High-reliability epoxy adhesive for IC (integrated circuit) packaging and preparation process of high-reliability epoxy adhesive

Abstract

The invention relates to the technical field of epoxy adhesives, in particular to a high-reliability epoxy adhesive for IC packaging and a preparation process of the high-reliability epoxy adhesive. The high-reliability epoxy adhesive for IC packaging is prepared from the following raw materials in parts by weight: 40 to 50 parts of bisphenol F type epoxy resin, 12 to 15 parts of novolac epoxy resin, 5 to 7 parts of a synergistic auxiliary agent, 1 to 3 parts of methylhexahydrophthalic anhydride, 2 to 4 parts of 2-ethyl-4-methylimidazole, 1 to 4 parts of a de-foaming agent and 1 to 3 parts of an antioxidant, the prepared high-reliability epoxy adhesive for IC packaging not only has better high-temperature resistance, but also has excellent low thermal expansion coefficient, high bonding strength and long-term stability, and the quality of the high-reliability epoxy adhesive is effectively guaranteed.

Description

Technical Field

[0001] This invention relates to the field of epoxy adhesive technology, specifically to a high-reliability epoxy adhesive for IC packaging and its preparation process. Background Technology

[0002] Integrated circuit packaging is a critical process that secures a chip to a substrate, connects it to external pins via electrical connections, and protects the chip from mechanical damage, dust, and chemical corrosion. In the field of integrated circuit (IC) packaging, epoxy adhesive is a key material that must ensure device reliability under harsh environments.

[0003] However, traditional polyethylene (PE) medical packaging film has the following problems:

[0004] (1) Traditional epoxy adhesives have low crosslinking density of epoxy resin matrix and glass transition temperature (Tg) usually <150℃, which cannot meet the requirements of high frequency and high power packaging for heat resistance (Tg≥160℃).

[0005] (2) Traditional epoxy adhesives have insufficient long-term effect on the modification of the filler-resin interface by ordinary silane coupling agents (such as KH-550), resulting in a decrease in bond strength (shear strength <20MPa).

[0006] (3) At the same time, traditional epoxy adhesives have poor stability, which affects the encapsulation effect.

[0007] Based on this, the present invention provides a high-reliability epoxy adhesive for IC packaging and its preparation process to solve the above-mentioned technical problems. Summary of the Invention

[0008] The purpose of this invention is to provide a high-reliability epoxy adhesive for IC packaging and its preparation process. The prepared high-reliability epoxy adhesive for IC packaging not only has good high-temperature resistance, but also has excellent low coefficient of thermal expansion, high bonding strength and long-term stability, effectively ensuring its quality and performance.

[0009] To achieve the above objectives, the present invention provides the following technical solution:

[0010] A first aspect of the present invention provides a high-reliability epoxy adhesive for IC packaging, comprising the following parts by weight of raw materials: 40-50 parts of bisphenol F type epoxy resin, 12-15 parts of phenolic epoxy resin, 5-7 parts of synergistic additives, 1-3 parts of methylhexahydrophthalic anhydride, 2-4 parts of 2-ethyl-4-methylimidazole, 1-4 parts of defoamer and 1-3 parts of antioxidant.

[0011] A further feature of this invention is that the preparation process of the synergistic adjuvant is as follows:

[0012] The composite material was placed in acetone and ultrasonically treated for 30-40 min at a dosage ratio of 0.2-0.4 g / mL, and then treated for 10-15 min under vacuum conditions of -0.095 to -0.092 MPa and 450-500 r / min to obtain the first base material.

[0013] Isophorone diisocyanate and polyurethane prepolymer were mixed at a mass ratio of 0.15 to 0.2:1. Dibutyltin dilaurate (1.1 to 1.3% by weight of polyurethane prepolymer) was added to the mixture. The mixture was treated at 55 to 60°C for 120 to 140 minutes and then diluted with acetone (460 to 470% by weight of polyurethane prepolymer) to obtain a diluted solution.

[0014] The first base material and the diluent were ultrasonically treated for 60-70 minutes at a mass ratio of 10-12:1, and then dried under vacuum at 60-70°C for 12-14 hours to obtain the second base material.

