Die attach adhesive composition

Abstract

In order to solve the problems that most of tackifiers added into existing solid crystal glue compositions are low-molecular-weight polysiloxane containing hydroxyl terminated and methoxyl terminated, bubbles are likely to occur in the curing process, and the solid crystal glue compositions are low in mechanical strength and insufficient in bonding performance, the invention provides a solid crystal glue composition. Comprising the following components in parts by weight: 30-100 parts of vinyl silicone resin, 10-35 parts of hydrogen-containing silicone oil, 1-10 parts of an organic silicon tackifier, 0.1-1.5 parts of an inhibitor and 0.1-1.5 parts of a catalyst, the organic silicon tackifier is a compound as shown in a structural formula 1, wherein the structural formula 1 is (R1R2R3SiO1 / 2) x (R4R5SiO2 / 2) y (R6SiO3 / 2) z; in the structural formula 1, 0 < x < 1, 0 < y < 1, 0 < z < 1, and 0 < x + y + z < 1; r1, R3 and R4 are selected from at least one of aryl and C1-C5 alkyl, and R2 is selected from C2-C8 alkenyl; r5 is selected from the group consisting of epoxy propoxy propyl; and R6 is selected from aryl. According to the solid crystal glue composition provided by the invention, the cross-linking density and the mechanical strength are improved, few bubbles are generated during curing, and the cold and hot impact resistance effect of the solid crystal glue composition is remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of crystal bonding adhesives, and in particular to a crystal bonding adhesive composition. Background Art

[0002] In the field of electronic packaging, die-bonding adhesive compositions play a crucial role in firmly bonding chips to substrates, providing adhesion. The performance of these adhesive compositions directly impacts the reliability, stability, and service life of electronic devices. With the rapid advancement of electronic technology, electronic devices are moving towards miniaturization, higher performance, and greater integration, placing higher demands on the mechanical strength and bonding properties of die-bonding adhesives.

[0003] Existing adhesive compositions include vinyl silicone resin, hydrogenated silicone oil, inhibitors, fillers, and catalysts. During the curing process, the vinyl silicone resin and hydrogenated silicone undergo a cross-linking reaction to form a three-dimensional network structure. While some degree of cross-linking can be achieved, the number of cross-linking points is limited, resulting in a loose network structure and low mechanical strength and adhesion. To further improve the adhesion of the adhesive composition, a silicone thickener is added. Currently, the majority of silicone thickeners used in addition-type silicones on the market are low-molecular-weight polyorganosiloxanes with hydroxyl and methoxy endcapping. These are prone to bubbles during the curing process, forming internal defects within the overall structure of the adhesive composition, which in turn leads to low mechanical strength and poor adhesion. Furthermore, the presence of a large number of terminal methoxy and terminal hydroxyl groups inevitably increases the hygroscopicity of the thickener itself, resulting in poor storage stability. Summary of the Invention

[0004] In order to solve the problems that the tackifiers added to existing solid crystal adhesive compositions are mostly low molecular weight polysiloxanes containing hydroxyl end-capping and methoxy end-capping, bubbles are easily generated during the curing process, and the solid crystal adhesive compositions have low mechanical strength and insufficient bonding performance, the present application provides a solid crystal adhesive composition.

[0005] In order to solve the above problems, the present invention provides a die-bonding adhesive composition, comprising the following parts by weight: 30-100 parts of vinyl silicone resin, 10-35 parts of hydrogenated silicone oil, 1-10 parts of organosilicon tackifier, 0.1-1.5 parts of inhibitor, and 0.1-1.5 parts of catalyst; The organosilicon tackifier is a compound represented by structural formula 1, (R1R2R3SiO 1 / 2 ) x (R4R5SiO 2 / 2 ) y (R6SiO 3 / 2 ) z ; Structural formula 1 Wherein, 0<x<1, 0<y<1, 0<z<1, and 0<x+y+z<1; R1, R3, and R4 are selected from at least one of an aromatic group and a C1-C5 alkyl group; R2 is selected from a C2-C8 alkenyl group; R5 is selected from a glycidoxypropyl group; and R6 is selected from an aromatic group.

[0006] Preferably, R1, R3, and R4 are selected from phenyl and C1-C2 alkyl; R2 is selected from C2~C3 alkenyl; R6 is selected from phenyl.

[0007] Preferably, x:y:z is (0.08~0.50):(0.20~0.75):(0.15~0.60).

[0008] Preferably, the vinyl silicone resin includes one or more of methyl vinyl silicone resin, phenyl vinyl silicone resin, methoxy vinyl silicone resin, and hydroxy vinyl silicone resin; The hydrogen-containing silicone oil includes one or more of methyl hydrogen-containing silicone oil, ethyl hydrogen-containing silicone oil, and phenyl hydrogen-containing silicone oil; The inhibitor includes one or more of 3-methylbutynol, 1-ethynylcyclohexanol, tris[(1,1-dimethyl-2-propynyl)oxy]methylsilane, tris[(1,1-dimethyl-2-propynyl)oxy]ethylsilane, bis[(1,1-dimethyl-2-propynyl)oxy]dimethylsilane, bis[(1,1-dimethyl-2-propynyl)oxy]methylvinylsilane, and bis(1-ethynylcyclohexyloxy)dimethylsilane; The catalyst includes one or more of chloroplatinic acid and Custer catalyst.

[0009] Preferably, the preparation method of the organosilicon tackifier comprises the following steps: performing a first reflux reaction on the first monomer, the second monomer, the acidic catalyst and water, and performing a first post-treatment after the first reflux reaction to obtain a first mixture; subjecting the first mixture, the alkaline catalyst, the third monomer and water to a second reflux reaction, and performing a second post-treatment after the second reflux reaction to obtain a second mixture; Separating the second mixture to obtain an organic phase, heating the organic phase and the alkaline catalyst to react, obtaining a third mixture after the reaction is completed, and performing a third post-treatment on the third mixture to obtain the organosilicon tackifier; The second monomer includes a compound represented by structural formula 2, , Wherein, R6 is selected from an aromatic group, and R7, R8, and R9 are selected from a C1 to C4 alkyl group; The third monomer includes the compound shown in structural formula 3, wherein R4 is selected from at least one of an aromatic group and a C1-C5 alkyl group, and R5 is selected from a glycidoxypropyl group; R 11 、R 12 Each independently selected from a C1~C4 alkyl group; The first monomer includes the compound shown in structural formula 4 or the compound shown in structural formula 5, 、 Wherein, R1 and R3 are selected from at least one of an aromatic group and a C1 to C5 alkyl group; R2 is selected from a C2 to C8 alkenyl group; R 10 An alkyl group selected from C1 to C4.

