Organopolysiloxane composition as well as preparation method and application thereof
Through the combination of a complex platinum catalyst and a low-temperature adhesion promoter, the problems of rapid strengthening and stability of the organopolysiloxane composition in the positioning and bonding of semiconductor chip heat dissipation cover plates are solved, low-temperature rapid curing and anti-interference capabilities are improved, and the complex environmental requirements of the semiconductor industry are met.
Patent Information
- Application Number
- CN202510966364.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-14
- Publication Date
- 2025-09-23
AI Technical Summary
Existing organopolysiloxane compositions are difficult to meet the requirements of rapid strengthening, process stability, low-temperature curing and adaptability to complex environments in the positioning and bonding of semiconductor chip heat dissipation cover plates. In particular, the bonding strength is affected in the presence of flux and water-cutting agents.
By combining a complex platinum catalyst with a low-temperature adhesion promoter and using a specific preparation method, the resulting organopolysiloxane composition can quickly bond and strengthen at temperatures above 80°C and maintain the operating time at room temperature, while also improving anti-interference capabilities and reducing the effects of flux and water-cutting agents.
It achieves rapid bonding and strengthening within 5-10 minutes at temperatures of 80°C and above, reaching more than 80% of full curing, and maintains an operating time of 48 hours at room temperature, enhancing the bonding strength stability of the composition in complex environments.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of structural bonding and sealing, and in particular to an organopolysiloxane composition and a preparation method and application thereof. Background Art
[0002] In the semiconductor field, curable organopolysiloxane compositions have found widespread application due to their low glass transition temperature (TG), low modulus, and excellent weather resistance. In particular, their low modulus facilitates stress relief, making them ideal for positioning and bonding semiconductor chip heat dissipation covers.
[0003] In practical applications, there are many performance requirements for organopolysiloxane compositions. On the one hand, the composition needs to have the function of rapid positioning and bonding to meet the needs of production efficiency; on the other hand, it must show excellent adhesion and outstanding bonding reliability to the cover and substrate to ensure the stability and durability of the bonding effect. Moreover, with the advancement of the localization process of the semiconductor industry chain, the electroplating treatment methods of the material interface have become more complicated, which poses more stringent challenges to the environment of the bonding interface. For example, in the presence of flux and water-cutting agents, the material needs to be able to bond quickly and achieve high strength.
[0004] However, existing conventional one-component silicone sealants have numerous shortcomings. They typically need to be stored at low temperatures (approximately -20°C) and, after returning to room temperature, must be used within 24 or even 12 hours. Otherwise, the sealant's viscosity increases significantly, leading to fluctuations in process stability. Conventional one-component silicone sealants typically require high temperatures (above 120°C) for curing, typically taking more than 30 minutes.
[0005] During the bonding and packaging of semiconductor chips onto heat sink covers, a snap-cure process is often used to pre-cure silicone sealants. This process aims to control the thickness of the polyimide thioether (PTIM) material and minimize chip movement during curing and transfer. Therefore, while ensuring sufficient shelf life, the lower the material's initial curing temperature, the better the cure during the pre-cure process, the more precise the PTIM thickness control, and the less likely chip movement will occur during curing and transfer.
[0006] In summary, existing organopolysiloxane compositions struggle to meet the requirements for fast build strength, process stability, low-temperature curing, and adaptability to complex environments for positioning and bonding semiconductor chip heat dissipation cover plates. Therefore, developing a novel organopolysiloxane composition and its preparation method that can address these challenges is of great practical significance. Summary of the Invention
[0007] In order to solve the above technical problems existing in the prior art, the present invention provides an organopolysiloxane composition and a preparation method and application thereof.
[0008] The technical solution of the present invention to solve the above technical problems is as follows: The first aspect of the present invention is to provide an organopolysiloxane composition comprising the following components in parts by weight: Component A: 80-100 parts of an organopolysiloxane containing at least two alkenyl groups per molecule; Component B: 2-25 parts of an organopolysiloxane containing at least two Si-H bonds per molecule; Component C: complex platinum catalyst, 0.001-2 parts; Component D: low temperature adhesion promoter, 0.5-5 parts.
