High-temperature-resistant epoxy resin pouring sealant for semiconductor packaging
Through the combination of hydrogen silicon addition technology and epoxy resin, a modified filler A was prepared and a high-temperature resistant epoxy resin potting was formed, which solved the problem of the degradation of the existing epoxy resin potting glue under high temperature conditions and achieved high temperature resistance of high Tg and Td.
Patent Information
- Application Number
- CN202411976347.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-11
- Estimated Expiration
- 2044-12-31
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of epoxy resin potting glue, and in particular relates to a high temperature resistant epoxy resin potting glue for semiconductor packaging. Background Art
[0002] In the semiconductor field, packaging technology plays a vital role in ensuring the performance and reliability of semiconductor devices. Among them, epoxy resin potting glue has been used as a common packaging material in semiconductor devices due to its excellent mechanical strength, bonding performance and other advantages. However, the existing epoxy resin potting glue still has certain disadvantages that limit its actual application effect. This is because most of the existing epoxy resin potting glues have limited high temperature resistance. In certain specific scenarios, such as packaging high-power semiconductors, welding, and aging testing after packaging, it is very easy to cause various performances to seriously degrade due to high temperature. Ultimately, it cannot play the role it should play. Summary of the invention
[0003] In view of the problems existing in the prior art, the purpose of the present invention is to provide a high-temperature resistant epoxy resin potting glue for semiconductor packaging. The present invention uses hydrogen-containing double heads and allyl glycidyl ether to prepare a compound with a silicon-hydrogen bond at one end and an epoxy group at the other end based on silicon hydroaddition, so that the compound continues to complete the grafting of epoxy groups on silicon dioxide modified with vinyltrimethoxysilane double bonds based on silicon hydroaddition, and then adds p-phenylenediamine to carry out epoxy-amino ring-opening bonding, construct a benzene ring structure and form terminal amino groups, and finally uses pentaerythritol glycidyl ether as a modifier to further carry out ring-opening bonding, that is, to prepare a modified filler A, which is mixed with epoxy resin as component A, and a curing agent, an accelerator and a filler B are mixed as component B, thereby obtaining a potting glue for semiconductor packaging, which not only has a high Tg temperature and a low linear expansion coefficient, but also a high Td temperature and excellent high temperature resistance.
[0004] The purpose of the present invention can be achieved through the following technical solutions:
[0005] A high temperature resistant epoxy resin potting glue for semiconductor packaging, comprising 100 parts by weight of component A and 30-35 parts by weight of component B; the component A is formed by mixing epoxy resin and modified filler A; the component B is formed by mixing a curing agent, an accelerator and filler B.
[0006] As a preferred technical solution of the present invention, the mass ratio of the epoxy resin to the modified filler A is 100:30-35; the mass ratio of the curing agent, the accelerator and the filler B is 100:0.5-1:10.
[0007] As a preferred technical solution of the present invention, the modified filler A is prepared by the following steps:
[0008] Step A: adding 6 parts by weight of a first platinum catalyst to 18-20 parts by weight of 1,1,3,3-tetramethyldisiloxane, and then adding dropwise 5 parts by weight of allyl glycidyl ether at 60-65° C. under a nitrogen atmosphere while stirring, and continuing to stir at a constant temperature for 6-8 hours after the addition is completed, filtering, removing the filter residue, and distilling to obtain a first component;
[0009] Step B: adding 2 parts by weight of double bond modified silica, 2-3 parts by weight of the first component and 0.2 parts by weight of the second platinum catalyst to 80 parts by weight of tetrahydrofuran, stirring at 60-70° C. for 8-10 hours under a nitrogen atmosphere, filtering, removing the filtrate, washing with toluene, and finally vacuum drying at 60-80° C. until constant weight, to obtain a second component;
[0010] Step C: adding 4 parts by weight of p-phenylenediamine to 80 parts by weight of dimethyl sulfoxide, stirring at 60-70° C. for 1 hour, keeping warm, then adding 2-3 parts by weight of the second component, continuing stirring for 8-10 hours, filtering, removing the filtrate, washing with deionized water, and finally vacuum drying at 60-80° C. until constant weight, to obtain a third component;
[0011] Step D: Add 6 parts by weight of pentaerythritol glycidyl ether to 80 parts by weight of dimethyl sulfoxide, and then stir at room temperature for 5-10 minutes to mix, then add 2-3 parts by weight of the third component, stir at 70-75°C for 8-10 hours, filter, remove the filtrate, wash with toluene, and finally vacuum dry at 50-70°C until constant weight, and the preparation is completed.