[0010] Preferably, the acidic catalyst includes one or more of hydrochloric acid, sulfuric acid, trifluoromethanesulfonic acid, phosphoric acid, perchloric acid, and acetic acid; The mass ratio of the acidic catalyst to the first monomer is (0.005-0.015):1; The alkaline catalyst includes one or more of potassium hydroxide, sodium hydroxide, magnesium hydroxide, barium hydroxide, urea, sodium methoxide, sodium ethoxide, triethylamine, and diethylamine; In the step of preparing the second mixture, the mass ratio of the alkaline catalyst to the third monomer is (0.003-0.007):1; In the heating reaction step, the mass ratio of the alkaline catalyst to the organic phase is (0.001-0.005):1.

[0011] Preferably, the reaction temperature of the first reflux reaction is 65-75° C., and the reaction time of the first reflux reaction is 0.5-3 h; The reaction temperature of the second reflux reaction is 75-85° C., and the reaction time of the second reflux reaction is 0.5-3 h.

[0012] Preferably, the first post-treatment to obtain the first mixture comprises the following steps: after the first reflux reaction is completed, a first mixed solution is obtained, and the first mixed solution is distilled until no fraction is left, and the remaining liquid is the first mixture; The second post-treatment to obtain the second mixture includes the following steps: after the second reflux reaction is completed, a second mixed solution is obtained, and the second mixed solution is distilled until there is no fraction, and the remaining liquid is the second mixture.

[0013] Preferably, separating the second mixture to obtain an organic phase comprises the following steps: adding an organic solvent to the second mixture for extraction and separation to obtain the organic phase; The heating reaction temperature is 90-130°C and the heating reaction time is 2-8 hours; The third mixture is subjected to a third post-processing to obtain the organosilicon tackifier, comprising the following steps: the third mixture is subjected to sequential neutralization, washing, adsorption, filtration, and reduced pressure distillation to obtain the organosilicon tackifier.

[0014] Preferably, the vinyl content of the organosilicon tackifier is 0.05 to 1.0 mol / 100 g; And / or, the epoxy equivalent of the silicone tackifier is 200-600 g / eq.

[0015] The solid crystal adhesive composition provided by the present application undergoes a silane-hydrogenation reaction with the hydrogenated silicone oil during curing to cross-link, generate multiple cross-linking points, and form a three-dimensional network, thereby giving the solid crystal adhesive mechanical strength; the organosilicon adhesive of the compound shown in Structural Formula 1 contains glycidoxypropyl and alkenyl groups. On the one hand, the alkenyl groups on the organosilicon adhesive molecular chain undergo silane-hydrogenation with the hydrogenated silicone oil to increase the cross-linking density, thereby forming a tightly interpenetrating three-dimensional network with the addition product of the vinyl silicone resin and the hydrogenated silicone oil, thereby increasing the mechanical strength of the solid crystal adhesive body; on the other hand, the epoxy groups on the organosilicon adhesive molecular chain are bonded to the hydroxyl groups on the surface of the substrate after ring opening, further increasing the adhesion force of the substrate surface, and under the premise that the x, y, and z in the compound shown in Structural Formula 1 are within the specified range, they can maintain excellent resistance to cold and hot shock; at the same time, the organosilicon adhesive provided by the present application is free of hydroxyl groups and alkoxy groups, and has better storage stability; there are few bubbles during curing, and the internal structure of the solid crystal adhesive composition will not be destroyed.

[0016] The crystal-bonding adhesive composition provided in the present application has a high cross-linking density, high mechanical strength, strong adhesion to the substrate surface, better resistance to cold and hot shocks, few bubbles during curing, and a stable internal structure of the crystal-bonding adhesive composition. DETAILED DESCRIPTION

[0017] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0018] In order to illustrate the technical solution of the present invention, specific embodiments are provided below.

[0019] In one aspect, the present application provides a die-bonding adhesive composition comprising the following parts by weight: 30-100 parts of vinyl silicone resin, 10-35 parts of hydrogenated silicone oil, 1-10 parts of organosilicon tackifier, 0.1-1.5 parts of inhibitor, and 0.1-1.5 parts of catalyst; The organosilicon tackifier is a compound represented by structural formula 1, (R1R2R3SiO 1 / 2 ) x (R4R5SiO 2 / 2 ) y (R6SiO 3 / 2 ) z ; Structural formula 1 Wherein, 0<x<1, 0<y<1, 0<z<1, and 0<x+y+z<1; R1, R3, and R4 are selected from at least one of an aromatic group and a C1-C5 alkyl group; R2 is selected from a C2-C8 alkenyl group; R5 is selected from a glycidoxypropyl group; and R6 is selected from an aromatic group.

[0020] Specifically, aromatic groups include phenyl or benzene derivatives. C1-C5 alkyl groups are alkyl groups with 1 to 5 carbon atoms, including linear alkyl groups with 1 to 5 carbon atoms, or branched alkyl groups with 1 to 5 carbon atoms, such as methyl, ethyl, propyl, butyl, or isopropyl, isobutyl, etc.

[0021] The C2~C8 alkenyl group is an alkenyl group having 2 to 8 carbon atoms, including a straight-chain alkenyl group having 2 to 8 carbon atoms, or a branched alkenyl group having 2 to 8 carbon atoms, such as vinyl, -CH=CHCH2CH3, or -CH=C(CH3)CH2CH3, -CH=C(CH3)CH3, etc.

[0022] The solid crystal adhesive composition provided by the present application undergoes a silylation reaction between the vinyl silicone resin and the hydrogenated silicone oil during curing to cross-link, generate multiple cross-linking points, and form a three-dimensional network, thereby giving the solid crystal adhesive mechanical strength; the organosilicon adhesive of the compound shown in Structural Formula 1 contains glycidoxypropyl and alkenyl groups. On the one hand, the alkenyl groups on the organosilicon adhesive molecular chain undergo silylation reaction with the hydrogenated silicone oil to increase the cross-linking density, thereby forming a tightly interpenetrating three-dimensional network between the addition products of the vinyl silicone resin and the hydrogenated silicone oil, thereby increasing the mechanical strength of the solid crystal adhesive body; on the other hand, the epoxy groups on the organosilicon adhesive molecular chain are bonded to the hydroxyl groups on the surface of the substrate after ring opening, further increasing the adhesion force of the substrate surface, and under the premise that the ranges of x, y, and z in the compound shown in Structural Formula 1 are limited, excellent resistance to cold and hot shock can be maintained; at the same time, the organosilicon adhesive provided by the present application is free of hydroxyl groups and alkoxy groups, and has better storage stability; few bubbles are generated during curing, and the internal structure of the solid crystal adhesive composition will not be damaged.

[0023] In some preferred embodiments, R1, R3, and R4 are selected from phenyl and C1~C2 alkyl.

[0024] Specifically, the C1-C2 alkyl group includes a methyl group and an ethyl group.