[0009] The organopolysiloxane composition provided by the present invention, through the combined action of a complex platinum catalyst and a low-temperature adhesion promoter, enables the composition of the present invention to rapidly bond and strengthen within 5-10 minutes at a temperature of 80°C or above, reaching more than 80% of full curing, while also ensuring that the composition can maintain an operating time of more than 48 hours at room temperature. Furthermore, the organopolysiloxane composition of the present invention has significantly improved anti-interference and anti-poisoning capabilities, and the degree to which the bonding strength is affected by the snap-cure process in the presence of flux or water-cutting agents is significantly reduced.
[0010] Among them, the snap cure process refers to the instantaneous curing technology achieved through a thermal initiation system.
[0011] On the basis of the above technical solution, the present invention can also make the following improvements: Furthermore, the preparation method of component C includes the following steps: adding a Karstedt catalyst to a vinyl-terminated silicone oil and diluting it to a Pt content of 1000-10000 ppm to obtain a mixed solution; then, adding a certain amount of a phosphorus-containing compound and a polyvinyl cyclic siloxane as a source of complexing ligand to the mixed solution; and treating the mixed solution under reduced pressure at 60-80°C for 0.5-4h to obtain the complexing platinum catalyst.
[0012] The beneficial effect of adopting the above-mentioned further technical solution is that: the lone pair electrons and unpaired electrons outside the P nucleus in the phosphorus-containing compound, the empty 3d orbital, and the polyvinyl electron-deficient structure of the polyvinyl cyclic siloxane are utilized to form a strong coordination complex with Pt(0). On the one hand, the coordination compound has a strong intermolecular coordination force, and on the other hand, it has a good spatial steric structure formation, which can effectively wrap the core Pt(0) and avoid the poisoning effect caused by the coordination of contaminating impurities.
[0013] Furthermore, the Karstedt catalyst is C8H 18 OPtSi2, the pressure of the decompression treatment is ≤-0.09MPa, and the viscosity of the vinyl-terminated silicone oil is ≤1000mPa.s; the addition amount of the phosphorus-containing compound is 0.2‰-2% of the mass of the mixed liquid, and the addition amount of the polyvinyl cyclic siloxane is 0‰-5% of the mass of the mixed liquid; the phosphorus-containing compound includes any one or more of vinyl diethyl phosphate, vinyl (diphenylphosphinoethyl) dimethyl silane, triisopropyl phosphite, trimethoxyphosphine, and triethyl phosphite.
[0014] The beneficial effect of adopting the above-mentioned further technical solution is that by changing the structure of the phosphorus-containing compound and its ratio with the polyvinyl cyclic siloxane, the reaction activity at different temperatures can be effectively controlled through the coordinated coupling of the steric effect, the polyvinyl coordination force, and the P atom coordination complex force.
[0015] Furthermore, the polyvinyl cyclic siloxane contains at least 4 Si-O structural units, and the general structural formula of the polyvinyl cyclic siloxane is ((CH2=CH)R 5 SiO 2 / 2 )(R 5 2SiO 2 / 2 ) y , R 5 Selected from unsubstituted or substituted monovalent hydrocarbon groups, y = 0 to 1.0. Monovalent hydrocarbon groups preferably have 1 to 10 carbon atoms, particularly preferably 1 to 6. Specific examples include lower alkyl groups such as methyl, ethyl, propyl, and isopropyl; cycloalkyl groups such as cyclohexyl; aryl groups such as phenyl, tolyl, and xylyl; aralkyl groups such as benzyl; alkyl groups containing olefinic bonds such as vinyl and propenyl; or groups in which some or all of the hydrogen atoms in the above groups are replaced with halogen atoms, cyano groups, or the like, such as chloromethyl and cyanoethyl. More preferably, groups such as methyl, ethyl, and phenyl are preferred.
[0016] The beneficial effect of adopting the above further technical solution is that the purpose of stimulating the reaction activity at different temperatures is achieved by controlling the structural ratio of the complex ligand.
[0017] Furthermore, the preparation method of component D includes the following steps: dehydrating geraniol at a high temperature of 100-110°C in a vacuum, then adding a mixed solution of tetramethylxylene diisocyanate (TMXDI) or diphenylmethane diisocyanate (MDI) and dehydrated toluene, heating to 100-120°C under nitrogen protection and reflux reaction for 1-4 hours, after the reaction is completed, cooling to below 80°C, adding 3-(2,3-epoxypropoxy)propyltrimethoxysilane, continuing to heat to 100-120°C and reflux reaction for 2-8 hours, and then removing the toluene solvent by reduced pressure distillation to obtain the low-temperature adhesion promoter.