[0012] Furthermore, the dripping rate in step A is controlled at 1-2 drops / s.
[0013] Furthermore, the distillation in step A refers to distilling at 71° C. for 2 hours to remove volatiles.
[0014] Furthermore, the double bond modified silica in step B is prepared by the following steps:
[0015] Add 2 parts by weight of silicon dioxide, 1-1.5 parts by weight of vinyltrimethoxysilane and 0.1-0.3 parts by weight of deionized water to 80 parts by weight of anhydrous ethanol, then stir at 70°C for 12 hours, filter, remove the filtrate, wash with deionized water, and finally vacuum dry at 70°C until constant weight, and the preparation is completed.
[0016] As a preferred technical solution of the present invention, the curing agent is methylhexahydrophthalic anhydride.
[0017] As a preferred technical solution of the present invention, the accelerator is DMP-30 accelerator.
[0018] As a preferred technical solution of the present invention, the filler B is silicon dioxide or boron nitride.
[0019] A method for preparing a high temperature resistant epoxy resin potting compound for semiconductor packaging, the method comprising the following steps:
[0020] (1) Preparation of component A: Mix epoxy resin and modified filler A at room temperature at a speed of 100-400 rpm for 5-10 min, and seal and store;
[0021] (2) Preparation of component B: Stir the curing agent, accelerator and filler B at room temperature at a speed of 500 rpm for 5-10 min and store in a sealed container.
[0022] A method for using a high temperature resistant epoxy resin potting adhesive for semiconductor packaging, the method comprising the following steps:
[0023] Component A and component B were mixed at room temperature at a speed of 200-400 rpm for 5 minutes, vacuum degassed for 5 minutes, potted, and finally cured at 120-125°C for 2 hours.
[0024] Beneficial effects of the present invention:
[0025] (1) The present invention uses hydrogen-containing double caps and allyl glycidyl ether to prepare a compound with a silicon-hydrogen bond at one end and an epoxy group at the other end based on the silicon dioxide modified with the double bond of vinyltrimethoxysilane to continue to complete the grafting of the epoxy group based on the silicon-hydrogen bond, and then by adding p-phenylenediamine, the epoxy group-amino group is subjected to ring-opening bonding to construct a benzene ring structure and form an amino group at the end. Finally, pentaerythritol glycidyl ether is used as a modifier to further perform ring-opening bonding, that is, to prepare a modified filler A, which is mixed with an epoxy resin as component A, and a curing agent, an accelerator and a filler B as component B, thereby obtaining a potting glue for semiconductor packaging, which not only has a high Tg temperature and a low linear expansion coefficient, but also has a high Td temperature and excellent high temperature resistance.
[0026] (2) The present invention uses hydrogen-containing double caps (excessive amounts) and allyl glycidyl ether to prepare a compound with a silicon-hydrogen bond at one end and an epoxy group at the other end, based on the hydrosilylation reaction, so that the compound can be grafted with epoxy groups on the silicon dioxide modified with the double bonds of vinyltrimethoxysilane by the hydrosilylation reaction. On the one hand, the epoxy group can pave the way for the next technical improvement. On the other hand, the Si-O bond has a large bond energy, and its introduction can greatly promote thermal stability and increase the decomposition temperature, i.e., the Td temperature. However, since the Si-O bond itself also has a certain degree of flexibility, it can enhance the movement of the molecular chain in the polymer structure of the epoxy resin, resulting in a decrease in the glass transition temperature, i.e., the Tg temperature. Based on this, the addition of p-phenylenediamine (excessive amounts) The invention discloses a novel nanostructured filler A comprising a plurality of epoxy groups and a plurality of epoxy groups. The nanostructured filler A comprises a plurality of epoxy groups and a plurality of epoxy groups. The plurality of epoxy groups are used as the nanostructured filler A ...
[0027] (3) The present invention adds modified filler A to give the prepared potting glue for semiconductor packaging excellent high temperature resistance. Not only does it have a high Tg temperature and a low linear expansion coefficient, but it also has a high Td temperature, and is very practical. DETAILED DESCRIPTION
[0028] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the specific implementation methods, structures, features and effects of the present invention are described in detail below in combination with the embodiments.
[0029] The epoxy resins in all embodiments and comparative examples of the present invention were purchased from Wuxi Xinyehao Chemical Co., Ltd., model E-52 (618); the first platinum catalysts were purchased from Shaanxi Ruike New Materials Co., Ltd., product name platinum carbon; the second platinum catalysts were purchased from Suzhou Beiteli Polymer Materials Co., Ltd., product name platinum catalyst, model CSAT-F7xxxx.