[0015] The second base material was placed in a perfluorooctyltriethoxysilane ethanol solution at a dosage ratio of 0.12–0.15 g / mL, and magnetically stirred at 55–60 °C for 4–5 h. After centrifugation, it was washed 2–4 times with anhydrous ethanol and then dried under vacuum at 120–130 °C for 8–10 h to obtain the synergistic adjuvant.

[0016] The present invention is further configured such that the composite material is prepared by mixing and compounding modified silica with a particle size of 5 μm, modified silica with a particle size of 0.5 μm and modified silica with a particle size of 50 nm in a mass ratio of 5 to 4: 3 to 2: 1.

[0017] The present invention is further configured such that the preparation process of the modified silica is as follows:

[0018] Spherical silica was placed in KH-560 ethanol solution at a dosage ratio of 0.05-0.1 g / mL, and magnetically stirred at 50-60℃ for 120-130 min. After centrifugation, it was washed 2-4 times with deionized water and then dried under vacuum at 60-70℃ for 12-14 h to obtain pretreated silica.

[0019] Zirconium oxynitrate was mixed in water at a ratio of 0.02–0.03 g / mL to obtain a pre-mixed solution. Pretreated silica was then added to the pre-mixed solution at a ratio of 0.05–0.07 g / mL. The pH was adjusted to 8.8–9 with ammonia and treated at 55–60 °C for 6–7 h. Finally, the silica was calcined at 600–650 °C for 120–140 min to obtain modified silica.

[0020] A further provision of the present invention is that the preparation process of the KH-560 ethanol solution is as follows:

[0021] KH-560 was mixed thoroughly in ethanol at a dosage ratio of 0.02–0.05 g / mL.

[0022] Add acetic acid to it and adjust the pH to 4-5 to obtain KH-560 ethanol solution.

[0023] A further feature of this invention is that the perfluorooctyltriethoxysilane ethanol solution is prepared by mixing and compounding perfluorooctyltriethoxysilane and ethanol at a mass ratio of 1:95-98.

[0024] The present invention is further configured such that the defoamer is a compound of defoamer BYK-066N and defoamer BYK-1790 in a mass ratio of 1:10 to 12.

[0025] The present invention is further configured such that the antioxidant is selected from any one of antioxidant 1010, antioxidant 1076, and antioxidant CA.

[0026] A second aspect of the present invention also provides a process for preparing the above-mentioned high-reliability IC packaging epoxy adhesive, characterized by comprising the following steps:

[0027] Step 1: Accurately weigh the bisphenol F type epoxy resin, phenolic epoxy resin, synergist, methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, defoamer, and antioxidant, and set aside.

[0028] Step 2: Preheat bisphenol F epoxy resin and phenolic epoxy resin separately at 50°C for 30 minutes. Then mix the preheated bisphenol F epoxy resin and phenolic epoxy resin, add synergistic additives, defoamers and antioxidants, and treat at 500-600 r / min for 10-15 minutes. Then add methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole and continue stirring for 12-15 minutes. Vacuum degassing and storage are then performed to prepare the high-reliability IC packaging epoxy adhesive product.

[0029] Compared with the prior art, the beneficial effects of the present invention are:

[0030] This invention uses bisphenol F type epoxy resin, phenolic epoxy resin, synergistic additives, methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, defoamer, and antioxidants as raw materials. The process involves preheating the bisphenol F type epoxy resin and phenolic epoxy resin separately, then mixing the preheated bisphenol F type epoxy resin and phenolic epoxy resin. Synergistic additives, defoamers, and antioxidants are then added and stirred. Methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole are then added and the mixture is stirred further. The mixture is then vacuum degassed and stored to obtain a high-reliability epoxy adhesive for IC packaging. The prepared high-reliability epoxy adhesive for IC packaging not only has good high-temperature resistance but also excellent low coefficient of thermal expansion, high adhesive strength, and long-term stability, effectively ensuring its quality. The high-reliability epoxy adhesive for IC packaging and its preparation process provided by this invention have a broader market prospect and are more suitable for widespread application. Detailed Implementation

[0031] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0032] Example 1

[0033] This embodiment provides a high-reliability epoxy adhesive for IC packaging, which is composed of the following raw materials in parts by weight: 40 parts bisphenol F type epoxy resin, 12 parts phenolic epoxy resin, 5 parts synergistic additives, 1 part methylhexahydrophthalic anhydride, 2 parts 2-ethyl-4-methylimidazole, 1 part defoamer and 1 part antioxidant.