[0018] Furthermore, the molar ratio of geraniol to tetramethylxylene diisocyanate or diphenylmethane diisocyanate is 2:1, the mass ratio of tetramethylxylene diisocyanate or diphenylmethane diisocyanate to dehydrated toluene is 1:1, and the molar ratio of 3-(2,3-epoxypropoxy)propyltrimethoxysilane to geraniol is 1-1.5:1.
[0019] The beneficial effect of adopting the above-mentioned further technical solution is that: the low-temperature adhesion promoter structure obtained by the above-mentioned preparation method contains long-chain alkanes, phenyl groups, alkoxy groups, etc. at the same time. During the curing process, due to the difference in polarity with the main resin molecules, it can quickly separate and migrate to the bonding surface, thereby strengthening the polar intermolecular force with the interface. At the same time, the presence of multiple polar alkane segments, phenyl groups, ester groups, etc., easily generates forces with different interfaces, plays a role in rapid strengthening and interfacial bonding, and promotes the organic polysiloxane composition to form an effective force with the interface faster at a temperature below 100°C.
[0020] Further, the general structural formula of component A is (R 1 R 2 2SiO 1 / 2 )(R 1 R 2 SiO 2 / 2 ) a (R 2 SiO 3 / 2 ) b (SiO 4 / 2 ) c , where R 1 、R 2 are independently selected from unsubstituted or substituted monovalent hydrocarbon groups, a = 0 to 400 (excluding 0), b = 0 to 2, c = 0 to 2, and a+b+c = 1 to 400; the monovalent hydrocarbon group is selected from a group with 1 to 10 carbon atoms, and R 1 and R 2At least one of the groups is a vinyl group. As the monovalent hydrocarbon group, a group having 1 to 6 carbon atoms is particularly preferred, and specific examples include lower alkyl groups such as methyl, ethyl, propyl, and isopropyl; cycloalkyl groups such as cyclohexyl; aryl groups such as phenyl, tolyl, and xylyl; aralkyl groups such as benzyl; olefinic alkyl groups such as vinyl and propenyl; or groups in which some or all of the hydrogen atoms of the above groups are replaced by halogen atoms, cyano groups, or the like, such as chloromethyl and cyanoethyl. More preferably, groups selected from the group consisting of methyl, ethyl, vinyl, and phenyl are preferred.
[0021] Further, the general structural formula of component B is (R 3 R 4 2SiO 1 / 2 )(R 3 R 4 2SiO 1 / 2 ) m (R 4 2SiO 2 / 2 ) n (SiO 4 / 2 ) x , where R 3 、R 4 are independently selected from unsubstituted or substituted monovalent hydrocarbon groups, m = 0 to 50, n = 0 to 6, x = 0.3 to 2, and m + n + x = 1 to 50; the monovalent hydrocarbon group is selected from a group with 1 to 10 carbon atoms, and R 3 and R 4 At least one of the groups is a Si-H bond. As monovalent hydrocarbon groups, groups having 1 to 6 carbon atoms are particularly preferred, including lower alkyl groups such as methyl, ethyl, propyl, and isopropyl; cycloalkyl groups such as cyclohexyl; aryl groups such as phenyl, tolyl, and xylyl; aralkyl groups such as benzyl; olefinic alkyl groups such as vinyl and propenyl; or groups in which some or all of the hydrogen atoms in the above groups are replaced by halogen atoms, cyano groups, or the like, such as chloromethyl and cyanoethyl. More preferably, groups selected from the group consisting of methyl, ethyl, and phenyl are preferred.
[0022] Furthermore, it also includes one or more of the following components: fluorescent agent, color paste, carbon black, color paste, titanium dioxide, inhibitor, fumed silica, silica powder, calcium powder, and aluminum hydroxide.
[0023] The beneficial effects of adopting the above-mentioned further technical solution are: adjusting the appearance color and detection function by adding fluorescent agents, carbon black, color paste, titanium dioxide, etc., and adding fluorescent agents can provide fluorescent detection function; adding fumed silica, silicon micropowder, calcium powder, aluminum hydroxide, etc. to adjust the strength and thixotropy; adding inhibitors, etc. to adjust the storage period and working time, adjust the curing speed, etc.
