate and 2,2-bipyridine at a molar ratio of 200:1, filling the entire reaction system with inert gas, then adding 0.1wt% of cuprous bromide, raising the temperature to 50°C for polymerization reaction for 2 hours, quenching in ice water after completion, washing the product with acetone, ethanol and water for multiple times, and then centrifugally drying to obtain the thermal conductive filler.
[0029] Furthermore, the preparation method of the toughened elastomer comprises the following steps: (1) placing hydrogenated hydroxyl-terminated polybutadiene (Mn=2000) and hydroxyl-terminated polybutadiene diol (Mn=3000) in a reaction container and stirring them evenly, then adding 2.5wt% toluene diisocyanate, 1wt% organotin catalyst T-12 and a small amount of dichloromethane thereto, dispersing them evenly under ultrasonic conditions, and stirring at room temperature for 3h; (2) adding 2wt% polyisobutylene succinic anhydride and 1wt% antioxidant 264 to the mixture obtained in step (1), heating and constant temperature at 80°C, stirring until the solvent evaporates to obtain a homogeneous mixed liquid, and finally curing by vacuum heating to obtain the toughened elastomer.
[0030] Furthermore, in step (1), the molar ratio of the hydroxyl groups contained in the hydrogenated hydroxyl-terminated polybutadiene to the hydroxyl-terminated polybutadiene diol is 1:1.
[0031] Furthermore, the curing agent is maleic anhydride; the accelerator is DMP-30; and the diluent is n-butyl glycidyl ether.
[0032] The preparation method of the high-performance epoxy resin adhesive in this embodiment comprises the following steps: fully mixing epoxy resin, thermal conductive filler and diluent and heating to 90°C, adding toughening elastomer thereto and continuing to heat to 140°C and fully mixing, then cooling to 70°C, adding curing agent and accelerator thereto and stirring evenly, thus obtaining the high-performance epoxy resin adhesive.
[0033] Example 2
[0034] The present embodiment provides a high-performance epoxy resin adhesive, comprising the following raw materials in parts by weight: 90 parts of epoxy resin, 20 parts of thermal conductive filler, 13 parts of toughening elastomer, 40 parts of curing agent, 2 parts of accelerator, and 18 parts of diluent.
[0035] Furthermore, the epoxy resin is phenolic epoxy resin F51.
[0036] Furthermore, the thermally conductive filler is a thermally conductive particle having acrylate double bonds obtained by surface modification, and the thermally conductive particles are compounded by aluminum nitride, silicon nitride and carbon nitride in a mass ratio of 4:2:1, wherein the particle size of aluminum nitride is 20nm, the particle size of silicon nitride is 10nm, and the particle size of carbon nitride is 3nm.
[0037] Furthermore, the preparation method of the thermally conductive filler comprises the following steps:
[0038] Step A, placing the thermal conductive particles in dichloromethane at a mass volume ratio of 1:7 for ultrasonic dispersion for 10 minutes, adding triethylamine under ice bath conditions and mixing evenly (the volume ratio of triethylamine to dichloromethane is 1:10), then adding a mixed solution of 2-bromoisobutyryl bromide and dichloromethane in an equal volume to triethylamine (the volume ratio of 2-bromoisobutyryl bromide to dichloromethane is 1:5), stirring at room temperature for 24 hours, and then repeatedly centrifuging and washing with acetone and ethanol, and drying to obtain solid particles;
[0039] Step B, placing the solid particles obtained in step A in cyclohexanone at a mass volume ratio of 1:20 for ultrasonic dispersion for 30 minutes, then adding 2,3-epoxypropyl methacrylate and 2,2-bipyridine at a molar ratio of 200:1, filling the entire reaction system with inert gas, then adding 0.1wt% of cuprous bromide, raising the temperature to 50°C for polymerization reaction for 2 hours, quenching in ice water after completion, washing the product with acetone, ethanol and water for multiple times, and then centrifugally drying to obtain the thermal conductive filler.
