Epoxy adhesive for semiconductor cutting and splicing rods and preparation method thereof
Through the combination of POSS-epoxy cage polysilsesquioxane and phenolic epoxy, the problem of insufficient hardness and temperature resistance of the existing stick glue during the cutting process is solved, high glass transition temperature and low water absorption rate are achieved, and the stability and yield of the cutting process are improved.
Patent Information
- Application Number
- CN202411879929.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-19
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2044-12-19
AI Technical Summary
The existing stick glue has low glass transition temperature and poor temperature resistance during the cutting process, resulting in a rapid decrease in hardness and strength when the temperature changes, making it difficult to meet the requirements of semiconductor cutting.
The combination of POSS-epoxy cage polysilsesquioxane, phenolic epoxy and modified amine curing agent is used to form components A and B, and the hardness, temperature resistance and bonding strength of the colloid are improved by mixing and use.
The glass transition temperature of the colloid is increased, compatibility with semiconductor materials is enhanced, water absorption is reduced, hardness stability during cutting process is ensured, and cutting yield is improved.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of epoxy adhesives, in particular to an epoxy adhesive for semiconductor cutting and splicing bars and a preparation method thereof. Background Art
[0002] In the field of semiconductor silicon carbide / silicon wafer cutting, since the semiconductor crystal pulling and growth process is relatively long and silicon carbide semiconductors are difficult to grow into large single rods, in order to ensure batch quality and uniformity of each cutting, silicon carbide semiconductor rods of different lengths are generally spliced together according to the crystal orientation and then cut simultaneously.
[0003] Existing adhesives for photovoltaic-grade monocrystalline and multicrystalline silicon ingots are primarily used for cutting. They include epoxy-modified amine adhesives, unsaturated bisphenol A acrylate adhesives, and inorganic adhesives based on oxides (copper, iron, yttrium, and lanthanum), with epoxy-modified amine adhesives being the most common. However, epoxy-modified amine adhesives, such as epoxy ingot adhesives, have significant limitations. Compared to silicon wafers, third-generation semiconductor silicon carbide has a higher hardness (9.2 on the Mohs scale) and is generally more brittle. While traditional photovoltaic-grade epoxy ingot adhesives are brittle at room temperature, they also have a low glass transition temperature and poor heat resistance. Their strength and hardness decrease rapidly during the cutting process, particularly as temperature and water absorption fluctuate. Unsaturated bisphenol A acrylate adhesives, due to oxygen inhibition during the curing process, react with oxygen at the bonding interface, making the adhesive difficult to cure and becoming very sticky. This can cause diamond wire to adhere to the adhesive, reducing cutting force. Furthermore, the adhesives produce a strong odor and generate significant heat during use, posing safety risks. Oxide inorganic glue usually needs to be heated and cured, which is quite different from the on-site construction process. In addition, the residual metal ions are difficult to remove, affecting the quality of the semiconductor.
[0004] In-depth research and exploration has been conducted domestically in the field of semiconductor silicon rod splicing adhesives. For example, CN118064089A discloses improving the cutting performance of splicing adhesives by increasing the hardness and brittleness of the adhesive at room temperature. However, the glass transition temperature of a common mercaptan curing agent (DMP-3-800LC) is only 35°C, and that of a modified amine is only 65°C, making it difficult to guarantee deformation caused by temperature fluctuations during cutting. CN115651580B discloses increasing the hardness of the adhesive by adding monomeric metallic silicon powder and increasing the density of the adhesive by adding a large amount of filler. However, the temperature resistance of common mercaptan curing agents is still insufficient to meet the high temperatures encountered during cutting. Moreover, increasing the filler content to 81% in the adhesive makes it difficult to achieve fluidity at room temperature, which inevitably increases the cavitation rate of the adhesive and significantly increases the wire breakage rate during cutting. CN117247756B discloses improving the temperature resistance by adding phenalkamine and a tetrafunctional mercaptan curing agent. However, due to the limitation of the glass transition temperature of the phenalkamine curing agent, the temperature resistance of the glue stick still fails to meet the hardness requirement at the cutting temperature. Summary of the Invention
[0005] The technical problem to be solved by the present invention is to improve the glass transition temperature, hardness and temperature resistance of semiconductor stick glue based on the deficiencies in the prior art.