[0024] The second aspect of the present invention is to provide a method for preparing the above-mentioned organopolysiloxane composition, comprising the following steps: mixing component A, component C, and component D uniformly at room temperature, adding component B, and stirring uniformly to obtain the organopolysiloxane composition.
[0025] Another aspect of the present invention is to provide the use of the above-mentioned organopolysiloxane composition in the bonding and packaging of semiconductor chip heat dissipation cover plates.
[0026] Compared with the prior art, the present invention has the following technical effects: The invention provides a fast-strengthening organopolysiloxane composition, which is suitable for fast positioning and strengthening in a snap-cure process for semiconductor chip heat dissipation cover plates. The organopolysiloxane composition is a single-component composition that, through the combined action of a novel complex platinum catalyst and a low-temperature adhesion promoter, can rapidly bond and strengthen within 5-10 minutes at a temperature of 80°C or above, achieving more than 80% of full curing. The composition can also be maintained at room temperature for more than 48 hours. The organopolysiloxane composition can improve its anti-interference and anti-poisoning capabilities, and in the presence of flux or a water-cutting agent, the degree to which the bonding strength after the snap-cure process is affected is significantly reduced. DETAILED DESCRIPTION
[0027] The following is an explanation of the embodiments of the present invention by specific specific examples. Those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. Although the description of the present invention will be introduced in conjunction with the preferred embodiment, this does not mean that the features of this invention are limited to this embodiment. On the contrary, the purpose of introducing the invention in conjunction with the embodiment is to cover other options or modifications that may be extended based on the claims of the present invention. In order to provide a deep understanding of the present invention, the following description will contain many specific details. The present invention can also be implemented without using these details. In addition, in order to avoid confusion or blurring the focus of the present invention, some specific details will be omitted in the description. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.
[0028] In the following functional groups: Vi represents CH2=CH-, Me represents CH3-, and Ph represents phenyl.
[0029] Example 1: Preparation of complex platinum catalyst C1 2.5 g of Karstedt catalyst having a Pt content of 20% was added to 97.5 g of vinyl-terminated silicone oil having a viscosity of 100 mPa.s and diluted to a Pt content of 5000 ppm to obtain a mixed solution. Subsequently, 0.05 g of trimethoxyphosphine, 0.05 g of triethyl phosphite, and 1 g of tetravinyltetramethylcyclotetrasiloxane were added thereto, and the mixture was heated under reduced pressure at 60°C for 1 h to obtain a complex platinum catalyst C1.
[0030] Example 2: Preparation of complex platinum catalyst C2 1.5 g of Karstedt catalyst with a Pt content of 20% was added to 98.5 g of vinyl-terminated silicone oil with a viscosity of 200 mPa.s and diluted to a Pt content of 3000 ppm to obtain a mixed solution. Subsequently, 0.1 g of diethyl vinyl phosphate, 0.1 g of triisopropyl phosphite and 2 g of trivinylcyclohexasiloxane (ViMeSiO 2 / 2 )(Me2SiO 2 / 2 ), and heated at 70°C under reduced pressure for 2 h to obtain a complex platinum catalyst C2.
[0031] Example 3: Preparation of complex platinum catalyst C3 1.0 g of Karstedt catalyst with a Pt content of 20% was added to 99 g of vinyl-terminated silicone oil with a viscosity of 500 mPa.s and diluted to a Pt content of 2000 ppm to obtain a mixed solution. Subsequently, 0.3 g of vinyl (diphenylphosphinoethyl) dimethylsilane, 1.0 g of triisopropyl phosphite and 5 g of trivinyldiphenylcyclopentasiloxane (ViMeSiO 2 / 2 )3(MePhSiO 2 / 2 ) 2. Heat under reduced pressure at 80°C for 2 h to obtain a complex platinum catalyst C3.
[0032] Example 4: Preparation of Low-Temperature Adhesion Accelerator D1 0.5 mol of geraniol was subjected to high-temperature vacuum dehydration at 110°C. After dehydration, a mixed solution of 0.25 mol of tetramethylxylylene diisocyanate (TMXDI) and dehydrated toluene was added. Under nitrogen protection, the temperature was raised to 110°C and refluxed for 2 hours. After the reaction was completed, the temperature was lowered to below 80°C, 0.55 mol of 3-(2,3-epoxypropoxy)propyltrimethoxysilane was added, and the temperature was further raised to 120°C and refluxed for 6 hours. The toluene solvent was then removed by reduced pressure distillation to obtain a low-temperature adhesion promoter D1.