[0034] In this embodiment, it should be noted that the bisphenol F type epoxy resin was purchased from Suzhou Senfida Chemical Co., Ltd., and the phenolic epoxy resin was purchased from Shandong Xindongneng Chemical Co., Ltd.

[0035] The preparation process of the synergistic agent is as follows:

[0036] The composite material was placed in acetone and ultrasonically treated for 30 min at a dosage ratio of 0.2 g / mL, and then treated under vacuum of -0.095 MPa and 450 r / min for 10 min to obtain the first base material.

[0037] Isophorone diisocyanate and polyurethane prepolymer were mixed at a mass ratio of 0.15:1. Dibutyltin dilaurate (1.1% by weight of polyurethane prepolymer) was added to the mixture. The mixture was treated at 55°C for 120 min and then diluted with acetone (460% by weight of polyurethane prepolymer) to obtain a diluted solution.

[0038] The first base material and the diluent were ultrasonically treated for 60 min at a mass ratio of 10:1, and then dried under vacuum at 60°C for 12 h to obtain the second base material.

[0039] The second base material was placed in a perfluorooctyltriethoxysilane ethanol solution at a dosage ratio of 0.12 g / mL, and magnetically stirred at 55 °C for 4 h. After centrifugation, it was washed once with anhydrous ethanol and then dried under vacuum at 120 °C for 8 h to obtain the synergistic additive.

[0040] Furthermore, the composite material is made by mixing and compounding modified silica with a particle size of 5μm, modified silica with a particle size of 0.5μm and modified silica with a particle size of 50nm in a mass ratio of 5:3:1.

[0041] In this embodiment, it should be noted that the polyurethane prepolymer was purchased from Hubei Watson Chemical Technology Co., Ltd.

[0042] The preparation process of modified silica is as follows:

[0043] Spherical silica was placed in KH-560 ethanol solution at a dosage ratio of 0.05 g / mL, and magnetically stirred at 50 °C for 120 min. After centrifugation, it was washed twice with deionized water and then dried under vacuum at 60 °C for 12 h to obtain pretreated silica.

[0044] Zirconium oxynitrate was mixed in water at a ratio of 0.02 g / mL to obtain a pre-mixed solution. Then, pretreated silica was added to the pre-mixed solution at a ratio of 0.05 g / mL. The pH was adjusted to 8.8 with ammonia water, and the solution was treated at 550℃ for 6 h. Finally, the solution was calcined at 600℃ for 120 min to obtain modified silica.

[0045] The preparation process of KH-560 ethanol solution is as follows:

[0046] KH-560 was mixed thoroughly in ethanol at a dosage ratio of 0.02 g / mL.

[0047] Acetic acid was added to the solution to adjust the pH to 4, resulting in a KH-560 ethanol solution.

[0048] In addition, the perfluorooctyltriethoxysilane ethanol solution is prepared by mixing and compounding perfluorooctyltriethoxysilane and ethanol at a mass ratio of 1:95.

[0049] The defoamer is composed of defoamer BYK-066N and defoamer BYK-1790 in a mass ratio of 1:10.

[0050] The antioxidant selected is antioxidant 1010.

[0051] Furthermore, this embodiment also provides a preparation process for the above-mentioned high-reliability IC packaging epoxy adhesive, characterized by including the following steps:

[0052] Step 1: Accurately weigh the bisphenol F type epoxy resin, phenolic epoxy resin, synergist, methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, defoamer, and antioxidant, and set aside.

[0053] Step 2: Preheat bisphenol F epoxy resin and phenolic epoxy resin separately at 50°C for 30 min. Then mix the preheated bisphenol F epoxy resin and phenolic epoxy resin, add synergistic additives, defoamers and antioxidants, and treat at 500 r / min for 10 min. Then add methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole and continue stirring for 12 min. Vacuum degassing and storage are then performed to prepare the high-reliability IC packaging epoxy adhesive product.