[0006] In order to solve the above problems, the present invention proposes the following technical solutions:
[0007] In a first aspect, the present invention provides an epoxy adhesive for semiconductor dicing and splicing bars, comprising component A and component B;
[0008] In parts by weight, the component A comprises the following ingredients:
[0009] POSS-epoxy caged polysilsesquioxane 17-25 parts by weight;
[0010] 8-15 parts by weight of novolac epoxy;
[0011] 58-72 parts by weight of the first filler;
[0012] 2-5 parts by weight of the first auxiliary agent;
[0013] The B component includes the following ingredients in parts by weight:
[0014] POSS-mercapto caged polysilsesquioxane 17-23 parts by weight;
[0015] 5-10 parts by weight of modified amine curing agent;
[0016] 3-5 parts by weight of accelerator;
[0017] 60-70 parts by weight of the second filler;
[0018] 2-3 parts by weight of the second auxiliary agent.
[0019] A further technical solution is that the POSS-epoxy caged polysilsesquioxane includes at least one of octaglycidyl ether POSS-glycidyl ether oxygen propyl caged polysilsesquioxane, alicyclic epoxy POSS-octaepoxycyclohexylethyl caged polysilsesquioxane, and glycidyl ether oxygen propyl cyclotetrasiloxane.
[0020] A further technical solution is that the POSS-epoxy caged polysilsesquioxane is octaglycidyl ether POSS-glycidyl ether oxygen propyl caged polysilsesquioxane.
[0021] A further technical solution is that the novolac epoxy includes at least one of EPICLON HP-4710 (ultra-high heat-resistant epoxy resin), novolac epoxy with a DCPD structure (diethylcyclopentadiene novolac epoxy), and NPPN-638 novolac epoxy.
[0022] A further technical solution is that the general formula of the POSS-mercapto caged polysilsesquioxane is (RSiO3 / 2)n, R is mercaptopropionate, and n=8.
[0023] A further technical solution is that the modified amine curing agent is obtained by condensing 3,3-dimethyl-4,4-diaminodicyclohexylmethane and thiourea.
[0024] A further technical solution is that the first filler and the second filler are independently selected from at least one of spherical silica, spherical alumina, and spherical silicon carbide, all of which have low linear expansion coefficients. It is understood that spherical silica, spherical alumina, and spherical silicon carbide are all spherical fillers with low linear expansion coefficients, which help reduce shrinkage after curing and ensure the firmness of the bonding interface.
[0025] A further technical solution is that the spherical silica includes spherical silica with a particle size of 3-8 μm, spherical silica with a particle size of 0.11-1.5 μm, and spherical silica with a particle size of 0.01-0.10 μm, and the usage ratio of the three particle sizes is 9-11:1-3:2-0.5;
[0026] The spherical alumina includes spherical alumina with a particle size of 1-5 μm, spherical alumina with a particle size of 0.2-0.8 μm, and spherical alumina with a particle size of 0.01-0.10 μm, and the usage ratio of the three particle sizes is 7-9:1-3:2-0.5;
[0027] The spherical silicon carbide includes spherical silicon carbide with a particle size of 5-10 μm, spherical silicon carbide with a particle size of 0.8-3 μm, and spherical silicon carbide with a particle size of 0.01-0.10 μm. The usage ratio of the three particle sizes is 6-8:1-3:2-0.5.
[0028] A further technical solution is that, in the first filler and the second filler, the usage ratio of low linear expansion coefficient spherical silica, spherical alumina and spherical silicon carbide is 1-3:2-4:4-6.
[0029] A further technical solution is that the accelerator includes at least one of Versamine EH-50, ACC 2950 (N,N-dimethyl-4-amino-2-azabutyl) phenol, and HI-54K.