[0030] All silicas are nano silicas with a particle size of 30 nm.
[0031] Example 1
[0032] A high temperature resistant epoxy resin potting glue for semiconductor packaging, comprising 100 parts by weight of component A and 30 parts by weight of component B; the component A is formed by mixing epoxy resin and modified filler A; the component B is formed by mixing a curing agent, an accelerator and filler B.
[0033] The mass ratio of the epoxy resin to the modified filler A is 100:30; the mass ratio of the curing agent, the accelerator and the filler B is 100:0.5:10.
[0034] The modified filler A is prepared by the following steps:
[0035] Step A: add 6 parts by weight of the first platinum catalyst to 18 parts by weight of 1,1,3,3-tetramethyldisiloxane, then dropwise add 5 parts by weight of allyl glycidyl ether at 60° C. under a nitrogen atmosphere while stirring, continue to stir at a constant temperature for 6 hours after the dropwise addition is completed, filter, remove the filter residue, and distill to obtain a first component;
[0036] Step B: adding 2 parts by weight of double-bond modified silica, 2 parts by weight of the first component and 0.2 parts by weight of the second platinum catalyst to 80 parts by weight of tetrahydrofuran, and then stirring at 60° C. for 8 hours under a nitrogen atmosphere, filtering, removing the filtrate, washing with toluene, and finally vacuum drying at 60° C. until constant weight, to obtain a second component;
[0037] Step C: adding 4 parts by weight of p-phenylenediamine to 80 parts by weight of dimethyl sulfoxide, stirring at 60° C. for 1 hour, keeping warm, then adding 2 parts by weight of the second component, stirring for 8 hours, filtering, removing the filtrate, washing with deionized water, and finally vacuum drying at 60° C. until constant weight, to obtain a third component;
[0038] Step D: Add 6 parts by weight of pentaerythritol glycidyl ether to 80 parts by weight of dimethyl sulfoxide, and then stir at room temperature for 5 minutes to mix, then add 2 parts by weight of the third component, stir at 70°C for 8 hours, filter, remove the filtrate, wash with toluene, and finally vacuum dry at 50°C until constant weight, and the preparation is completed.
[0039] The rate of dripping in step A is controlled at 1 drop / s.
[0040] The distillation in step A refers to distilling at 71° C. for 2 hours to remove volatiles.
[0041] The double bond modified silica in step B is prepared by the following steps:
[0042] Add 2 parts by weight of silicon dioxide, 1 part by weight of vinyltrimethoxysilane and 0.1 parts by weight of deionized water to 80 parts by weight of anhydrous ethanol, then stir at 70°C for 12 hours, filter, remove the filtrate, wash with deionized water, and finally vacuum dry at 70°C until constant weight, and the preparation is completed.
[0043] The curing agent is methyl hexahydrophthalic anhydride.
[0044] The accelerator is DMP-30 accelerator.
[0045] The filler B is silicon dioxide.
[0046] A method for preparing a high temperature resistant epoxy resin potting compound for semiconductor packaging, the method comprising the following steps:
[0047] (1) Preparation of component A: Mix epoxy resin and modified filler A at room temperature at a speed of 100 rpm for 5 min and seal for storage;
[0048] (2) Preparation of component B: Stir the curing agent, accelerator and filler B at room temperature at a speed of 500 rpm for 5 min and store in a sealed container.
[0049] A method for using a high temperature resistant epoxy resin potting adhesive for semiconductor packaging, the method comprising the following steps:
[0050] Component A and component B were mixed at room temperature at a speed of 200 rpm for 5 minutes, vacuum degassed for 5 minutes, potted, and finally cured at 120°C for 2 hours.
[0051] Example 2
[0052] A high temperature resistant epoxy resin potting glue for semiconductor packaging, comprising 100 parts by weight of component A and 35 parts by weight of component B; the component A is formed by mixing epoxy resin and modified filler A; the component B is formed by mixing a curing agent, an accelerator and filler B.
[0053] The mass ratio of the epoxy resin to the modified filler A is 100:35; the mass ratio of the curing agent, the accelerator and the filler B is 100:1:10.