[0040] Furthermore, the preparation method of the toughened elastomer comprises the following steps: (1) placing hydrogenated hydroxyl-terminated polybutadiene (Mn=2000) and hydroxyl-terminated polybutadiene diol (Mn=3000) in a reaction container and stirring them evenly, then adding 2.5wt% toluene diisocyanate, 1wt% organotin catalyst T-12 and a small amount of dichloromethane thereto, dispersing them evenly under ultrasonic conditions, and stirring at room temperature for 3h; (2) adding 2wt% polyisobutylene succinic anhydride and 1wt% antioxidant 264 to the mixture obtained in step (1), heating and constant temperature at 80°C, stirring until the solvent evaporates to obtain a homogeneous mixed liquid, and finally curing by vacuum heating to obtain the toughened elastomer.
[0041] Furthermore, in step (1), the molar ratio of the hydroxyl groups contained in the hydrogenated hydroxyl-terminated polybutadiene to the hydroxyl-terminated polybutadiene diol is 1:1.
[0042] Furthermore, the curing agent is methyltetrahydrophthalic anhydride; the accelerator is tetraethylenetriamine; and the diluent is ethylene glycol diglycidyl ether.
[0043] The preparation method of the high-performance epoxy resin adhesive in this embodiment comprises the following steps: fully mixing the epoxy resin, thermal conductive filler and diluent and heating to 80° C., adding a toughening elastomer thereto and continuing to heat to 145° C. and fully mixing, then cooling to 60° C., adding a curing agent and an accelerator thereto and stirring evenly, thereby obtaining the high-performance epoxy resin adhesive.
[0044] Example 3
[0045] The present embodiment provides a high-performance epoxy resin adhesive, comprising the following raw materials in parts by weight: 100 parts of epoxy resin, 30 parts of thermal conductive filler, 17 parts of toughening elastomer, 30-55 parts of curing agent, 1-5 parts of accelerator, and 10-30 parts of diluent.
[0046] Furthermore, the thermally conductive filler is a thermally conductive particle having acrylate double bonds obtained by surface modification, and the thermally conductive particles are compounded by aluminum nitride, silicon nitride and carbon nitride in a mass ratio of 4:2:1, wherein the particle size of aluminum nitride is 20nm, the particle size of silicon nitride is 10nm, and the particle size of carbon nitride is 5nm.
[0047] Furthermore, the epoxy resin is bisphenol F epoxy resin DER324.
[0048] Furthermore, the thermally conductive filler is a thermally conductive particle having acrylate double bonds obtained by surface modification, and the thermally conductive particles are compounded by aluminum nitride, silicon nitride and carbon nitride in a mass ratio of 4:2:1, wherein the particle size of aluminum nitride is 20nm, the particle size of silicon nitride is 10nm, and the particle size of carbon nitride is 3nm.
[0049] Furthermore, the preparation method of the thermally conductive filler comprises the following steps:
[0050] Step A, placing the thermal conductive particles in dichloromethane at a mass volume ratio of 1:7 for ultrasonic dispersion for 10 minutes, adding triethylamine under ice bath conditions and mixing evenly (the volume ratio of triethylamine to dichloromethane is 1:10), then adding a mixed solution of 2-bromoisobutyryl bromide and dichloromethane in an equal volume to triethylamine (the volume ratio of 2-bromoisobutyryl bromide to dichloromethane is 1:5), stirring at room temperature for 24 hours, and then repeatedly centrifuging and washing with acetone and ethanol, and drying to obtain solid particles;
[0051] Step B, placing the solid particles obtained in step A in cyclohexanone at a mass volume ratio of 1:20 for ultrasonic dispersion for 30 minutes, then adding 2,3-epoxypropyl methacrylate and 2,2-bipyridine at a molar ratio of 200:1, filling the entire reaction system with inert gas, then adding 0.1wt% of cuprous bromide, raising the temperature to 50°C for polymerization reaction for 2 hours, quenching in ice water after completion, washing the product with acetone, ethanol and water for multiple times, and then centrifugally drying to obtain the thermal conductive filler.
[0052] Furthermore, the preparation method of the toughened elastomer comprises the following steps: (1) placing hydrogenated hydroxyl-terminated polybutadiene (Mn=2000) and hydroxyl-terminated polybutadiene diol (Mn=3000) in a reaction container and stirring them evenly, then adding 2.5wt% toluene diisocyanate, 1wt% organotin catalyst T-12 and a small amount of dichloromethane thereto, dispersing them evenly under ultrasonic conditions, and stirring at room temperature for 3h; (2) adding 2wt% polyisobutylene succinic anhydride and 1wt% antioxidant 264 to the mixture obtained in step (1), heating and constant temperature at 80°C, stirring until the solvent evaporates to obtain a homogeneous mixed liquid, and finally curing by vacuum heating to obtain the toughened elastomer.