[0025] In some preferred embodiments, R2 is selected from C2~C3 alkenyl.

[0026] The C2~C3 alkenyl group includes vinyl, -CH=CH-CH3 or -CH2-CH=CH2.

[0027] In some preferred embodiments, R6 is selected from phenyl.

[0028] In some embodiments, x:y:z is (0.08-0.60):(0.20-0.75):(0.15-0.60).

[0029] Specifically, in structural formula 1, R5 is selected from glycidoxypropyl, R2 is selected from alkenyl of C2~C8, and x:y:z is limited to the range of (0.08~0.60):(0.20~0.75):(0.15~0.60), which helps to obtain the epoxy equivalent in the silicone tackifier in the range of 200~600g / eq and the vinyl content in the silicone tackifier in the range of 0.05~1.0mol / 100g; it is beneficial for the silicone tackifier to be interspersed into the three-dimensional network structure formed by cross-linking the vinyl silicone resin and the hydrogenated silicone oil, thereby forming a tightly interpenetrating three-dimensional network structure, improving the crosslinking density and mechanical strength, and thus increasing the mechanical strength of the solid crystal adhesive body.

[0030] Specifically, x:y:z can be 0.08:0.2:0.15, 0.1:0.3:0.2, 0.2:0.35:0.4, 0.3:0.4:0.4, 0.4:0.5:0.4, 0.5:0.6:0.45, 0.6:0.7:0.55, etc., as long as the value of x:y:z is in the range of (0.08~0.60): (0.20~0.75): (0.15~0.60).

[0031] In some embodiments, the vinyl silicone resin includes one or more of methyl vinyl silicone resin, phenyl vinyl silicone resin, methoxy vinyl silicone resin, and hydroxy vinyl silicone resin.

[0032] Specifically, the vinyl silicone resin is selected from the above types, which is conducive to reacting with hydrogenated silicone oil to form a three-dimensional network structure; at the same time, it is conducive to the reaction between the vinyl silicone resin and the organic silicone tackifier, so that the die-bonding adhesive has mechanical strength.

[0033] In some embodiments, the hydrogen-containing silicone oil includes one or more of methyl hydrogen-containing silicone oil, ethyl hydrogen-containing silicone oil, and phenyl hydrogen-containing silicone oil.

[0034] Specifically, the hydrogenated silicone oil is selected from the above types, which is conducive to reacting with the vinyl silicone resin to form a three-dimensional network structure; at the same time, it is conducive to the reaction of the hydrogenated silicone oil with the organosilicon tackifier, so that the die-bonding adhesive has mechanical strength.

[0035] In some embodiments, the inhibitor includes one or more of 3-methylbutynol, 1-ethynylcyclohexanol, tris[(1,1-dimethyl-2-propynyl)oxy]methylsilane, tris[(1,1-dimethyl-2-propynyl)oxy]ethylsilane, bis[(1,1-dimethyl-2-propynyl)oxy]dimethylsilane, bis[(1,1-dimethyl-2-propynyl)oxy]methylvinylsilane, and bis(1-ethynylcyclohexyloxy)dimethylsilane.

[0036] Specifically, the inhibitor is selected from the above types, which can effectively control the curing reaction, prevent premature polymerization or cross-linking, improve the stability of the solid crystal adhesive, and facilitate transportation and storage.

[0037] In some embodiments, the catalyst includes one or more of chloroplatinic acid and Custer's catalyst.

[0038] In some embodiments, the preparation method of the organosilicon tackifier comprises the following steps: performing a first reflux reaction on the first monomer, the second monomer, the acidic catalyst and water, and performing a first post-treatment after the first reflux reaction to obtain a first mixture; subjecting the first mixture, the alkaline catalyst, the third monomer and water to a second reflux reaction, and performing a second post-treatment after the second reflux reaction to obtain a second mixture; Separating the second mixture to obtain an organic phase, heating the organic phase and the alkaline catalyst to react, obtaining a third mixture after the reaction is completed, and performing a third post-treatment on the third mixture to obtain the organosilicon tackifier; The second monomer includes a compound represented by structural formula 2, , Wherein, R6 is selected from an aromatic group, and R7, R8, and R9 are selected from a C1 to C4 alkyl group; The third monomer includes the compound shown in structural formula 3, wherein R4 is selected from at least one of an aromatic group and a C1-C5 alkyl group, and R5 is selected from a glycidoxypropyl group; R 11 、R 12 Each independently selected from a C1~C4 alkyl group; The first monomer includes the compound shown in structural formula 4 or the compound shown in structural formula 5, 、 Wherein, R1 and R3 are selected from at least one of an aromatic group and a C1 to C5 alkyl group; R2 is selected from a C2 to C8 alkenyl group; R 10 An alkyl group selected from C1 to C4.

[0039] Specifically, because the third monomer contains a glycidoxypropyl group, if an acidic catalyst is present, the glycidoxypropyl group is easily ring-opened in an acidic environment, and the epoxy equivalent content in the resulting silicone tackifier is reduced. Therefore, it is necessary to add the third monomer to react in the absence of an acidic catalyst, which is conducive to preparing a silicone tackifier with an epoxy equivalent in the range of 200 to 600 g / eq.

[0040] The first monomer and the second monomer undergo a first reflux reaction under the catalytic action of an acidic catalyst to generate short molecular chains. After the first reflux reaction, a first post-treatment is performed to obtain a first mixture. An alkaline catalyst is first added to the first mixture to remove the previous acidic catalyst. Then, the third monomer is added to prevent the third monomer from causing the glycidoxypropyl ring-opening due to the acidic environment, thereby reducing the number of effective epoxy groups in the silicone tackifier.

[0041] The organic phase contains a shorter molecular chain structure. Under the action of an alkaline catalyst, the organic phase continues to undergo a heating reaction, allowing the molecular chain to further grow, thereby forming an organosilicon thickener of the compound shown in structural formula 1.

[0042] The preparation method of the organosilicon thickener provided in the present application has the following effects: 1) a staged polymerization process is adopted to ensure that there are no residual reactive alkoxy groups and hydroxyl groups, and the required ratio and structure can be more accurately controlled to generate an organosilicon thickener with a suitable molecular weight; 2) the yield of the obtained organosilicon thickener is as low as 90% and as high as 96%, which is a high yield and improves production efficiency; the organosilicon thickener has a low ion concentration (conductivity <3.00μS / cm) and can be directly used in the field of electronic-grade glue; 3) the organosilicon thickener has no alkoxy groups and no hydroxyl groups, greatly reduces moisture absorption, can be stored for at least 18 months without deterioration, and has strong storage stability; 4) the organosilicon thickener, when used in the solid crystal adhesive composition, produces fewer bubbles during curing, can significantly improve the adhesion of the solid crystal adhesive composition to the substrate, and significantly improves the resistance to cold and hot shock.