[0054] The modified filler A is prepared by the following steps:
[0055] Step A: add 6 parts by weight of the first platinum catalyst to 20 parts by weight of 1,1,3,3-tetramethyldisiloxane, then dropwise add 5 parts by weight of allyl glycidyl ether at 65° C. under a nitrogen atmosphere while stirring, continue to stir at a constant temperature for 8 hours after the dropwise addition is completed, filter, remove the filter residue, and distill to obtain a first component;
[0056] Step B: adding 2 parts by weight of double-bond modified silica, 3 parts by weight of the first component and 0.2 parts by weight of the second platinum catalyst to 80 parts by weight of tetrahydrofuran, and then stirring at 70° C. for 10 hours under a nitrogen atmosphere, filtering, removing the filtrate, washing with toluene, and finally vacuum drying at 80° C. until constant weight, to obtain a second component;
[0057] Step C: adding 4 parts by weight of p-phenylenediamine to 80 parts by weight of dimethyl sulfoxide, stirring at 70° C. for 1 hour, keeping warm, then adding 3 parts by weight of the second component, stirring for 10 hours, filtering, removing the filtrate, washing with deionized water, and finally vacuum drying at 80° C. until constant weight, to obtain a third component;
[0058] Step D: Add 6 parts by weight of pentaerythritol glycidyl ether to 80 parts by weight of dimethyl sulfoxide, and then stir and mix at room temperature for 10 minutes, then add 3 parts by weight of the third component, stir at 75°C for 10 hours, filter, remove the filtrate, wash with toluene, and finally vacuum dry at 70°C until constant weight, and the preparation is completed.
[0059] The rate of dripping in step A is controlled at 2 drops / s.
[0060] The distillation in step A refers to distilling at 71° C. for 2 hours to remove volatiles.
[0061] The double bond modified silica in step B is prepared by the following steps:
[0062] Add 2 parts by weight of silicon dioxide, 1.5 parts by weight of vinyltrimethoxysilane and 0.3 parts by weight of deionized water to 80 parts by weight of anhydrous ethanol, then stir at 70°C for 12 hours, filter, remove the filtrate, wash with deionized water, and finally vacuum dry at 70°C until constant weight, and the preparation is completed.
[0063] The curing agent is methyl hexahydrophthalic anhydride.
[0064] The accelerator is DMP-30 accelerator.
[0065] The filler B is silicon dioxide.
[0066] A method for preparing a high temperature resistant epoxy resin potting compound for semiconductor packaging, the method comprising the following steps:
[0067] (1) Preparation of component A: Mix epoxy resin and modified filler A at room temperature at a speed of 400 rpm for 10 min and seal for storage;
[0068] (2) Preparation of component B: Stir the curing agent, accelerator and filler B at room temperature at a speed of 500 rpm for 10 min and store in a sealed container.
[0069] A method for using a high temperature resistant epoxy resin potting adhesive for semiconductor packaging, the method comprising the following steps:
[0070] Component A and component B were mixed at room temperature at a rotation speed of 400 rpm for 5 minutes, vacuum degassed for 5 minutes, potted, and finally cured at 125°C for 2 hours.
[0071] Example 3
[0072] A high temperature resistant epoxy resin potting glue for semiconductor packaging, comprising 100 parts by weight of component A and 32 parts by weight of component B; the component A is formed by mixing epoxy resin and modified filler A; the component B is formed by mixing a curing agent, an accelerator and filler B.
[0073] The mass ratio of the epoxy resin to the modified filler A is 100:33; the mass ratio of the curing agent, the accelerator and the filler B is 100:0.8:10.
[0074] The modified filler A is prepared by the following steps:
[0075] Step A: add 6 parts by weight of the first platinum catalyst to 19 parts by weight of 1,1,3,3-tetramethyldisiloxane, then dropwise add 5 parts by weight of allyl glycidyl ether at 63° C. under a nitrogen atmosphere while stirring, continue to stir at a constant temperature for 7 hours after the dropwise addition is completed, filter, remove the filter residue, and distill to obtain a first component;
[0076] Step B: Add 2 parts by weight of double-bond modified silica, 2.5 parts by weight of the first component and 0.2 parts by weight of the second platinum catalyst to 80 parts by weight of tetrahydrofuran, then stir at 65° C. for 9 hours under a nitrogen atmosphere, filter, remove the filtrate, wash with toluene, and finally vacuum dry at 70° C. until constant weight to obtain a second component;
[0077] Step C: Add 4 parts by weight of p-phenylenediamine to 80 parts by weight of dimethyl sulfoxide, then stir at 65° C. for 1 hour, keep warm, then add 2.5 parts by weight of the second component, continue stirring for 9 hours, filter, remove the filtrate, wash with deionized water, and finally vacuum dry at 70° C. until constant weight, to obtain a third component;
[0078] Step D: Add 6 parts by weight of pentaerythritol glycidyl ether to 80 parts by weight of dimethyl sulfoxide, and then stir at room temperature for 8 minutes, then add 2.5 parts by weight of the third component, stir at 73°C for 9 hours, filter, remove the filtrate, wash with toluene, and finally vacuum dry at 60°C until constant weight, and the preparation is completed.
