Low-temperature curable low-modulus low-stress adhesive for optical modules and preparation method thereof
By using a method for preparing composite epoxy resin and modified fillers, the problems of high-temperature damage, stress concentration, and mismatch of expansion coefficients in optical module adhesive materials have been solved, enabling the application of low-temperature curing, low-modulus, and low-stress adhesives, thereby improving the stability and reliability of optical modules.
Patent Information
- Application Number
- CN202511186826.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-25
- Publication Date
- 2025-11-11
- Estimated Expiration
- 2045-08-25
AI Technical Summary
Existing optical module bonding materials are prone to damaging heat-sensitive components during high-temperature curing. They also have high modulus and high stress, leading to stress concentration and a mismatch in the material's coefficient of thermal expansion, which affects the stability and reliability of the optical module.
A low-temperature curing, low-modulus, low-stress adhesive was prepared by combining bisphenol F type epoxy resin and organosilicon modified epoxy resin, along with plasma-treated hollow glass microspheres and silane coupling agent-treated nano-silica, and introducing DOPO grafted modified composite filler. This improved the interfacial compatibility and flame retardant properties.
It achieves low-temperature curing while reducing the modulus and stress of the adhesive, improving adhesion and flame retardant properties with various materials, making it suitable for precision bonding of optical modules and enhancing the stability and reliability of optical modules.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of adhesive technology, specifically relating to a low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method. Background Technology
[0002] With the rapid development of information technology, optical fiber communication technology plays a crucial role in data transmission, network communication, and other fields. As the core component of an optical fiber communication system, the optical module performs photoelectric signal conversion and is widely used in high-frequency scenarios such as data centers, 5G, and AI computing power. Its performance and reliability directly affect the operating efficiency and stability of the entire communication system. The internal structure of an optical module is complex, containing various materials with significantly different physical and chemical properties, such as plastics, glass, ceramics, metals, PCB boards, and various electronic components. The high-density packaging requirements inevitably place extremely high performance demands on the bonding materials.
[0003] Currently, traditional adhesives face the following problems in the manufacturing and assembly of optical modules: 1) High curing temperature: Most high-performance adhesives require curing at temperatures above 150°C, which can easily damage heat-sensitive components (such as DFB lasers); 2) High modulus and high stress: Traditional adhesives typically have high modulus and stress after curing, which may lead to stress concentration inside the optical module, causing deformation or damage to components and affecting the long-term stability of the optical module; 3) Large coefficient of thermal expansion: The coefficients of thermal expansion of different materials inside the optical module vary greatly. The coefficient of thermal expansion of traditional adhesives does not match these materials, resulting in stress accumulation during thermal cycling, leading to cracking of the ceramic / glass substrate or failure of fiber coupling.
[0004] Therefore, there is an urgent need for a low-temperature curable, low-modulus, low-stress adhesive for optical modules, which aims to solve the above-mentioned problems of existing adhesive materials, improve the overall performance of the adhesive, enable it to have good adhesion to a variety of materials, and meet the growing market demand. Summary of the Invention
[0005] To address the existing technical problems, the present invention aims to provide a low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method. The adhesive of the present invention can cure within a wide temperature range of 80℃ to 150℃, and simultaneously possesses the characteristics of low modulus, low stress, and ultra-low coefficient of thermal expansion. It exhibits good adhesion to plastics, glass ceramics, metals, PCB boards, electronic components, etc., and is suitable for bonding and protecting microelectronic and optical devices.
[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0007] The present invention provides a low-temperature curable, low-modulus, low-stress adhesive for optical modules, comprising the following raw materials by weight: 10-20 parts of a first epoxy resin, 5-15 parts of a second epoxy resin, 60-80 parts of a modified filler, and 5-30 parts of an amine curing agent; wherein the second epoxy resin is an organosilicon-modified epoxy resin.
[0008] In some embodiments of the present invention, the first epoxy resin is a bisphenol F type epoxy resin and / or a bisphenol E type epoxy resin.