[0043] In some preferred embodiments, the second monomer includes phenyltrimethoxysilane.

[0044] In some preferred embodiments, the third monomer includes [2,3-glycidoxypropyl]methyldimethoxysilane.

[0045] Specifically, the structural formula of [2,3-glycidoxypropyl]methyldimethoxysilane is .

[0046] In some preferred embodiments, the first monomer includes 1,1,3,3-tetramethyl-1,3-divinyldisiloxane.

[0047] In some embodiments, the acidic catalyst includes one or more of hydrochloric acid, sulfuric acid, trifluoromethanesulfonic acid, phosphoric acid, perchloric acid, and acetic acid.

[0048] Specifically, the acidic catalyst helps the first monomer and the second monomer to hydrolyze to generate Si—OH, and also helps the Si—OH to condense to generate a polymer with a small molecular chain.

[0049] In some preferred embodiments, the acidic catalyst comprises trifluoromethanesulfonic acid.

[0050] In some embodiments, the mass ratio of the acidic catalyst to the first monomer is (0.005-0.015):1.

[0051] Specifically, the mass ratio of the added acidic catalyst to the first monomer is in the range of (0.005-0.015):1, which accelerates the hydrolysis and polymerization reactions of the first monomer and the second monomer. The mass ratio of the acidic catalyst to the first monomer can be in the following ranges: (0.005-0.008):1, (0.008-0.01):1, (0.01-0.012):1, or (0.012-0.015):1.

[0052] In some embodiments, the alkaline catalyst includes one or more of potassium hydroxide, sodium hydroxide, magnesium hydroxide, barium hydroxide, urea, sodium methoxide, sodium ethoxide, triethylamine, and diethylamine.

[0053] A portion of the alkaline catalyst is used to react with the acidic catalyst to remove the acidic catalyst contained in the first mixture and prevent the glycidoxypropyl group from ring-opening under an acidic environment. The other portion of the alkaline catalyst promotes the hydrolysis of the third monomer to generate Si-OH and at the same time helps the Si-OH condensation reaction to generate a polymer of the small molecular chain shown in structural formula 1.

[0054] In some preferred embodiments, the basic catalyst comprises potassium hydroxide.

[0055] In some embodiments, in the step of preparing the second mixture, the mass ratio of the alkaline catalyst to the third monomer is (0.003-0.007):1.

[0056] Specifically, the mass ratio of the added alkaline catalyst to the third monomer is in the range of (0.003-0.007):1, a portion of which can neutralize the acidic catalyst, and the other portion can accelerate the hydrolysis of the third monomer and the polymerization reaction with the first mixture.

[0057] In the heating reaction step, the mass ratio of the alkaline catalyst to the third monomer is (0.001-0.005):1.

[0058] Specifically, during the heating reaction step, adding a basic catalyst helps the organic phase to continue to polymerize to form an organosilicon viscosity enhancer with a suitable molecular weight.

[0059] In some embodiments, the reaction temperature of the first reflux reaction is 65-75° C., and the reaction time of the first reflux reaction is 0.5-3 h.

[0060] Specifically, the temperature of the first reflux reaction is in the range of 65-75°C, which facilitates the hydrolysis of the first and second monomers to form Si-OH groups and also facilitates the Si-OH condensation reaction to form a polymer with a small molecular chain. Specifically, the temperature of the first reflux reaction can be 65°C, 67°C, 68°C, 69°C, 70°C, 72°C, 73°C, 75°C, etc., as long as the temperature is within the range of 65-75°C.

[0061] In some embodiments, in the first reflux reaction step of the first monomer, the second monomer, the acidic catalyst, and water, the mass ratio of water to the first monomer is (0.8-2.2):1.

[0062] In some embodiments, the reaction temperature of the second reflux reaction is 75-85° C., and the reaction time of the second reflux reaction is 0.5-3 h.

[0063] Specifically, the temperature of the second reflux reaction is in the range of 75°C to 85°C, which facilitates the hydrolysis of the third monomer to form Si-OH and the condensation reaction of Si-OH to form the polymer of the small molecular chain shown in Structural Formula 1. Specifically, the temperature of the second reflux reaction can be 75°C, 77°C, 78°C, 79°C, 80°C, 82°C, 83°C, 85°C, etc., as long as the temperature is within the range of 75°C to 85°C.

[0064] In some embodiments, in the second reflux reaction step of the first mixture, the alkaline catalyst, the third monomer, and water, the mass ratio of water to the third monomer is (0.3-0.4):1.

[0065] In some embodiments, the first post-treatment to obtain the first mixture includes the following steps: after the first reflux reaction is completed, a first mixed solution is obtained, and the first mixed solution is distilled until there is no fraction, and the remaining liquid is the first mixture.

[0066] Specifically, the first mixed solution obtained after the first reflux reaction contains an acidic catalyst and byproducts such as methanol produced by the decomposition of the first and second monomers. During the distillation of the first mixed solution, byproducts such as methanol produced by the first and second monomers are evaporated and removed. The resulting first mixture includes a polymer of small molecular chains generated by the reaction of the first and second monomers, an acidic catalyst, and a small amount of water.

[0067] In some embodiments, the second post-treatment to obtain the second mixture comprises the following steps: after the second reflux reaction is completed, a second mixed solution is obtained, and the second mixed solution is distilled until there is no fraction, and the remaining liquid is the second mixture.

[0068] Specifically, similarly, distilling the second mixed solution also removes by-products produced during the reaction.

[0069] In some embodiments, separating the second mixture to obtain an organic phase comprises the following steps: adding an organic solvent to the second mixture for extraction and separation to obtain the organic phase.

[0070] Specifically, an organic solvent is added to the second mixture to perform extraction and liquid separation to obtain an organic phase, thereby removing water from the second mixture.

[0071] In some embodiments, the heating reaction temperature is 90-130° C., and the heating reaction time is 2-8 hours.

[0072] Specifically, the organic phase and the alkaline catalyst are heated to react. Under the catalytic action of the alkaline catalyst, the heating temperature is within the range of 90-130°C, which is conducive to the continued growth of the molecular chains in the organic phase, forming long molecular chains, thereby making it easier to control the molecular weight of the generated organosilicon tackifier. The heating temperature of the heating reaction can be 90°C, 92°C, 95°C, 98°C, 100°C, 102°C, 104°C, 108°C, 110°C, 115°C, 118°C, 120°C, 126°C, 130°C, 140°C, 150°C, etc., as long as the heating reaction temperature is within the range of 90°C-130°C.

[0073] In some preferred embodiments, the temperature of the heating reaction is 120°C.