[0053] Furthermore, in step (1), the molar ratio of the hydroxyl groups contained in the hydrogenated hydroxyl-terminated polybutadiene to the hydroxyl-terminated polybutadiene diol is 1:1.
[0054] Furthermore, the curing agent is methyl nadic anhydride; and the accelerator is benzyl dimethylamine.
[0055] Furthermore, the diluent is benzyl glycidyl ether.
[0056] The preparation method of the high-performance epoxy resin adhesive in this embodiment comprises the following steps: fully mixing the epoxy resin, thermal conductive filler and diluent and heating to 85° C., adding a toughening elastomer thereto and continuing to heat to 150° C. and fully mixing, then cooling to 60° C., adding a curing agent and an accelerator thereto and stirring evenly, thereby obtaining the high-performance epoxy resin adhesive.
[0057] Comparative Example 1
[0058] The difference between this comparative example and Example 2 is that this comparative example uses untreated spherical aluminum nitride particles as thermal conductive fillers, and the particle size of the spherical aluminum nitride particles is 20 μm.
[0059] Comparative Example 2
[0060] The difference between this comparative example and Example 2 is that the thermally conductive filler used in this comparative example is thermally conductive particles that have not been surface-modified, and the thermally conductive particles are compounded with aluminum nitride, silicon nitride, and carbon nitride in a mass ratio of 4:2:1, wherein the particle size of aluminum nitride is 20 nm, the particle size of silicon nitride is 10 nm, and the particle size of carbon nitride is 3 nm. .
[0061] Comparative Example 3
[0062] The difference between this comparative example and Example 2 is that the toughening elastomer in Example 2 is not added to this comparative example.
[0063] Comparative Example 4
[0064] The difference between this comparative example and Example 2 is that the preparation method of the toughened elastomer described in this comparative example comprises the following steps: (1) placing terminal hydroxyl polyisoprene and polyether diol in a reaction container and stirring evenly, then adding 2.5wt% toluene diisocyanate, 1wt% organotin catalyst T-12 and a small amount of dichloromethane thereto, dispersing evenly under ultrasonic conditions, and stirring at room temperature for 3h; (2) adding 2wt% polyisobutylene succinic anhydride and 1wt% antioxidant 264 to the mixture obtained in step (1), heating and constant temperature at 80°C, stirring until the solvent evaporates to obtain a homogeneous mixed liquid, and finally curing by vacuum heating to obtain the toughened elastomer.
[0065] Furthermore, in step (1), the molar ratio of the hydroxyl groups in the hydroxyl-terminated polyisoprene and the hydroxyl groups in the polyether diol is 1:1.
[0066] In the present invention, the high-performance epoxy resin adhesive prepared in the above-mentioned embodiments 1-3 and comparative examples 1-3 is subjected to performance tests, including tensile strength, impact strength, shear strength and heat resistance tests. Among them, the tensile strength is tested using GB / T2567-2008, and the impact strength (without notch) is tested using ASTM D256-10. The test pieces used for the test are the test pieces of the epoxy resin adhesive prepared in each embodiment and comparative example after heating and curing, and the size is 80*10*4mm; the shear strength is tested using GB / T 7124-2008, and is divided into two groups at room temperature and after aging at 150°C for 240h; the heat resistance of the epoxy resin adhesive is tested using thermogravimetric analysis, the test temperature is 25-800°C, the heating rate is 10°C / min, and the test atmosphere is nitrogen and air.
[0067] The results are shown in the following table.
[0068]
[0069]
[0070] It can be seen from the above data that the epoxy resin adhesive prepared by Examples 1-3 of the present invention has high tensile strength, impact strength and shear strength. Comparison of Example 2 with Comparative Examples 1-2 shows that the particle size configuration and surface modification of the thermally conductive filler have played a significant role in improving the mechanical properties, bonding properties and heat resistance of the epoxy resin adhesive. Comparison of Example 2 with Comparative Examples 3-4 shows that under the action of the toughening elastomer, the toughness and impact resistance of the epoxy resin adhesive of the present invention are significantly improved. On the other hand, the epoxy resin adhesive prepared by Examples 1-3 of the present invention has a higher glass transition temperature Tg, indicating that it has good heat resistance. This is mainly because the modified thermally conductive filler is evenly dispersed on the epoxy resin matrix and has a good bonding force, and the high thermal conductivity and high stability of the thermally conductive particles are used to significantly improve the heat resistance of the epoxy resin adhesive.