[0054] Example 2

[0055] The preparation process of the high-reliability IC packaging epoxy adhesive provided in this embodiment is basically the same as that in Embodiment 1, except that the specific raw material composition and preparation process of the high-reliability IC packaging epoxy adhesive in this embodiment are different. The specific raw material composition and preparation process of the high-reliability IC packaging epoxy adhesive in this embodiment are as follows:

[0056] A high-reliability epoxy adhesive for IC packaging is composed of the following raw materials in parts by weight: 45 parts bisphenol F type epoxy resin, 13 parts phenolic epoxy resin, 6 parts synergistic additives, 2 parts methylhexahydrophthalic anhydride, 3 parts 2-ethyl-4-methylimidazole, 2 parts defoamer and 2 parts antioxidant.

[0057] In this embodiment, it should be noted that the bisphenol F type epoxy resin was purchased from Suzhou Senfida Chemical Co., Ltd., and the phenolic epoxy resin was purchased from Shandong Xindongneng Chemical Co., Ltd.

[0058] The preparation process of the synergistic agent is as follows:

[0059] The composite material was placed in acetone and ultrasonically treated for 35 min at a dosage ratio of 0.3 g / mL, and then treated for 12 min under a vacuum of -0.094 MPa and a speed of 450-500 r / min to obtain the first base material.

[0060] Isophorone diisocyanate and polyurethane prepolymer were mixed at a mass ratio of 0.17:1. Dibutyltin dilaurate (1.2% by weight of polyurethane prepolymer) was added to the mixture. The mixture was treated at 57°C for 130 min and then diluted with acetone (465% by weight of polyurethane prepolymer) to obtain a diluted solution.

[0061] The first base material and the diluent were ultrasonically treated for 65 minutes at a mass ratio of 11:1, and then dried under vacuum at 65°C for 13 hours to obtain the second base material.

[0062] The second base material was placed in a perfluorooctyltriethoxysilane ethanol solution at a dosage ratio of 0.13 g / mL, and magnetically stirred at 57°C for 5 h. After centrifugation, it was washed three times with anhydrous ethanol and then dried under vacuum at 125°C for 9 h to obtain the synergistic adjuvant.

[0063] Furthermore, the composite material is made by mixing modified silica with a particle size of 5μm, modified silica with a particle size of 0.5μm, and modified silica with a particle size of 50nm in a mass ratio of 4:2:1.

[0064] In this embodiment, it should be noted that the polyurethane prepolymer was purchased from Hubei Watson Chemical Technology Co., Ltd.

[0065] The preparation process of modified silica is as follows:

[0066] Spherical silica was placed in KH-560 ethanol solution at a dosage ratio of 0.07 g / mL, and magnetically stirred at 55 °C for 125 min. After centrifugation, it was washed three times with deionized water and then dried under vacuum at 65 °C for 13 h to obtain pretreated silica.

[0067] Zirconium oxynitrate was mixed in water at a ratio of 0.03 g / mL to obtain a pre-mixed solution. Then, pretreated silica was added to the pre-mixed solution at a ratio of 0.06 g / mL. The pH was adjusted to 8.9 with ammonia water, and the solution was treated at 57°C for 7 h. Finally, the solution was calcined at 625°C for 130 min to obtain modified silica.

[0068] The preparation process of KH-560 ethanol solution is as follows:

[0069] KH-560 was mixed thoroughly in ethanol at a dosage ratio of 0.03 g / mL.

[0070] Add acetic acid to it and adjust the pH to 5 to obtain KH-560 ethanol solution.

[0071] In addition, the perfluorooctyltriethoxysilane ethanol solution is prepared by mixing and compounding perfluorooctyltriethoxysilane and ethanol at a mass ratio of 1:97.

[0072] The defoamer is composed of defoamer BYK-066N and defoamer BYK-1790 in a mass ratio of 1:11.

[0073] Antioxidant 1076 was selected as the antioxidant.

[0074] Furthermore, this embodiment also provides a preparation process for the above-mentioned high-reliability IC packaging epoxy adhesive, characterized by including the following steps:

[0075] Step 1: Accurately weigh the bisphenol F type epoxy resin, phenolic epoxy resin, synergist, methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, defoamer, and antioxidant, and set aside.