[0009] Preferably, the first epoxy resin is a bisphenol F type epoxy resin.
[0010] In some embodiments of the present invention, the method for preparing the second epoxy resin includes the following steps:
[0011] Q1. Mix 3-(methacryloyloxy)propyltrimethoxysilane, di(methacryloyloxyethyloxy)diphenylsilane and toluene and add them to a reaction vessel. Stir, add azobisisobutyronitrile and n-dodecyl mercaptan, heat to react, separate, dry and obtain the reactants.
[0012] Q2. Mix the reactants obtained in step Q1, toluene, and ethanol, stir, add dilute hydrochloric acid solution, stir and control the temperature at 25-30℃ for 1-2 hours, adjust the pH to neutral, and distill under reduced pressure to obtain organosilicon compounds.
[0013] Q3. Add maleic anhydride and triethylamine to bisphenol A epoxy resin and stir at 80-100℃ for 1-2 hours to obtain pretreated bisphenol A epoxy resin.
[0014] Q4. Mix the organosilicon compound obtained in step Q2 with the pretreated bisphenol A epoxy resin obtained in step Q3, stir, and then add tetrabutyl titanate and xylene in sequence. Under an inert gas protective atmosphere, heat and react in stages, and then distill under reduced pressure to obtain the second epoxy resin.
[0015] In some embodiments of the present invention, the mass ratio of 3-(methacryloyloxy)propyltrimethoxysilane to di(methacryloyloxyethyloxy)diphenylsilane in step Q1 is (1.6-2.2):1.
[0016] In some embodiments of the present invention, the mass ratio of the organosilicon compound and the pretreated bisphenol A epoxy resin in step Q4 is 1:(3-4).
[0017] In step Q4 of this invention, the specific operation of the staged heating reaction is as follows: first heat to 75-85℃ for 1-1.5h, then raise the temperature to 120-125℃ for 3-5h.
[0018] Epoxy resin adhesives are widely used in many fields due to their excellent bonding performance, good mechanical properties, and chemical stability. However, epoxy resin adhesives themselves have problems such as high shrinkage rate after curing, high brittleness, and poor flame retardancy. To solve these problems, this invention uses composite epoxy resins, namely bisphenol F type epoxy resin and silicone-modified epoxy resin.
[0019] This invention uses a specific mass ratio of 3-(methacryloyloxy)propyltrimethoxysilane and bis(methacryloyloxyethyloxy)diphenylsilane as raw materials to prepare organosilicon compounds. This not only introduces a low-modulus organosilicon structure, improving the resin's flexibility, but also makes the curing process more stable, further reducing stress and shrinkage. This is crucial for the bonding and protection of precision microelectronic and optical devices such as optical modules, as excessive stress and shrinkage can lead to device damage or cracking at the bonding site. Simultaneously, the modified second epoxy resin improves the interfacial compatibility between the epoxy adhesive and various materials, enhancing adhesion. Furthermore, the second epoxy resin may form a synergistic "silicon-nitrogen-phosphorus" mechanism with the modified filler, improving flame retardant properties.
[0020] In some embodiments of the present invention, the method for preparing the modified filler includes the following steps:
[0021] P1. The hollow glass microspheres are immersed in acetone with continuous stirring during immersion, filtered, washed, dried, and then subjected to plasma treatment to obtain plasma-treated hollow glass microspheres.
[0022] P2. Mix nano-silica, vinyl silane coupling agent, anhydrous ethanol, and water, adjust the pH to acidic, heat to 50-70℃ and react for 3-5 hours, wash, and dry to obtain silanized silica;
[0023] P3. Mix the plasma-enhanced hollow glass microspheres obtained in step P1, the silanized silica obtained in step P2, and anhydrous ethanol, stir, and dry to obtain the composite filler.