[0071] The above specific embodiments are further explanations of the technical solutions and beneficial effects of the present invention, and are not limitations of the implementation methods. For those skilled in the art, any obvious replacements that do not depart from the concept of the present invention are within the protection scope of the present invention.
Claims
1. A high performance epoxy resin adhesive, characterized in that: The invention comprises the following raw materials in parts by weight: 80-100 parts of epoxy resin, 10-40 parts of thermal conductive filler, 5-20 parts of toughening elastomer, 30-55 parts of curing agent, 1-5 parts of accelerator and 10-30 parts of diluent.
2. The high performance epoxy resin adhesive according to claim 1, characterized in that: The epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin or novolac epoxy resin.
3. The high performance epoxy resin adhesive according to claim 1, characterized in that: The thermally conductive filler is thermally conductive particles having acrylate double bonds obtained by surface modification, and the thermally conductive particles are at least one of aluminum nitride, silicon nitride or carbon nitride.
4. The high performance epoxy resin adhesive according to claim 3, characterized in that: The particle size of the thermally conductive particles is 3-50 μm.
5. The high performance epoxy resin adhesive according to claim 3, characterized in that: The preparation method of the thermal conductive filler comprises the following steps: Step A, placing the thermally conductive particles in dichloromethane for ultrasonic dispersion, adding triethylamine in an ice bath to mix evenly, then adding a mixture of 2-bromoisobutyryl bromide and dichloromethane, stirring at room temperature for 20-24 hours, and then repeatedly centrifuging and washing with acetone and ethanol, and drying to obtain solid particles; Step B, placing the solid particles obtained in step A in cyclohexanone for ultrasonic dispersion, then adding 2,3-epoxypropyl methacrylate and 2,2-bipyridine, filling the entire reaction system with inert gas, then adding a catalyst, raising the temperature to 50±3° C. for polymerization reaction, quenching in ice water after completion, washing the product with acetone, ethanol and water for multiple times, and then centrifugally drying to obtain the thermal conductive filler.
6. The high performance epoxy resin adhesive according to claim 1, characterized in that: The preparation method of the toughened elastomer comprises the following steps: (1) placing hydrogenated hydroxyl-terminated polybutadiene and hydroxyl-terminated polybutadiene diol in a reaction container and stirring them uniformly, then adding toluene diisocyanate, an organic tin catalyst and dichloromethane thereto, dispersing them uniformly under ultrasonic conditions, and stirring them at room temperature for 2-3 hours; (2) adding polyisobutylene succinic anhydride and an antioxidant to the mixture obtained in step (1), heating and stirring until the solvent evaporates to obtain a homogeneous mixed liquid, and finally curing by vacuum heating to obtain the toughened elastomer.
7. The high performance epoxy resin adhesive according to claim 1, characterized in that: The curing agent is an acid anhydride curing agent.
8. The high performance epoxy resin adhesive according to claim 1, characterized in that: The accelerator is at least one of DMP-30, tetraethylenetriamine or benzyldimethylamine.
9. The high performance epoxy resin adhesive according to claim 1, characterized in that: The diluent is at least one of benzyl glycidyl ether, n-butyl glycidyl ether or ethylene glycol diglycidyl ether.
10. The method for preparing the high performance epoxy resin adhesive according to any one of claims 1 to 9, characterized in that: The method comprises the following steps: fully mixing epoxy resin, thermal conductive filler and diluent and heating the mixture to 80-90°C, adding toughening elastomer and continuing to heat the mixture to 130-150°C and fully mixing the mixture, then cooling the mixture to 60-80°C, adding curing agent and accelerator and stirring the mixture evenly, thereby obtaining the high-performance epoxy resin adhesive.
Citation Information
Cited By
Epoxy resin-based composition and application thereof in electronic packaging
CN121293681A
An epoxy resin-based composition and its use in electronic encapsulation
CN121293681B