[0033] Example 5: Preparation of Low-Temperature Adhesion Accelerator D2 0.5 mol of geraniol was subjected to high-temperature vacuum dehydration at 110°C. After dehydration, a mixed solution of 0.25 mol of diphenylmethane diisocyanate (MDI) and dehydrated toluene was added. Under nitrogen protection, the temperature was raised to 110°C and refluxed for 1 hour. After the reaction was completed, the temperature was lowered to below 80°C, 0.65 mol of 3-(2,3-epoxypropoxy)propyltrimethoxysilane was added, and the temperature was further raised to 120°C and refluxed for 4 hours. The toluene solvent was then removed by reduced pressure distillation to obtain a low-temperature adhesion promoter D2.
[0034] Example 6: Organopolysiloxane composition I 20 parts of organopolysiloxane A1 (ViMe2SiO 1 / 2 ) 0.8 (Me3SiO 1 / 2 ) 0.2 (Me2SiO 2 / 2 )1(SiO 4 / 2 ) 0.8 and 20 parts of organopolysiloxane A3 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 100 mixture, 40 parts of organopolysiloxane A2 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 330 , 0.3 parts of complex platinum catalyst C1 and 2.0 parts of low-temperature adhesion promoter D1 were mixed uniformly at room temperature, and then 12.5 parts of organopolysiloxane B1 (HMe2SiO 1 / 2 )(SiO 4 / 2 ), and after being thoroughly stirred, a fast-strengthening organopolysiloxane composition I was obtained.
[0035] Example 7: Organopolysiloxane Composition II 50 parts of organopolysiloxane A2 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 330 、50 parts of organopolysiloxane A3 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 100 15 parts of hydrophobic fumed silica were mixed evenly at room temperature, 0.6 parts of complex platinum catalyst C2 and 2.5 parts of low-temperature adhesion promoter D2 were added thereto, and mixed evenly at room temperature. Finally, 1.02 parts of organopolysiloxane B1 (HMe2SiO 1 / 2 )(SiO 4 / 2 ) and 1.02 parts of organopolysiloxane B2 (Me3SiO 1 / 2 )(HMeSiO 2 / 2 )10 (Me2SiO 2 / 2 ) 20 After being thoroughly stirred, a fast-strengthening organopolysiloxane composition II is obtained.
[0036] Example 8: Organopolysiloxane Composition III 25 parts of organopolysiloxane A1 (ViMe2SiO 1 / 2 ) 0.8 (Me3SiO 1 / 2 ) 0.2 (Me2SiO 2 / 2 )1(SiO 4 / 2 ) 0.8 and 20 parts of organopolysiloxane A3 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 100 mixture, 45 parts of organopolysiloxane A2 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 330 , 1.0 part of complex platinum catalyst C3, 0.5 part of low-temperature adhesion promoter D1 and 1.0 part of low-temperature adhesion promoter D2 were mixed uniformly at room temperature, and then 10 parts of organopolysiloxane B1 (HMe2SiO 1 / 2 )(SiO 4 / 2 ) and 12.5 parts of organopolysiloxane B2 (Me3SiO 1 / 2 )(HMeSiO 2 / 2 ) 10 (Me2SiO 2 / 2 ) 20 After being thoroughly stirred, a fast-strengthening organopolysiloxane composition III is obtained.
[0037] Comparative Example 1 25 parts of organopolysiloxane A1 (ViMe2SiO 1 / 2 ) 0.8 (Me3SiO 1 / 2 ) 0.2 (Me2SiO 2 / 2 )1(SiO 4 / 2 ) 0.8 and 20 parts of organopolysiloxane A3 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 100 mixture, 45 parts of organopolysiloxane A2 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 3301.0 part of platinum catalyst (1.0 g of Karstedt catalyst with a Pt content of 20% was added to 99 g of 500 mPa.s vinyl-terminated silicone oil and diluted to a Pt content of 2000 ppm), 0.5 part of methyl butynol, and 1.5 parts of adhesion promoter (a prepolymer of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and vinyltrimethoxysilane in a 1:1 molar ratio) were mixed uniformly at room temperature, and then 10 parts of organopolysiloxane B1 (HMe2SiO 1 / 2 )(SiO 4 / 2 ) and 12.5 parts of organopolysiloxane B2 (Me3SiO 1 / 2 )(HMeSiO 2 / 2 ) 10 (Me2SiO 2 / 2 ) 20 , and stirred thoroughly to obtain the organopolysiloxane composition of Comparative Example 1.