[0030] A further technical solution is that the first auxiliary agent and the second auxiliary agent independently include at least one of a defoaming agent, a leveling agent and a dispersant.
[0031] A further technical solution is that the defoaming agent in the first auxiliary agent is selected from ShinEtsu KS-603, the leveling agent is selected from BYK-310, and the dispersant is selected from BYK Disperbyk-2150.
[0032] A further technical solution is that the defoamer in the second additive is selected from BYK019, the leveling agent is selected from BASF-EFKA3600, and the dispersant is selected from TIGO-Dispers 655.
[0033] A further technical solution is that the mass ratio of component A to component B is 1:0.9-1.1, preferably 1:1. Component A and component B are prepared and stored separately, and then mixed before use.
[0034] In a second aspect, the present invention further provides a method for preparing the epoxy adhesive for semiconductor cutting and splicing bars according to the first aspect, comprising the following steps:
[0035] POSS-epoxy caged polysilsesquioxane, phenolic epoxy, a first filler and a first auxiliary agent are mixed and dispersed to prepare component A;
[0036] POSS-mercapto caged polysilsesquioxane, modified amine curing agent, accelerator, second filler and second auxiliary agent are mixed and dispersed to prepare component B;
[0037] Mix component A and component B in proportion and use immediately.
[0038] Compared with the prior art, the present invention can achieve the following technical effects:
[0039] The epoxy adhesive for semiconductor cutting splicing rods provided by the present invention has a synergistic effect between the components under the compounding of component A (mainly comprising POSS-epoxy, phenolic epoxy) and component B (mainly comprising POSS-thiol curing agent, modified amine curing agent). After curing, the obtained colloid is similar to the structure of semiconductor silicon wafers or silicon carbide, and the hardness and strength are close to the hardness, strength and crystal properties of semiconductor materials, which helps to improve the compatibility of epoxy adhesive with semiconductor materials. The POSS structure is an inorganic core composed of a silicon-oxygen skeleton alternately connected by Si-O, which is similar to the skeleton of semiconductor silicon wafers or silicon carbide. It is supplemented by phenolic epoxy and modified amine curing agents and has good curing speed, viscosity and low water absorption. The use of fillers with low linear expansion coefficients can better fill the bonding interface and reduce volume change. In addition, the epoxy adhesive of the present invention has a higher glass transition temperature after curing, can withstand temperature changes during the cutting process, and the hardness is little affected by temperature and remains almost unchanged, which can enable semiconductor materials to pass through tungsten steel wire more smoothly, reduce wire bow, and improve cutting yield. DETAILED DESCRIPTION
[0040] The technical solutions in the embodiments are described clearly and completely below. Obviously, the embodiments described below are only some of the embodiments of the present invention, not all of them. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without creative effort are also within the scope of protection of the present invention.
[0041] It will be understood that when used in this specification and the appended claims, the terms “comprises” and “comprising” indicate the presence of described features, integers, steps, operations, elements and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or groups thereof.
[0042] It should also be understood that the terms used in this description of the embodiments of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the embodiments of the present invention. As used in the description of the embodiments of the present invention and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms unless the context clearly indicates otherwise.
[0043] An embodiment of the present invention provides an epoxy adhesive for semiconductor cutting and splicing rods, comprising component A and component B;
[0044] In parts by weight, the component A comprises the following ingredients:
[0045] POSS-epoxy caged polysilsesquioxane 17-25 parts by weight;
[0046] 8-15 parts by weight of novolac epoxy;
[0047] 58-72 parts by weight of the first filler;
[0048] 2-5 parts by weight of the first auxiliary agent;
[0049] The B component includes the following ingredients in parts by weight:
[0050] POSS-mercapto caged polysilsesquioxane 17-23 parts by weight;
[0051] 5-10 parts by weight of modified amine curing agent;
[0052] 3-5 parts by weight of accelerator;
[0053] 60-70 parts by weight of the second filler;
[0054] 2-3 parts by weight of the second auxiliary agent.