[0076] Step 2: Preheat bisphenol F epoxy resin and phenolic epoxy resin separately at 50°C for 30 min. Then mix the preheated bisphenol F epoxy resin and phenolic epoxy resin, add synergistic additives, defoamers and antioxidants, and treat at 550 r / min for 12 min. Then add methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole and continue stirring for 13 min. Vacuum degassing and storage are then performed to prepare the high-reliability IC packaging epoxy adhesive product.

[0077] Example 3

[0078] The preparation process of the high-reliability IC packaging epoxy adhesive provided in this embodiment is basically the same as that in Embodiment 1, except that the specific raw material composition and preparation process of the high-reliability IC packaging epoxy adhesive in this embodiment are different. The specific raw material composition and preparation process of the high-reliability IC packaging epoxy adhesive in this embodiment are as follows:

[0079] A high-reliability IC packaging epoxy adhesive is composed of the following raw materials in parts by weight: 50 parts bisphenol F type epoxy resin, 15 parts phenolic epoxy resin, 7 parts synergistic additives, 3 parts methylhexahydrophthalic anhydride, 4 parts 2-ethyl-4-methylimidazole, 4 parts defoamer and 3 parts antioxidant.

[0080] In this embodiment, it should be noted that the bisphenol F type epoxy resin was purchased from Suzhou Senfida Chemical Co., Ltd., and the phenolic epoxy resin was purchased from Shandong Xindongneng Chemical Co., Ltd.

[0081] The preparation process of the synergistic agent is as follows:

[0082] The composite material was placed in acetone and ultrasonically treated for 40 min at a dosage ratio of 0.4 g / mL, and then treated under vacuum of -0.092 MPa and 500 r / min for 15 min to obtain the first base material.

[0083] Isophorone diisocyanate and polyurethane prepolymer were mixed at a mass ratio of 0.2:1. Dibutyltin dilaurate (1.3% by weight of polyurethane prepolymer) was added to the mixture. The mixture was treated at 60°C for 140 min and then diluted with acetone (470% by weight of polyurethane prepolymer) to obtain a diluted solution.

[0084] The first base material and the diluent were ultrasonically treated for 70 min at a mass ratio of 12:1, and then dried under vacuum at 70°C for 14 h to obtain the second base material.

[0085] The second base material was placed in a perfluorooctyltriethoxysilane ethanol solution at a dosage ratio of 0.15 g / mL, and magnetically stirred at 60 °C for 5 h. After centrifugation, it was washed four times with anhydrous ethanol and then dried under vacuum at 130 °C for 10 h to obtain the synergistic agent.

[0086] Furthermore, the composite material is made by mixing modified silica with a particle size of 5μm, modified silica with a particle size of 0.5μm, and modified silica with a particle size of 50nm in a mass ratio of 4:2:1.

[0087] In this embodiment, it should be noted that the polyurethane prepolymer was purchased from Hubei Watson Chemical Technology Co., Ltd.

[0088] The preparation process of modified silica is as follows:

[0089] Spherical silica was placed in KH-560 ethanol solution at a dosage ratio of 0.1 g / mL, and magnetically stirred at 60 °C for 130 min. After centrifugation, it was washed 4 times with deionized water and then dried under vacuum at 70 °C for 14 h to obtain pretreated silica.

[0090] Zirconium oxynitrate was mixed in water at a ratio of 0.03 g / mL to obtain a pre-mixed solution. Then, pretreated silica was added to the pre-mixed solution at a ratio of 0.07 g / mL. The pH was adjusted to 9 with ammonia water, and the solution was treated at 60°C for 7 h. Finally, the solution was calcined at 650°C for 140 min to obtain modified silica.

[0091] The preparation process of KH-560 ethanol solution is as follows:

[0092] KH-560 was mixed thoroughly in ethanol at a dosage ratio of 0.05 g / mL.

[0093] Add acetic acid to it and adjust the pH to 5 to obtain KH-560 ethanol solution.

[0094] In addition, the perfluorooctyltriethoxysilane ethanol solution is prepared by mixing and compounding perfluorooctyltriethoxysilane and ethanol at a mass ratio of 1:98.

[0095] The defoamer is composed of defoamer BYK-066N and defoamer BYK-1790 in a mass ratio of 1:12.

[0096] The antioxidant selected is antioxidant CA.