[0074] In some embodiments, subjecting the third mixture to a third post-treatment to obtain the organosilicon tackifier comprises the following steps: subjecting the third mixture to sequential neutralization, washing, adsorption, filtration, and reduced pressure distillation to obtain the organosilicon tackifier.

[0075] Specifically, the third mixture is first neutralized using a pH adjuster, which is an acidic compound. The pH adjuster is required to react with the added alkaline catalyst to form a salt, thereby removing the alkaline catalyst. After neutralization, the mixture is washed to remove the salt and the acidic compound. After washing, an adsorbent is added to adsorb the pigment ions. After adsorption, the mixture is filtered to remove water-insoluble impurities, such as the adsorbent. After filtration, the mixture is subjected to reduced pressure distillation to obtain the organosilicon thickener.

[0076] Adsorbents include one or more combinations of activated carbon, diatomaceous earth, anhydrous calcium chloride, and anhydrous magnesium sulfate. Since residual halogens and colored cations may remain in the raw silane monomer during production, packaging, and transportation, as well as residual ions from the neutralization and washing steps, these can cause the finished resin to yellow and affect light transmittance. Adding adsorbents to the polymer can achieve lower color values and lower ion concentrations.

[0077] In some embodiments, the organosilicon tackifier has a vinyl content of 0.05 to 1.0 mol / 100 g.

[0078] Specifically, the organosilicon tackifier prepared by the preparation method of the present application has a vinyl content within the range of 0.05 mol / 100 g to 1.0 mol / 100 g, which increases the crosslinking density of the die-bonding adhesive composition and improves the bonding effect of the die-bonding adhesive composition. If the vinyl content is less than 0.05 mol / 100 g, the bonding effect of the die-bonding adhesive composition is poor; if the vinyl content is greater than 1.0 mol / 100 g, it is easily oxidized, causing the adhesive to yellow. Specifically, the vinyl content of the silicone tackifier may be in the range of 0.05 mol / 100 g to 0.1 mol / 100 g, 0.1 mol / 100 g to 0.15 mol / 100 g, 0.15 mol / 100 g to 0.25 mol / 100 g, 0.25 mol / 100 g to 0.45 mol / 100 g, 0.45 mol / 100 g to 0.56 mol / 100 g, 0.56 mol / 100 g to 0.7 mol / 100 g, 0.7 mol / 100 g to 0.85 mol / 100 g, or 0.85 mol / 100 g to 1.0 mol / 100 g.

[0079] In some embodiments, the epoxy equivalent weight of the silicone tackifier is 200 g / eq to 600 g / eq.

[0080] Specifically, the epoxy equivalent weight of the silicone tackifier is in the range of 200 g / eq to 600 g / eq. The epoxy groups can serve as crosslinking points. The epoxy groups can form ring-opening connections with other epoxy groups, with reactive groups in hydrogenated silicone oils and vinyl silicone resins, and with groups on the surface of the substrate. This creates a dense, interpenetrating network structure within the three-dimensional network formed by the vinyl silicone resin, hydrogenated silicone oil, and the like, further enhancing the crosslink density and mechanical strength of the die-bonding adhesive composition. Specifically, the epoxy equivalent weight of the silicone tackifier can be in the following ranges: 200 g / eq to 300 g / eq, 300 g / eq to 400 g / eq, 400 g / eq to 500 g / eq, or 500 g / eq to 600 g / eq.

[0081] If the epoxy equivalent of the silicone tackifier is lower than 200g / eq, the lower the epoxy equivalent, the more epoxy groups are contained in the silicone tackifier system, the curing hardness is too high, and the resistance to cold and hot shock performance deteriorates; if the epoxy equivalent of the silicone tackifier is higher than 600g / eq, the higher the epoxy equivalent, the fewer epoxy groups are in the silicone tackifier system, the cross-linking density is too low, the adhesion to the substrate surface is insufficient, and the bonding effect deteriorates.

[0082] In a second aspect, the present application provides a method for preparing a die-bonding adhesive composition, comprising the following steps: The die-bonding adhesive composition is obtained by uniformly mixing 30-100 parts of vinyl silicone resin, 10-35 parts of hydrogenated silicone oil, 1-10 parts of organosilicon tackifier, 0.1-1.5 parts of inhibitor, and 0.1-1.5 parts of catalyst.

[0083] The preparation method of the crystal-bonding adhesive composition provided in the present application generates few bubbles during curing, has a simple preparation process, and the obtained crystal-bonding adhesive composition has strong adhesion to the substrate, high mechanical strength, and good resistance to cold and hot shocks.

[0084] The present invention is further described below with reference to the following examples.

[0085] Example 1 S1: Preparation of silicone adhesion promoter S11 obtains raw materials: the first monomer is 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, the second monomer is phenyltrimethoxysilane, and the third monomer is 3-[(2,3)-epoxypropyloxy]propylmethyldimethoxysilane. The acidic catalyst is trifluoromethanesulfonic acid, and the alkaline catalyst is potassium hydroxide.

[0086] S12: 1105 g of phenyltrimethoxysilane, 346 g of 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, and 2.4 g of trifluoromethanesulfonic acid were added to a reaction kettle, 330 g of water was added dropwise, and a first reflux reaction was carried out at 70° C. for 1 hour, followed by distillation until no fraction was produced to obtain a first mixture.

[0087] S13: Add 4 g of potassium hydroxide and 220 g of water to the first mixture obtained in step S11, and dropwise add 682 g of 3-[(2,3)-epoxypropoxy]propylmethyldimethoxysilane. Perform a second reflux reaction at 80° C. for 1 hour, and then distill until no fraction is produced to obtain a second mixture.

[0088] S14: Add 1900g of toluene to the second mixture obtained in step S13, stir and extract, separate the lower liquid, obtain the upper liquid organic phase, add 2g of potassium hydroxide to the organic phase, heat to 120℃ for heating reaction, the heating reaction time is 4h, cool down after the heating reaction, cool down to 40~60℃, add acidic solution (such as acetic acid) for neutralization, wash with pure water after neutralization, add adsorbent activated carbon and stir and adsorb for 8h after washing, filter after adsorption, and distill under reduced pressure at -0.1MPa vacuum to obtain the product. The structural formula of the organic silicone thickener in the obtained product is (R1R2R3SiO 1 / 2 ) 0.3 (R4R5SiO 2 / 2 ) 0.25 (R6SiO 3 / 2 ) 0.45 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0089] S2: Preparation of die-bonding adhesive composition S21 obtains raw materials: vinyl silicone resin is selected from methoxyvinyl silicone resin, hydrogen-containing silicone oil is selected from ethyl hydrogen-containing silicone oil, the silicone tackifier is prepared by the above step S1, the inhibitor is selected from tris[(1,1-dimethyl-2-propynyl)oxy]methylsilane, and the catalyst is selected from Custer catalyst.