[0055] The following is an introduction to each ingredient:
[0056] The POSS-epoxy caged polysilsesquioxane of the present invention includes at least one of octaglycidyl ether POSS-glycidyl ether oxygen propyl caged polysilsesquioxane (such as structural formula 1), alicyclic epoxy POSS-octaepoxycyclohexylethyl caged polysilsesquioxane (such as structural formula 2), and glycidyl ether oxygen propyl cyclotetrasiloxane.
[0057] Structural formula 1, Structural formula 2, R=CH2CH2CH2OCH2(CHCH2O).
[0058] The POSS-epoxy caged polysilsesquioxane used in the embodiment of the present invention is octaglycidyl ether POSS-glycidyl ether oxygen propyl caged polysilsesquioxane.
[0059] The epoxy novolac resin of the present invention comprises at least one of EPICLON HP-4710 (ultra-high heat-resistant epoxy resin, such as structural formula 3), epoxy novolac resin having a DCPD structure (diethylcyclopentadiene epoxy novolac resin, such as structural formula 4), and NPPN-638 epoxy novolac resin.
[0060] Structural formula 3, Structural formula 4, R = glycidyl ether, n = 1-2.
[0061] The epoxy novolac used in the embodiment of the present invention is a combination of EPICLON HP-4710 and diethylcyclopentadiene novolac epoxy DCPD, and the usage ratio of the two is 1:2.
[0062] The first filler used in the embodiment of the present invention is a combination of spherical silica, spherical alumina, and spherical silicon carbide with a low linear expansion coefficient, with the three used in a ratio of 2:3:5. The spherical silica is a combination of 5μm spherical silica, 0.5μm spherical silica, and 0.05μm spherical silica in a ratio of 10:2:1; the spherical alumina is a combination of 3μm spherical alumina, 0.5μm spherical alumina, and 0.03μm spherical alumina in a ratio of 8:2:1; and the spherical silicon carbide is a combination of 8μm spherical silicon carbide, 1μm spherical silicon carbide, and 0.05μm spherical silicon carbide in a ratio of 7:2:1.
[0063] The first auxiliary agent used in the embodiment of the present invention is a combination of ShinEtsu KS-603 defoamer, BYK-310 leveling agent, and Disperbyk-2150 dispersant, wherein the ratio of defoamer:leveling agent:dispersant is 6:2:2.
[0064] The POSS-mercapto caged polysilsesquioxane used in the embodiment of the present invention is shown in structural formula 5:
[0065] Structural formula 5, R = mercaptopropionate.
[0066] The modified amine curing agent used in the present invention is obtained by condensation reaction of 3,3-dimethyl-4,4-diaminodicyclohexylmethane (DMDC) and thiourea. The specific preparation process is as follows:
[0067] 490 g of 3,3'-dimethyl-4,4-diaminodicyclohexylmethane was added to the reactor, the stirring motor was turned on, and the temperature was raised and stirred until the temperature reached 95°C. Then 76 g of thiourea was added to the reactor, and the mixture was stirred and heated to 150°C under nitrogen atmosphere. The generation of gas was observed during the reaction, and then heating was continued for 3 hours. The temperature was raised to 170°C, vacuum was turned on and continued for 60 minutes, and then the temperature was lowered and the material was discharged to obtain a high Tg modified amine curing agent that can be cured quickly.
[0068] The accelerator used in the embodiment of the present invention is a combination of Versamine EH-50, 2.4.6-tri(N,N-dimethyl-4-amino-2-azabutyl)phenol (ACC 2950), and HI-54K, with the usage ratio of EH-50: 2950: HI-54K being 2: 3: 5.
[0069] The composition of the second filler used in the embodiment of the present invention is the same as that of the first filler.
[0070] The second additive used in the embodiment of the present invention is a combination of defoamer BYK019, leveling agent BASF-EFKA3600, and dispersant TIGO-Dispers 655. The ratio of defoamer: leveling agent: dispersant is 6:2:2.