[0038] Comparative Example 2 20 parts of organopolysiloxane A1 (ViMe2SiO 1 / 2 ) 0.8 (Me3SiO 1 / 2 ) 0.2 (Me2SiO 2 / 2 )1(SiO 4 / 2 ) 0.8 and 20 parts of organopolysiloxane A3 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 100 mixture, 40 parts of organopolysiloxane A2 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 330 , 0.3 parts of complex platinum catalyst C1, 1.0 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and 1.0 parts of 3-(methacryloyloxy)propyltrimethoxysilane were mixed uniformly at room temperature, and then 12.5 parts of organopolysiloxane B1 (HMe2SiO 1 / 2 )(SiO 4 / 2 ), and stirred thoroughly to obtain the organopolysiloxane composition of Comparative Example 2.
[0039] Comparative Example 3 20 parts of organopolysiloxane A1 (ViMe2SiO 1 / 2 ) 0.8 (Me3SiO 1 / 2 ) 0.2 (Me2SiO 2 / 2 )1(SiO 4 / 2 ) 0.8and 20 parts of organopolysiloxane A3 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 100 mixture, 40 parts of organopolysiloxane A2 (ViMe2SiO 1 / 2 )(Me2SiO 2 / 2 ) 330 , 0.3 parts of platinum catalyst (2.5 g of Karstedt catalyst with a Pt content of 20% was added to 97.5 g of vinyl-terminated silicone oil with a viscosity of 100 mPa.s and diluted to a Pt content of 5000 ppm), 0.5 parts of methyl butynol and 2.0 parts of low-temperature adhesion promoter D1 were mixed uniformly at room temperature, and then 12.5 parts of organopolysiloxane B1 (HMe2SiO 1 / 2 )(SiO 4 / 2 ), and stirred thoroughly to obtain the organopolysiloxane composition of Comparative Example 3.
[0040] Test sample preparation method: Snap-cure sample curing method: Dispense glue on a nickel-plated steel plate, add a gap wire (150μm) after dispensing, bond a PCB sample block (10mm*5mm), and then perform hot pressing curing at the required temperature, maintaining a hot pressing pressure of 1-1.5MPa.
[0041] Final curing sample processing method: Place the sample after the above snap-cure treatment in an oven and perform deep curing at 150℃*30min.
[0042] Special treatment samples: After spraying a thin layer of flux and water-cutting agent on the sample (nickel-plated steel plate and PCB board), wipe it with a dust-free cloth, and then perform glue dispensing and hot pressing curing.
[0043] The specific test results are shown in Table 1.
[0044] Table 1 Performance test results of organopolysiloxane compositions of Examples and Comparative Examples
[0045] Test results demonstrate that the organopolysiloxane composition of the present invention exhibits rapid bond strength development, achieving over 80% of full cure within 5-10 minutes at temperatures of 80°C or above. The composition can also maintain a working life of over 48 hours at room temperature. Furthermore, in the presence of influencing factors such as flux and water-cutting agents, the organopolysiloxane composition of the present invention exhibits minimal degradation in snap-cure strength, remaining relatively stable and meeting basic bonding requirements.
[0046] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. An organopolysiloxane composition, characterized in that According to parts by weight, it includes the following components: Component A: 80-100 parts of an organopolysiloxane containing at least two alkenyl groups per molecule; Component B: 2-25 parts of an organopolysiloxane containing at least two Si-H bonds per molecule; Component C: complex platinum catalyst, 0.001-2 parts; Component D: low temperature adhesion promoter, 0.5-5 parts.
2. The organopolysiloxane composition according to claim 1, wherein The preparation method of component C includes the following steps: adding a Karstedt catalyst to vinyl-terminated silicone oil and diluting it to a Pt content of 1000-10000 ppm to obtain a mixed solution; then, adding a certain amount of a phosphorus-containing compound and a polyvinyl cyclic siloxane as a source of complexing ligand to the mixed solution; and treating the mixed solution under reduced pressure at 60-80°C for 0.5-4 hours to obtain the complexing platinum catalyst.