[0097] Furthermore, this embodiment also provides a preparation process for the above-mentioned high-reliability IC packaging epoxy adhesive, characterized by including the following steps:

[0098] Step 1: Accurately weigh the bisphenol F type epoxy resin, phenolic epoxy resin, synergist, methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, defoamer, and antioxidant, and set aside.

[0099] Step 2: Preheat bisphenol F epoxy resin and phenolic epoxy resin separately at 50°C for 30 min. Then mix the preheated bisphenol F epoxy resin and phenolic epoxy resin, add synergistic additives, defoamers and antioxidants, and treat at 550 r / min for 12 min. Then add methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole and continue stirring for 13 min. Vacuum degassing and storage are then performed to prepare the high-reliability IC packaging epoxy adhesive product.

[0100] Comparative Example 1: The difference from Example 1 is that this example does not contain synergistic adjuvants.

[0101] Comparative Example 2: The difference from Example 1 is that the composite material in this example is replaced by an equal amount of modified silica with a particle size of 5μm.

[0102] Comparative Example 3: The difference from Example 1 is that the composite material in this example is replaced by an equal amount of spherical silica.

[0103] Performance Testing: The epoxy adhesive samples for high-reliability IC packaging provided in Examples 1-3 and Comparative Examples 1-3 were labeled as Examples 1-3 and Comparative Examples 1-3, respectively; and the relevant performance of the epoxy adhesives for high-reliability IC packaging provided in Examples 1-3 and Comparative Examples 1-2 were tested as follows:

[0104] 1. High temperature resistance test: The test method is GB / T 19466.2-2004 (Part 2, 10℃ / min, nitrogen atmosphere); ISO 11358:2021 (10℃ / min, nitrogen flow rate 50mL / min).

[0105] 2. Low coefficient of thermal expansion test: The test method is ASTM E831-19 (sample size: 10mm×10mm×2mm, heating rate 5℃ / min, load 0.05N).

[0106] 3. Bond strength test: The test method is ASTM D1002-10 (overlap area: 12.5mm×25mm, adhesive layer thickness 0.1mm, tensile rate 1.3mm / min).

[0107] 4. Stability test: The test method is JEDEC JESD22-A101 (the sample is placed in an environment of 85℃ / 85%RH for 1000h).

[0108] The obtained test data are recorded in Tables 1 to 4 below:

[0109] Table 1. High-temperature resistance test results of epoxy adhesives in each group.

[0110]

[0111]

[0112] Table 2. Test results of low thermal expansion coefficient of each group of epoxy adhesives

[0113] Group Low coefficient of thermal expansion (ppm / ℃) Example 1 group 18.4 Example 2 group 16.2 Example 3 15.6 Comparison Group 1 32.1 Comparison of 2 groups 25.3 Comparison of 3 groups 38.3

[0114] Table 3. Test results of adhesive strength performance of each group of epoxy adhesives

[0115] Group Shear strength (MPa) Example 1 group 28.2 Example 2 group 30.8 Example 3 33.5 Comparison Group 1 15.6 Comparison of 2 groups 20.2 Comparison of 3 groups 12.8

[0116] Table 4. Stability test results of epoxy adhesives in each group

[0117]

[0118]

[0119] By comparing and analyzing the relevant data in Tables 1 to 4, it can be seen that the high-reliability epoxy adhesive for IC packaging prepared by this invention not only has good high-temperature resistance, but also excellent low coefficient of thermal expansion, high bonding strength, and long-term stability, effectively ensuring its quality. This indicates that the high-reliability epoxy adhesive for IC packaging and its preparation process provided by this invention have a broader market prospect and are more suitable for widespread application.

[0120] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0121] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. A high-reliability epoxy adhesive for IC packaging, characterized in that, It is composed of the following raw materials in parts by weight: 40-50 parts of bisphenol F type epoxy resin, 12-15 parts of phenolic epoxy resin, 5-7 parts of synergistic additives, 1-3 parts of methylhexahydrophthalic anhydride, 2-4 parts of 2-ethyl-4-methylimidazole, 1-4 parts of defoamer and 1-3 parts of antioxidant.