[0071] The embodiment of the present invention also provides a method for preparing the epoxy adhesive for semiconductor cutting and splicing rods, comprising the following steps:
[0072] Preparation of component A: POSS-epoxy caged polysilsesquioxane, phenolic epoxy, the first filler, and the first auxiliary agent were placed into a 2 L planetary mixer according to the formula. The temperature was raised to 45°C within 30 minutes. The mixture was vacuumed and stirred for 2 hours (speed 100 rmp / min, dispersion speed 800 rmp / min). After cooling to room temperature, the mixture was discharged and sealed with nitrogen to obtain component A.
[0073] Preparation of component B: POSS-mercapto caged polysilsesquioxane, modified amine curing agent, accelerator, second filler, and second auxiliary agent were placed into a 2 L planetary power mixer according to the formula. The temperature was raised to 45°C within 30 minutes. Vacuum was turned on and stirred for 2 hours (speed 100 rmp / min, dispersion speed 800 rmp / min). After cooling to room temperature, the material was discharged and sealed with nitrogen to obtain component B.
[0074] The above-mentioned component A and component B are prepared and stored separately, and then mixed at a mass ratio of 1:1 before use, and are ready for use.
[0075] According to the ratios shown in Tables 1 and 2 below, the above method was used to prepare component A and component B of each example. Table 1 shows the composition and amount of component A of each example, and Table 2 shows the composition and amount of component B of each example.
[0076] Table 1 Composition and dosage of component A in each embodiment
[0077]
[0078] It should be noted that in Comparative Example A5, only POSS-epoxy was replaced by tetrafunctional glycidylamine (AG-80H), and the remaining components were the same as in Example; in Comparative Example A6, only phenolic epoxy was replaced by triglycidyl p-aminophenol (AFG-90), and the remaining components were the same as in Example.
[0079] Table 2 Composition and dosage of component B in each example
[0080]
[0081] It should be noted that in Comparative Example B5, only the POSS-mercapto group was replaced by dipentaerythritol hexa(3-mercaptopropionate), and the remaining ingredients were the same as in Example 1; in Comparative Example B6, only the modified amine curing agent was Huntsman Capcure 3-800, and the remaining ingredients were the same as in Example 1.
[0082] The component A and the component B of each of the above embodiments were combined at a mass ratio of 1:1 as shown in Table 3 below to prepare epoxy adhesives for semiconductor dicing rods of different embodiments.
[0083] Table 3 Composition of the epoxy adhesive for semiconductor cutting rods in Examples 1-8
[0084] composition Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Component A Example A1 Example A2 Example A3 Example A4 Comparative Example A5 Comparative Example A6 Comparative Example A5 Example A2 Component B Example B1 Example B2 Example B3 Example B4 Comparative Example B5 Comparative Example B6 Example B3 Comparative Example B6
[0085] The performance tests of the following test items were conducted on the epoxy adhesive for semiconductor dicing splicing bars obtained in Examples 1-8 above (hereinafter referred to as "splicing bar adhesive") and two commercially available splicing bar adhesives:
[0086] Shore D hardness tester (Shore D): Prepare the rubber into round blocks with a diameter of 6-8mm and a weight of 15-25g. Test the Shore D hardness of each round block according to the national standard GB / T2411-2008. Test in a 100°C oven. Quickly test the hardness of 5 points and take the average value.
[0087] Water Absorption Test: After the hardness test, return the round rubber blocks to room temperature and immerse them in 25°C water. After 24 hours, measure the weight change of the blocks. Take five samples from each group and calculate the average value. Low water absorption effectively prevents moisture from entering the colloid during the cutting process, thereby lowering the glass transition temperature of the colloid.
[0088] Glass Transition Temperature (Tg) Test: Each rubber compound is tested using TMA according to GB / T 19466.2. A higher Tg value indicates a higher temperature at which the material transitions from the glassy state to the rubbery state, indicating better temperature resistance.
[0089] Impact toughness (SM) testing: Each rubber component is tested using the standard method of GB / T 1843-2008. Impact toughness represents the mechanical strength of a material during an impact, and can be expressed as the material's toughness. The smaller the value, the greater the brittleness of the material.