[0079] The rate of the dripping in step A is controlled at 1.5 drops / s.
[0080] The distillation in step A refers to distilling at 71° C. for 2 hours to remove volatiles.
[0081] The double bond modified silica in step B is prepared by the following steps:
[0082] Add 2 parts by weight of silicon dioxide, 1.3 parts by weight of vinyltrimethoxysilane and 0.2 parts by weight of deionized water to 80 parts by weight of anhydrous ethanol, then stir at 70°C for 12 hours, filter, remove the filtrate, wash with deionized water, and finally vacuum dry at 70°C until constant weight, and the preparation is completed.
[0083] The curing agent is methyl hexahydrophthalic anhydride.
[0084] The accelerator is DMP-30 accelerator.
[0085] The filler B is silicon dioxide.
[0086] A method for preparing a high temperature resistant epoxy resin potting compound for semiconductor packaging, the method comprising the following steps:
[0087] (1) Preparation of component A: Mix epoxy resin and modified filler A at room temperature at a speed of 200 rpm for 8 min and seal for storage;
[0088] (2) Preparation of component B: Stir the curing agent, accelerator and filler B at room temperature at a speed of 500 rpm for 8 min and store in a sealed container.
[0089] A method for using a high temperature resistant epoxy resin potting adhesive for semiconductor packaging, the method comprising the following steps:
[0090] Component A and component B were mixed at room temperature at a rotation speed of 300 rpm for 5 minutes, vacuum degassed for 5 minutes, potted, and finally cured at 123°C for 2 hours.
[0091] Comparative Example 1
[0092] Based on Example 3, pentaerythritol glycidyl ether in step D was replaced with trimethylolpropane triglycidyl ether of equal weight, and the rest remained unchanged.
[0093] Comparative Example 2
[0094] Based on Example 3, the p-phenylenediamine in step C was replaced with ethylenediamine of equal weight, and the rest remained unchanged.
[0095] Comparative Example 3
[0096] On the basis of Example 3, step A is omitted, and step B is changed to adding 2 parts by weight of silicon dioxide and 1.3 parts by weight of 3-glycidyloxypropyltrimethoxysilane to 80 parts by weight of toluene, followed by stirring at 70°C for 12 hours, filtering, removing the filtrate, washing with acetone, and finally vacuum drying at 70°C until constant weight to obtain the second component; the rest remain unchanged.
[0097] Comparative Example 4
[0098] Based on Example 3, step C and step D are not performed, and the rest remain unchanged.
[0099] Comparative Example 5
[0100] On the basis of Example 3, the modified filler A was replaced with an equal weight of silicon dioxide, and the rest remained unchanged.
[0101] Test Example 1
[0102] High temperature resistance test:
[0103] The high temperature resistant epoxy resin potting glue prepared in Example 3 and Comparative Examples 1-5 were respectively made into test pieces (component A and component B were stirred and mixed at a speed of 400 rpm at room temperature for 5 min, vacuum degassed for 5 min, and finally cured at 125° C. for 2 h to obtain the test pieces);
[0104] The Tg temperature of the above sample was tested by differential thermal analyzer (nitrogen atmosphere throughout the process, first heated to 250°C at a heating rate of 30°C / min, kept at a constant temperature for 5 minutes, then cooled to 30°C at a cooling rate of 10°C / min, and finally heated to 250°C at a heating rate of 10°C / min. The test was performed during the second heating, and the integer was rounded off);
[0105] The Td temperature of the above sample was tested by a thermogravimetric analyzer (nitrogen atmosphere throughout the process, the heating rate was controlled at 5°C / min, and the temperature at which the mass loss reached 5% was recorded as the Td temperature, rounded to the nearest integer).
[0106] Table 1. High temperature resistance test results
[0107] Tg temperature / ℃ Td temperature / ℃ Example 3 213 430 Comparative Example 1 202 423 Comparative Example 2 160 425 Comparative Example 3 214 413 Comparative Example 4 137 416 Comparative Example 5 141 403
[0108] Comparison between Example 3 and Comparative Examples 1-5 shows that:
[0109] The difference between Comparative Example 1 and Example 3 is that pentaerythritol glycidyl ether is replaced by trimethylolpropane triglycidyl ether of equal weight, that is, the number of chemical crosslinking points is reduced, thereby lowering the crosslinking density.