2. The epoxy adhesive for high-reliability IC packaging according to claim 1, characterized in that, The preparation process of the synergistic agent is as follows: The composite material was placed in acetone and ultrasonically treated for 30-40 min at a dosage ratio of 0.2-0.4 g / mL, and then treated for 10-15 min under vacuum conditions of -0.095 to -0.092 MPa and 450-500 r / min to obtain the first base material. Isophorone diisocyanate and polyurethane prepolymer were mixed at a mass ratio of 0.15 to 0.2:

1. Dibutyltin dilaurate (1.1 to 1.3% by weight of polyurethane prepolymer) was added to the mixture. The mixture was treated at 55 to 60°C for 120 to 140 minutes and then diluted with acetone (460 to 470% by weight of polyurethane prepolymer) to obtain a diluted solution. The first base material and the diluent were ultrasonically treated for 60-70 minutes at a mass ratio of 10-12:1, and then dried under vacuum at 60-70°C for 12-14 hours to obtain the second base material. The second base material was placed in a perfluorooctyltriethoxysilane ethanol solution at a dosage ratio of 0.12–0.15 g / mL, and magnetically stirred at 55–60 °C for 4–5 h. After centrifugation, it was washed 2–4 times with anhydrous ethanol and then dried under vacuum at 120–130 °C for 8–10 h to obtain the synergistic adjuvant.

3. The epoxy adhesive for high-reliability IC packaging according to claim 2, characterized in that, The composite material is prepared by mixing modified silica with a particle size of 5 μm, modified silica with a particle size of 0.5 μm, and modified silica with a particle size of 50 nm in a mass ratio of 5 to 4:3 to 2:

1.

4. The epoxy adhesive for high-reliability IC packaging according to claim 3, characterized in that, The preparation process of the modified silica is as follows: Spherical silica was placed in KH-560 ethanol solution at a dosage ratio of 0.05-0.1 g / mL, and magnetically stirred at 50-60℃ for 120-130 min. After centrifugation, it was washed 2-4 times with deionized water and then dried under vacuum at 60-70℃ for 12-14 h to obtain pretreated silica. Zirconium oxynitrate was mixed in water at a ratio of 0.02–0.03 g / mL to obtain a pre-mixed solution. Pretreated silica was then added to the pre-mixed solution at a ratio of 0.05–0.07 g / mL. The pH was adjusted to 8.8–9 with ammonia and treated at 55–60 °C for 6–7 h. Finally, the silica was calcined at 600–650 °C for 120–140 min to obtain modified silica.

5. The epoxy adhesive for high-reliability IC packaging according to claim 4, characterized in that, The preparation process of the KH-560 ethanol solution is as follows: KH-560 was mixed thoroughly in ethanol at a dosage ratio of 0.02–0.05 g / mL. Add acetic acid to it and adjust the pH to 4-5 to obtain KH-560 ethanol solution.

6. The epoxy adhesive for high-reliability IC packaging according to claim 2, characterized in that, The perfluorooctyltriethoxysilane ethanol solution is prepared by mixing and compounding perfluorooctyltriethoxysilane and ethanol at a mass ratio of 1:95-98.

7. The epoxy adhesive for high-reliability IC packaging according to claim 1, characterized in that, The defoamer is a compound of defoamer BYK-066N and defoamer BYK-1790 in a mass ratio of 1:10 to 12.

8. The epoxy adhesive for high-reliability IC packaging according to claim 1, characterized in that, The antioxidant is selected from any one of antioxidant 1010, antioxidant 1076, and antioxidant CA.

9. The preparation process of the high-reliability IC packaging epoxy adhesive according to any one of claims 1 to 8, characterized in that, Includes the following steps: Step 1: Accurately weigh the bisphenol F type epoxy resin, phenolic epoxy resin, synergist, methylhexahydrophthalic anhydride, 2-ethyl-4-methylimidazole, defoamer, and antioxidant, and set aside. Step 2: Preheat bisphenol F epoxy resin and phenolic epoxy resin separately at 50°C for 30 minutes. Then mix the preheated bisphenol F epoxy resin and phenolic epoxy resin, add synergistic additives, defoamers and antioxidants, and treat at 500-600 r / min for 10-15 minutes. Then add methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole and continue stirring for 12-15 minutes. Vacuum degassing and storage are then performed to prepare the high-reliability IC packaging epoxy adhesive product.

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