[0090] Coefficient of Linear Expansion (CTE): Tested in accordance with GB / T1036-2008, "Test Method for Coefficient of Linear Expansion of New Materials," the linear expansion coefficients of each adhesive are measured below and above its Tg. A low linear expansion coefficient prevents thermal stress from occurring during the cutting process, potentially damaging the semiconductor material.
[0091] Cutting yield test: Silicon carbide ingots were spliced using various examples and commercially available splicing glue. The spliced ingots were then diamond wire cut using 30 cutters. The tungsten diamond wire was used at a speed of 25 m / s, a wire diameter of 35 μm, and a wire mesh spacing of 330 μm. Cutting defects were classified as line marks and fragments on the silicon carbide wafers, and the cutting yield was calculated. Yield = number of qualified wafers / total number of wafers cut.
[0092] Commercially available 1 is Prober / A-8860 stick glue, and commercially available 2 is SK / R-677 stick glue.
[0093] The test results of the above test items are shown in Table 4.
[0094] Table 4 Test results
[0095]
[0096] According to the test results in Table 4, the glue sticks provided by the embodiments of the present invention (Examples 1-4), when compounded with component A and component B containing specific ingredients, the obtained cured products show good performance in hardness, Tg, temperature resistance and other aspects, and can meet the requirements of semiconductor cutting: it has a water absorption rate of less than 0.3%, which can effectively prevent water vapor from entering during the cutting process; the Shore hardness is as high as 97HD, which is similar to the hardness of semiconductor materials, and the lower impact toughness indicates that the colloid is brittle after curing, which is close to the crystal properties of semiconductor materials; and the glass transition temperature is above 130°C, which can withstand the temperature of the cutting front end (50-100°C). At the same time, the linear expansion coefficient at Tg and the linear expansion coefficient on Tg are much lower than those of Examples 5-8 and two commercially available glue sticks, and it has the advantage of good temperature resistance.
[0097] Compared with Examples 1-4, the glue stick of Example 5 uses a combination of tetrafunctional glycidylamine (AG-80H) and phenolic epoxy in component A, and a combination of dipentaerythritol hexa(3-mercaptopropionic acid) ester and a modified amine curing agent in component B. It does not contain a POSS skeleton structure. Its hardness, glass transition temperature, brittleness, etc. are far lower than those of Examples 1-4, and its linear expansion coefficient is high, showing poor temperature resistance. Compared with Examples 1-4, the glue stick of Example 6 uses a combination of POSS-epoxy and triglycidyl p-aminophenol (AFG-90) in component A, and a combination of POSS-thiol curing agent and Huntsman Capcure 3-800 in component B. Although it contains a POSS skeleton structure, the hardness, glass transition temperature, brittleness, etc. of the obtained cured product are far lower than those of Examples 1-4, and its linear expansion coefficient is high, showing poor temperature resistance. The results of Examples 5 and 6 show that the cured products obtained using components A and B that are not of the present invention cannot meet actual processing requirements in terms of hardness, Tg, temperature resistance, etc.
[0098] Furthermore, in the stick glue of Example 7, component B is the same as Example B3 of the present invention, but component A adopts a combination of tetrafunctional glycidylamine (AG-80H) and phenolic epoxy, and its performance is slightly better than that of Example 5, indicating that component B of the present invention, with the combination of specific components, can improve the hardness, Tg, temperature resistance, etc. of the cured product; in the stick glue of Example 8, component A is the same as Example A2 of the present invention, but component B adopts a combination of POSS-thiol curing agent and Huntsman Capcure 3-800, and its performance is slightly better than that of Example 6, indicating that component A of the present invention, with the combination of specific components, can improve the hardness, Tg, temperature resistance, etc. of the cured product.