[0090] S22: 100 parts of methoxyvinyl silicone resin, 5 parts of silicone tackifier, 23 parts of ethyl hydrogen silicone oil, 0.4 parts of Custer catalyst, and 0.5 parts of tris[(1,1-dimethyl-2-propynyl)oxy]methylsilane are mixed evenly to obtain a solid crystal adhesive composition.

[0091] Example 2 Most of the steps in this example are identical to those in Example 1, with the following differences: in step S12, the mass of 1,1,3,3-tetramethyl-1,3-divinyldisiloxane is 160 g, the mass of phenyltrimethoxysilane is 1010 g, the mass of trifluoromethanesulfonic acid is 1.8 g, and the mass of water is 315 g; in step S13, the mass of 3-[(2,3)-epoxypropyloxy]propylmethyldimethoxysilane is 1000 g, and the mass of water is 325 g; the organic solvent for extraction in step S14 is xylene, the mass of xylene is 1900 g; and the heating reaction temperature in step S14 is 150° C., and the heating reaction time is 4 hours. The remaining steps are identical to those in Example 1.

[0092] The structural formula of the organosilicon tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 0.15 (R4R5SiO 2 / 2 ) 0.40 (R6SiO 3 / 2 ) 0.45 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0093] Example 3 Most of the steps in this embodiment are the same as those in Example 1, except that: in step S11, the acidic catalyst is concentrated hydrochloric acid, and the alkaline catalyst is barium hydroxide; in step S12, 107 g of phenyltrimethoxysilane, 18 g of 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, 0.54 g (36.5 wt%) of concentrated hydrochloric acid, and 32 g of water are used; in step S13, the mass of barium hydroxide is 0.35 g, water is 21 g, and 3-[(2,3)-epoxypropyloxy]propylmethyldimethoxysilane is 62 g; the mass of toluene, the organic solvent for extraction used in step S14, is 200 g; and the alkaline catalyst added in step S14 is barium hydroxide, and the mass of the added barium hydroxide is 0.2 g.

[0094] The structural formula of the organosilicon tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 0.20 (R4R5SiO 2 / 2 ) 0.28 (R6SiO 3 / 2 ) 0.54 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0095] Example 4 Most of the steps in this example are the same as those in Example 1, except that the first monomer is vinyldimethylethoxysilane, the second monomer is phenyltriethoxysilane, and the third monomer is [2,3-glycidoxypropyl]methyldiethoxysilane. The rest is the same as in Example 1. The structural formula of the organic silicone tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 0.3 (R4R5SiO 2 / 2 ) 0.25 (R6SiO 3 / 2 ) 0.45 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0096] Example 5 Most of the steps in this example are the same as those in Example 1, except that steps S12 and S13 are different from those in Example 1; in Example 5, 1105 g of phenyltrimethoxysilane, 346 g of 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, 2.4 g of trifluoromethanesulfonic acid, 330 g of water, and 682 g of [2,3-glycidoxypropyl]methyldimethoxysilane are mixed and reacted at a reaction temperature of 80°C to obtain a second mixture. Steps S11 and S14 are the same as those in Example 1; and step S2 is the same as that in Example 1. The structural formula of the organosilicon tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 0.30 (R4R5SiO 2 / 2 ) 0.03 (R6SiO 3 / 2 ) 0.45 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0097] Example 6 Most of the steps in this embodiment are the same as those in embodiment 1, except that: in step S14 in embodiment 6, there is no heating reaction step; that is, embodiment 6 does not have the step of "adding 2 g of potassium hydroxide to the organic phase, heating to 120° C. for heating reaction, heating reaction time is 4 h, cooling after the heating reaction is completed, cooling to a range of 40-60° C.".

[0098] Example 7 Most of the steps in this embodiment are the same as those in Example 1, except that in step S14 in Example 7, the heating reaction temperature is 80° C. and the heating reaction time is 4 h. The rest are the same as in Example 1.

[0099] Example 8 Most of the steps in this example are the same as those in Example 1, except that in step S14 of Example 8, the heating reaction temperature is 160°C and the heating reaction time is 4 hours. The rest is the same as in Example 1. The structural formula of the organic silicon tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 0.17 (R4R5SiO 2 / 2 ) 0.18 (R6SiO 3 / 2 ) 0.45 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0100] Example 9 Most of the steps in this example are the same as those in Example 1, except that the temperature of the first reflux reaction in step S12 of Example 9 is 75° C., and the temperature of the second reflux reaction in step S13 is 85° C. The rest is the same as in Example 1.

[0101] Example 10 Most of the steps in this example are identical to those in Example 1, except that in step S22, the components are present in different quantities: 90 parts methoxyvinyl silicone resin, 10 parts organosilicon tackifier, 35 parts ethyl hydrogen silicone oil, 1.5 parts Custer catalyst, and 1.5 parts tris[(1,1-dimethyl-2-propynyl)oxy]methylsilane. The remainder of the steps is identical to Example 1.

[0102] Example 11 Most of the steps in this embodiment are the same as those in Example 1, except that: in step S12, 170 g of phenyltrimethoxysilane, 3.7 g of 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, 0.26 g of trifluoromethanesulfonic acid, and 51 g of water are added. In step S13, 22 g of [2,3-epoxypropoxypropyl]methyldimethoxysilane, 0.4 g of potassium hydroxide, and 7.2 g of water are added. In step S14, 180 g of toluene is added. The rest is the same as in Example 1. The structural formula of the organosilicon tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 0.04 (R4R5SiO 2 / 2 ) 0.10 (R6SiO 3 / 2 ) 0.86 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl. Example 12 Most of the steps in this embodiment are the same as those in embodiment 1, except that the masses of the first monomer, the second monomer, and the third monomer in embodiment 12 are different, specifically: 525g phenyltrimethoxysilane, 121g 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, 1g trifluoromethylsulfonic acid, and 157g water in step S12. 313g [2,3-epoxypropoxypropyl]methyldimethoxysilane, 1.8g potassium hydroxide, 102g water in step S13, and 1163g toluene in step S14. The rest are the same as in embodiment 1. The structural formula of the organosilicon tackifier in the obtained product is (R1R2R3SiO 1 / 2 ) 1.30 (R4R5SiO 2 / 2 ) 1.42 (R6SiO 3 / 2 ) 2.65 , wherein R6 is selected from phenyl, R1 and R3 are selected from methyl, R2 is selected from vinyl, R5 is selected from glycidoxypropyl, and R4 is selected from methyl.

[0103] Comparative Example 1 Comparative Example 1 is similar to Example 1 in most of its steps, except that: Comparative Example 1 does not include Step S1, and Step S2 in Comparative Example 1, in which the die-bonding adhesive composition is prepared, does not include the organosilicon tackifier used in Step S1. The remainder of the steps is the same as Example 1.