3. The organopolysiloxane composition according to claim 2, characterized in that The Karstedt catalyst is C8H 18 OPtSi2, the pressure of the decompression treatment is ≤-0.09MPa, and the viscosity of the vinyl-terminated silicone oil is ≤1000mPa.s; the addition amount of the phosphorus-containing compound is 0.2‰-2% of the mass of the mixed liquid, and the addition amount of the polyvinyl cyclic siloxane is 0‰-5% of the mass of the mixed liquid; the phosphorus-containing compound includes any one or more of vinyl diethyl phosphate, vinyl (diphenylphosphinoethyl) dimethyl silane, triisopropyl phosphite, trimethoxyphosphine, and triethyl phosphite.
4. The organopolysiloxane composition according to claim 2, characterized in that The polyvinyl cyclic siloxane contains at least 4 Si-O structural units, and the general structural formula of the polyvinyl cyclic siloxane is ((CH2=CH)R 5 SiO 2 / 2 )(R 5 2SiO 2 / 2 ) y , R 5 is selected from unsubstituted or substituted monovalent hydrocarbon groups, y=0~1.
0.
5. The organopolysiloxane composition according to claim 1, wherein The preparation method of component D includes the following steps: dehydrating geraniol under high temperature and vacuum, then adding a mixed solution of tetramethylxylylene diisocyanate (TMXDI) or diphenylmethane diisocyanate (MDI) and dehydrated toluene, heating the mixture to 100-120°C under nitrogen protection and reflux reaction for 1-4 hours, cooling the mixture to below 80°C after the reaction, adding 3-(2,3-epoxypropoxy)propyltrimethoxysilane, continuing to heat the mixture to 100-120°C and reflux reaction for 2-8 hours, and then removing the toluene solvent by reduced pressure distillation to obtain the low-temperature adhesion promoter.
6. The organopolysiloxane composition according to claim 5, characterized in that The molar ratio of the geraniol to tetramethylxylene diisocyanate or diphenylmethane diisocyanate is 2:1, the mass ratio of tetramethylxylene diisocyanate or diphenylmethane diisocyanate to dehydrated toluene is 1:1, and the molar ratio of 3-(2,3-epoxypropoxy)propyltrimethoxysilane to geraniol is 1-1.5:
1.
7. The organopolysiloxane composition according to claim 1, wherein The general structural formula of component A is (R 1 R 2 2SiO 1 / 2 )(R 1 R 2 SiO 2 / 2 ) a (R 2 SiO 3 / 2 ) b (SiO 4 / 2 ) c , where R 1 、R 2 are independently selected from unsubstituted or substituted monovalent hydrocarbon groups, a = 0 to 400 (excluding 0), b = 0 to 2, c = 0 to 2, and a+b+c = 1 to 400; the monovalent hydrocarbon group is selected from a group with 1 to 10 carbon atoms, and R 1 and R 2 At least one of the groups is a vinyl group; The general structural formula of component B is (R 3 R 4 2SiO 1 / 2 )(R 3 R 4 2SiO 1 / 2 ) m (R 4 2SiO 2 / 2 ) n (SiO 4 / 2 ) x , where R 3 、R 4 are independently selected from unsubstituted or substituted monovalent hydrocarbon groups, m = 0 to 50, n = 0 to 6, x = 0.3 to 2, and m + n + x = 1 to 50; the monovalent hydrocarbon group is selected from a group with 1 to 10 carbon atoms, and R 3 and R 4 At least one of the groups is a Si-H bond.
8. The organopolysiloxane composition according to claim 1, wherein It also includes one or more of the following components: fluorescent agent, color paste, carbon black, color paste, titanium dioxide, inhibitor, fumed silica, silica powder, calcium powder, and aluminum hydroxide.
9. A method for preparing the organopolysiloxane composition according to any one of claims 1 to 8, characterized in that: The method comprises the following steps: mixing component A, component C and component D uniformly at room temperature, adding component B, and stirring uniformly to obtain the organopolysiloxane composition.
10. Use of the organopolysiloxane composition according to any one of claims 1 to 8 in bonding and packaging semiconductor chip heat dissipation cover plates.