[0099] The above results show that the epoxy glue for semiconductor cutting and splicing rods provided by the present invention has a synergistic effect between the components under the compounding of component A (including POSS-epoxy, phenolic epoxy, a first filler, a first auxiliary agent) and component B (including POSS-thiol curing agent, modified amine curing agent, accelerator, second filler, and second auxiliary agent), so that the obtained splicing rod glue has a hardness and brittleness close to that of the semiconductor material after curing, better compatibility with the semiconductor material, low water absorption and high glass transition temperature, and excellent temperature resistance, which can better adapt to the cutting and splicing of third-generation semiconductor high-brittle materials, and can ensure that the hardness after curing, especially the hardness during cutting, remains unchanged, and the temperature change during the cutting process will not damage the semiconductor material. It can pass through the tungsten steel wire more smoothly, reduce the wire bow, and improve the cutting yield.
[0100] In the above embodiments, the description of each embodiment has its own focus. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.
[0101] The above description is a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and such modifications or substitutions are intended to be within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be subject to the scope of protection of the claims.
Claims
1. An epoxy adhesive for semiconductor cutting and splicing rods, characterized in that: It includes component A and component B; In parts by weight, the component A comprises the following ingredients: POSS-epoxy caged polysilsesquioxane 17-25 parts by weight; 8-15 parts by weight of novolac epoxy; 58-72 parts by weight of the first filler; 2-5 parts by weight of the first auxiliary agent; The B component includes the following ingredients in parts by weight: POSS-mercapto caged polysilsesquioxane 17-23 parts by weight; 5-10 parts by weight of modified amine curing agent; 3-5 parts by weight of accelerator; 60-70 parts by weight of the second filler; 2-3 parts by weight of the second auxiliary agent; The POSS-epoxy caged polysilsesquioxane includes at least one of octa-glycidyl ether POSS-glycidyl ether oxygen propyl caged polysilsesquioxane, alicyclic epoxy POSS-octa-epoxy cyclohexylethyl caged polysilsesquioxane, and glycidyl ether oxygen propyl cyclotetrasiloxane; The phenolic epoxy is a combination of EPICLON HP-4710 and diethylcyclopentadiene phenolic epoxy DCPD; The general formula of the POSS-mercapto caged polysilsesquioxane is (RSiO 3 / 2 )n, R is mercaptopropionate, n=8; The modified amine curing agent is obtained by condensation reaction of 3,3-dimethyl-4,4-diaminodicyclohexylmethane and thiourea; The first filler is a combination of spherical silica, spherical alumina, and spherical silicon carbide with a low linear expansion coefficient, and the usage ratio of the three is 2:3:5; wherein the spherical silica is a combination of 5μm spherical silica, 0.5μm spherical silica, and 0.05μm spherical silica at a ratio of 10:2:1; the spherical alumina is a combination of 3μm spherical alumina, 0.5μm spherical alumina, and 0.03μm spherical alumina at a ratio of 8:2:1; and the spherical silicon carbide is a combination of 8μm spherical silicon carbide, 1μm spherical silicon carbide, and 0.05μm spherical silicon carbide at a ratio of 7:2:1; The composition of the second filler is the same as that of the first filler.
2. The epoxy adhesive for semiconductor cutting and splicing sticks according to claim 1, wherein: The accelerator includes at least one of Versamine EH-50, ACC 2950, and HI-54K.
3. The epoxy adhesive for semiconductor cutting and splicing sticks according to claim 1, wherein: The first auxiliary agent and the second auxiliary agent independently include at least one of a defoaming agent, a leveling agent, and a dispersant.
4. The epoxy adhesive for semiconductor cutting and splicing sticks according to claim 1, wherein: The mass ratio of the component A to the component B is 1:0.9-1.
1. The component A and the component B are prepared and stored separately, and then mixed before use.
5. A method for preparing the epoxy adhesive for semiconductor dicing sticks according to any one of claims 1 to 4, characterized in that: The following steps are involved: POSS-epoxy caged polysilsesquioxane, phenolic epoxy, a first filler and a first auxiliary agent are mixed and dispersed to prepare component A; POSS-mercapto caged polysilsesquioxane, modified amine curing agent, accelerator, second filler and second auxiliary agent are mixed and dispersed to prepare component B; Mix component A and component B in proportion and use immediately.
Citation Information
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Epoxy Resin Adhesives, Their Preparation Methods, and Applications
CN115651580B
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