[0104] Comparative Example 2 The tackifier in Comparative Example 2 was prepared in the same manner as in Example 1, except that step S1 of Example 1 was omitted. The tackifier in Comparative Example 2 was a condensation product of 3-glycidylpropyltrimethoxysilane and a methylvinylsiloxane oligomer having two silanol-terminated molecular chain ends. The remaining steps were the same as in Example 1.

[0105] test 1. The yield of the organosilicon tackifier was calculated for the products prepared in the above examples and comparative examples. The vinyl content in the organosilicon tackifier was tested according to GB / T 28610-2012; the epoxy equivalent in the organosilicon tackifier was tested according to GB / T 4612-2008. The specific test results are shown in Table 1.

[0106] The bonding adhesive compositions obtained in the above embodiments and comparative examples were subjected to the following performance tests, and the test results are shown in Table 2.

[0107] 2. Viscosity test: According to GB / T 2794-2022, at 25° C., a cone and plate viscometer (Brookfield, Cap2000+) was used to measure the viscosity of the die-bonding adhesive compositions obtained in each embodiment and comparative example according to the instructions.

[0108] 3. Thixotropy test: According to GB / T 2794-2022, a thixotrope (Brookfield, DVNXHACJG model) was used, and a 25 mm parallel plate was selected to perform a frequency sweep test on the die-bonding adhesive compositions obtained in the above embodiments and comparative examples for 0.01 s. -1 →100S -1 , calculate thixotropic index = 1S -1 / 10S -1 .

[0109] 4. Tensile strength and elongation at break test: According to GB / T 30776-2014, the die-bonding adhesive compositions obtained in the above examples and comparative examples were cut into dumbbell-shaped standard samples, and the tensile strength and elongation at break were tested using an electronic tensile testing machine (BGD570, BGD Precision Instruments (Guangzhou) Co., Ltd.).

[0110] 5. Curing hardness test: According to GB / T 2411-2008, the cured samples of the die-bonding adhesive compositions obtained in the examples and comparative examples were tested at 25° C. using a Shore hardness tester (SD-J, Shanghai Lunjie Electromechanical Instrument Co., Ltd.).

[0111] 6. Number of bubbles: visually.

[0112] 7. Thrust test: Referring to GB / T 7124-2008, the brackets of the cured sheets of the die-bonding adhesive compositions obtained in the Examples and Comparative Examples were cured at 170°C for 2 hours, and the thrust force when the lamp beads were pushed away was tested using a thrust tester (force gauge, LB-8100A model); 8. Hot and cold shock test: The thermal shock performance of the die-bonding adhesive compositions obtained in each embodiment and comparative example was tested using a thermal shock tester (IAI1507-001, Jufu Instrument Industrial Co., Ltd.) in accordance with GB / T 2423.22-87. The test conditions were -45°C for 15 min and 125°C for 15 min, with a transition time of less than 15 s and 1000 cycles.

[0113] Table 1 Table 2 As shown in Tables 1 and 2, when comparing Example 1 with Comparative Examples 1 and 2, the solid crystal adhesive composition in Comparative Example 1 does not contain an organic silicon tackifier, and the viscosity of the solid crystal adhesive composition is high, the tensile strength is low, and the bonding strength between the solid crystal adhesive and the substrate is poor. The tackifier used in Comparative Example 2 is a condensation product of 3-glycidylpropyltrimethoxysilane and a methylvinylsiloxane oligomer with two molecular chain ends capped with silanol groups, which contains hydroxyl groups. During curing, more bubbles are generated, and the bonding strength between the solid crystal adhesive and the substrate is poor, indicating that the addition of the compound shown in structural formula 1 (R1R2R3SiO 1 / 2 ) x (R4R5SiO 2 / 2 ) y (R6SiO 3 / 2 ) z ; Among them, 0<x<1, 0<y<1, 0<z<1, and 0<x+y+z<1; the obtained solid crystal adhesive composition has few bubbles when solidified, a large initial maximum thrust, a small number of lamp beads peeled off in 1000cyc of cold punching, a strong bonding force between the solid crystal adhesive composition and the substrate, high hardness, and high mechanical strength.

[0114] Comparing Example 1 with Example 5, Example 5 reacts the first monomer, the second monomer and the third monomer under the action of an acidic catalyst. Under the acidic catalyst, the glycidoxypropyl group in the third monomer is easily ring-opened, and the epoxy equivalent of the obtained silicone tackifier is greater than 200~600g / eq. The initial maximum thrust value is small, and the number of peeled lamp beads is large. It is speculated that the higher the epoxy equivalent, the fewer epoxy groups in the silicone tackifier system, the low cross-linking density, the insufficient adhesion to the substrate surface, and the poor bonding effect; This indicates that when the epoxy equivalent of the silicone tackifier is in the range of 200~600g / eq, the obtained solid crystal adhesive has good adhesion to the substrate surface, thereby improving the cross-linking density and mechanical strength of the solid crystal adhesive composition.

[0115] Comparing Example 1 with Examples 6 to 8, there is no heating reaction step in Example 6, and the heating reaction temperature in Example 7 is lower than 90 to 130°C. Incomplete heating reaction will lead to incomplete condensation and an increase in residual hydroxyl groups in the tackifier molecules, thereby leading to an increase in the number of solidification bubbles in the solidification adhesive composition, and the initial maximum thrust value is also low; the heating temperature in Example 8 is higher than 90 to 130°C, and the vinyl group is easily oxidized under overheating conditions, resulting in a decrease in the crosslinking density of the final glue, a decrease in mechanical strength, and a decrease in hardness; this indicates that heating the organic phase and the alkaline catalyst to react and controlling the heating temperature within the range of 90 to 130°C is conducive to the continued growth of the molecular chains in the organic phase, forming long molecular chains, controlling the molecular weight, and making the crosslinking density and mechanical strength of the solidification adhesive high.

[0116] Comparing Example 1 with Example 11, the vinyl content in Example 11 is lower than the range of 0.05~1.0mol / 100g, the initial maximum thrust is small, the hardness is low, the number of peeled lamp beads is large, and the mechanical strength and bonding performance of the solid crystal glue are significantly deteriorated, indicating that the vinyl content of the silicone tackifier is in the range of 0.05~1.0mol / 100g, which is beneficial to improving the bonding force between the solid crystal glue and the substrate and high mechanical strength. Comparing Example 1 with Example 12, the prepared silicone tackifier does not satisfy Structural Formula 1. Although a good bonding effect can be obtained, the compound viscosity of the solid crystal adhesive composition will increase significantly, and the thixotropic index increases, which is not conducive to construction. However, it can be seen from Examples 1 to 4 and 9 that the solid crystal adhesive composition using a tackifier satisfying the compound shown in Structural Formula 1 can achieve better bonding performance, fewer curing bubbles, and better resistance to cold and hot shock performance. Comparing Example 1 with Example 10, it can be seen that the solid crystal adhesive composition contains 30 to 100 parts of vinyl silicone resin, 10 to 35 parts of hydrogenated silicone oil, 1 to 10 parts of silicone tackifier, 0.1 to 1.5 parts of inhibitor, and 0.1 to 1.5 parts of catalyst. The obtained solid crystal adhesive composition has few bubbles during curing, good resistance to cold and hot shock performance, high mechanical strength, and high bonding strength with the substrate.