[0110] The difference between Comparative Example 2 and Example 3 is that p-phenylenediamine is replaced by ethylenediamine of equal weight, that is, no benzene ring structure is constructed, and no spatial constraint effect is achieved.
[0111] The difference between Comparative Example 3 and Example 3 is that no Si-O-Si segment is introduced.
[0112] The difference between Comparative Example 4 and Example 3 is that step C and step D are not performed.
[0113] The difference between Comparative Example 5 and Example 3 is that the modified filler A is replaced by an equal weight of silicon dioxide.
[0114] From Test Example 1, it can be seen from the comparison between Example 3 and Comparative Examples 1-5 that the high temperature resistant epoxy resin potting glue prepared by the present invention has both high Tg temperature and Td temperature, and the high temperature resistance performance is very excellent; although the Tg temperature of Comparative Example 3 is slightly higher than that of the present invention, it is not significant, which indirectly indicates that the presence or absence of the Si-O-Si segment has a very small effect on the Tg temperature at this time.
[0115] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A high temperature resistant epoxy resin potting compound for semiconductor packaging, characterized in that: The high temperature resistant epoxy resin potting glue comprises 100 parts by weight of component A and 30-35 parts by weight of component B; the component A is formed by mixing epoxy resin and modified filler A; the component B is formed by mixing a curing agent, an accelerator and filler B.
2. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 1, characterized in that: The mass ratio of the epoxy resin to the modified filler A is 100:30-35; the mass ratio of the curing agent, the accelerator and the filler B is 100:0.5-1:
10.
3. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 1, characterized in that: The modified filler A is prepared by the following steps: Step A: adding 6 parts by weight of a first platinum catalyst to 18-20 parts by weight of 1,1,3,3-tetramethyldisiloxane, and then adding dropwise 5 parts by weight of allyl glycidyl ether at 60-65° C. under a nitrogen atmosphere while stirring, and continuing to stir at a constant temperature for 6-8 hours after the addition is completed, filtering, removing the filter residue, and distilling to obtain a first component; Step B: adding 2 parts by weight of double bond modified silica, 2-3 parts by weight of the first component and 0.2 parts by weight of the second platinum catalyst to 80 parts by weight of tetrahydrofuran, stirring at 60-70° C. for 8-10 hours under a nitrogen atmosphere, filtering, removing the filtrate, washing with toluene, and finally vacuum drying at 60-80° C. until constant weight, to obtain a second component; Step C: adding 4 parts by weight of p-phenylenediamine to 80 parts by weight of dimethyl sulfoxide, stirring at 60-70° C. for 1 hour, keeping warm, then adding 2-3 parts by weight of the second component, continuing stirring for 8-10 hours, filtering, removing the filtrate, washing with deionized water, and finally vacuum drying at 60-80° C. until constant weight, to obtain a third component; Step D: Add 6 parts by weight of pentaerythritol glycidyl ether to 80 parts by weight of dimethyl sulfoxide, and then stir at room temperature for 5-10 minutes to mix, then add 2-3 parts by weight of the third component, stir at 70-75°C for 8-10 hours, filter, remove the filtrate, wash with toluene, and finally vacuum dry at 50-70°C until constant weight, and the preparation is completed.
4. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 3, characterized in that: The dripping rate in step A is controlled at 1-2 drops / s.
5. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 3, characterized in that: The distillation in step A refers to distilling at 71° C. for 2 hours to remove volatiles.
6. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 3, characterized in that: The double bond modified silica in step B is prepared by the following steps: Add 2 parts by weight of silicon dioxide, 1-1.5 parts by weight of vinyltrimethoxysilane and 0.1-0.3 parts by weight of deionized water to 80 parts by weight of anhydrous ethanol, then stir at 70°C for 12 hours, filter, remove the filtrate, wash with deionized water, and finally vacuum dry at 70°C until constant weight, and the preparation is completed.
7. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 1, characterized in that: The curing agent is methyl hexahydrophthalic anhydride.
8. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 1, characterized in that: The accelerator is DMP-30 accelerator.
9. The high temperature resistant epoxy resin potting adhesive for semiconductor packaging according to claim 1, characterized in that: The filler B is silicon dioxide or boron nitride.
Citation Information
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