[0117] The above embodiments are intended only to illustrate the technical solutions of the present invention and are not intended to limit them. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they may still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein with equivalents. However, such modifications or replacements do not deviate from the spirit and scope of the technical solutions of the various embodiments of the present invention and are intended to be included within the scope of protection of the present invention.

Claims

1. A die-bonding adhesive composition, characterized in that: Comprises the following weight parts: 30-100 parts of vinyl silicone resin, 10-35 parts of hydrogenated silicone oil, 1-10 parts of organosilicon tackifier, 0.1-1.5 parts of inhibitor, and 0.1-1.5 parts of catalyst; The organosilicon tackifier is a compound represented by structural formula 1, (R1R2R3SiO 1 / 2 ) x (R4R5SiO 2 / 2 ) y (R6SiO 3 / 2 ) z ; Structural formula 1 Wherein, 0<x<1, 0<y<1, 0<z<1, and 0<x+y+z<1; R1, R3, and R4 are selected from at least one of an aromatic group and a C1-C5 alkyl group; R2 is selected from a C2-C8 alkenyl group; R5 is selected from a glycidoxypropyl group; and R6 is selected from an aromatic group.

2. The die-bonding adhesive composition according to claim 1, wherein R1, R3, and R4 are selected from phenyl and C1-C2 alkyl; R2 is selected from C2~C3 alkenyl; R6 is selected from phenyl.

3. The die-bonding adhesive composition according to claim 1, wherein x： y:z is (0.08~0.50): (0.20~0.75): (0.15~0.60).

4. The die-bonding adhesive composition according to claim 1, wherein The vinyl silicone resin includes one or more of methyl vinyl silicone resin, phenyl vinyl silicone resin, methoxy vinyl silicone resin, and hydroxy vinyl silicone resin; The hydrogen-containing silicone oil includes one or more of methyl hydrogen-containing silicone oil, ethyl hydrogen-containing silicone oil, and phenyl hydrogen-containing silicone oil; The inhibitor includes one or more of 3-methylbutynol, 1-ethynylcyclohexanol, tris[(1,1-dimethyl-2-propynyl)oxy]methylsilane, tris[(1,1-dimethyl-2-propynyl)oxy]ethylsilane, bis[(1,1-dimethyl-2-propynyl)oxy]dimethylsilane, bis[(1,1-dimethyl-2-propynyl)oxy]methylvinylsilane, and bis(1-ethynylcyclohexyloxy)dimethylsilane; The catalyst includes one or more of chloroplatinic acid and Custer catalyst.

5. The die-bonding adhesive composition according to claim 1, wherein The preparation method of the organosilicon tackifier comprises the following steps: performing a first reflux reaction on the first monomer, the second monomer, the acidic catalyst and water, and performing a first post-treatment after the first reflux reaction to obtain a first mixture; subjecting the first mixture, the alkaline catalyst, the third monomer and water to a second reflux reaction, and performing a second post-treatment after the second reflux reaction to obtain a second mixture; Separating the second mixture to obtain an organic phase, heating the organic phase and the alkaline catalyst to react, obtaining a third mixture after the reaction is completed, and performing a third post-treatment on the third mixture to obtain the organosilicon tackifier; The second monomer includes a compound represented by structural formula 2, ， Wherein, R6 is selected from an aromatic group, and R7, R8, and R9 are selected from a C1 to C4 alkyl group; The third monomer includes the compound shown in structural formula 3, wherein R4 is selected from at least one of an aromatic group and a C1-C5 alkyl group, and R5 is selected from a glycidoxypropyl group; R 11 、R 12 Each independently selected from a C1~C4 alkyl group; The first monomer includes the compound shown in structural formula 4 or the compound shown in structural formula 5, 、 Wherein, R1 and R3 are selected from at least one of an aromatic group and a C1 to C5 alkyl group; R2 is selected from a C2 to C8 alkenyl group; R 10 An alkyl group selected from C1 to C4.

6. The die-bonding adhesive composition according to claim 5, characterized in that: The acidic catalyst includes one or more of hydrochloric acid, sulfuric acid, trifluoromethanesulfonic acid, phosphoric acid, perchloric acid, and acetic acid; The mass ratio of the acidic catalyst to the first monomer is (0.005-0.015):1; The alkaline catalyst includes one or more of potassium hydroxide, sodium hydroxide, magnesium hydroxide, barium hydroxide, urea, sodium methoxide, sodium ethoxide, triethylamine, and diethylamine; In the step of preparing the second mixture, the mass ratio of the alkaline catalyst to the third monomer is (0.003-0.007):1; In the heating reaction step, the mass ratio of the alkaline catalyst to the third monomer is (0.001-0.005):

1.

7. The die-bonding adhesive composition according to claim 5, characterized in that: The reaction temperature of the first reflux reaction is 65-75° C., and the reaction time of the first reflux reaction is 0.5-3 h; The reaction temperature of the second reflux reaction is 75-85° C., and the reaction time of the second reflux reaction is 0.5-3 h.

8. The die-bonding adhesive composition according to claim 5, wherein The first post-processing to obtain the first mixture comprises the following steps: obtaining a first mixed solution after the first reflux reaction is completed, distilling the first mixed solution until no fraction remains, and the remaining liquid is the first mixture; The second post-treatment to obtain the second mixture includes the following steps: after the second reflux reaction is completed, a second mixed solution is obtained, and the second mixed solution is distilled until there is no fraction, and the remaining liquid is the second mixture.

9. The die-bonding adhesive composition according to claim 5, characterized in that: Separating the second mixture to obtain an organic phase comprises the following steps: adding an organic solvent to the second mixture to perform extraction and separation to obtain the organic phase; The heating reaction temperature is 90-130°C and the heating reaction time is 2-8 hours; The third mixture is subjected to a third post-processing to obtain the organosilicon tackifier, which comprises the following steps: the third mixture is subjected to sequential neutralization, washing, adsorption, filtration, and reduced pressure distillation to obtain the organosilicon tackifier.

10. The die-bonding adhesive composition according to claim 1, wherein The vinyl content of the organosilicon tackifier is 0.05 / 100g~1.0mol / 100g; And / or, the epoxy equivalent of the silicone tackifier is 200 g / eq to 600 g / eq.

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