[0024] P4. Mix the composite filler obtained in step P3, DOPO, and AIBN, and heat to 80-110℃ for 4-8 hours under an inert gas protective atmosphere. Centrifuge, wash, and dry to obtain the modified filler.
[0025] In some embodiments of the present invention, the D50 particle size of the nano-silica in step P2 is 20-80 nm.
[0026] In some embodiments of the present invention, the mass ratio of silanized silicon dioxide to plasma-enhanced hollow glass microspheres in step P3 is 1:(0.1-0.4).
[0027] In some embodiments of the present invention, the mass ratio of the composite filler and DOPO in step P4 is 10:(1-1.5).
[0028] In step P1 of this invention, the solid-liquid ratio of the hollow glass microspheres to acetone is not emphasized; it is only necessary to ensure that the hollow glass microspheres are completely immersed in acetone throughout the impregnation process.
[0029] In step P2 of this invention, the reagents used to adjust the pH to acidity include, but are not limited to, glacial acetic acid.
[0030] One of the main functions of silica in epoxy resin-based composites is to significantly reduce the coefficient of thermal expansion (CTE). Uniformly dispersing silica fillers within the epoxy resin matrix can effectively limit chain segment movement and volume expansion during heating, thereby reducing the overall CTE of the adhesive to a level compatible with electronic components. However, silica is prone to poor dispersibility in epoxy resin systems; furthermore, solely using silica as a modifier filler may actually increase the modulus of the adhesive.
[0031] Good interfacial bonding can effectively transfer stress, improve the mechanical properties of adhesives, and help reduce CTE and modulus. This invention not only introduces hydroxyl / carboxyl groups onto the surface of hollow glass microspheres through plasma treatment, but also treats nano-silica with a silane coupling agent. This surface treatment forms a strong "bridge" between the filler and epoxy resin, significantly improving interfacial bonding strength, enhancing filler dispersibility, and reducing interfacial defects. Simultaneously, the surface-treated plasma-treated hollow glass microspheres and silanized silica interact under high-speed stirring, improving the compatibility and dispersion stability of the two particles (compared to their original state), enhancing the physical bonding force between particles, and facilitating subsequent grafting modification.
[0032] In addition, epoxy resin is a relatively flammable material, which is not conducive to its use in microelectronics, optical devices, and other similar applications. Furthermore, using silica and hollow glass microspheres alone can only provide synergistic flame retardancy to a certain extent, and cannot independently impart a V-0 rating to epoxy adhesives. Therefore, the applicant improved the flame retardancy of the epoxy resin system by introducing DOPO grafted modified composite filler, resulting in low smoke and halogen-free properties.
[0033] In some embodiments of the present invention, the amine curing agent is a latent amine curing agent.
[0034] Another aspect of the present invention provides a method for preparing a low-temperature curable, low-modulus, low-stress adhesive for optical modules, comprising the following steps:
[0035] S1. Add the first epoxy resin and the second epoxy resin to the reactor and stir. Then add the modified filler, stir, degas, and obtain the mixture.
[0036] S2. Add an amine curing agent to the mixture obtained in step S1, stir, and degas to obtain the adhesive. In this invention, the curing temperature of the epoxy adhesive is 80℃~150℃, and the curing time is 15-60min.
[0037] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0038] 1. This invention uses bisphenol F type epoxy resin and organosilicon modified epoxy resin as a composite. The specific organosilicon compound improves flexibility, reduces curing stress and shrinkage, enhances interfacial compatibility and adhesion, and may also enhance flame retardant properties, making it suitable for precision devices such as optical modules.
[0039] 2. This invention improves the interfacial bonding between the filler and epoxy resin by treating hollow glass microspheres with plasma and treating nano-silica with silane coupling agent, thereby enhancing dispersibility and compatibility and reducing the coefficient of thermal expansion and modulus; at the same time, it introduces DOPO grafted modified composite filler to improve flame retardant performance. Detailed Implementation
[0040] The present invention will be described below with reference to specific embodiments. It should be noted that the following embodiments are examples of the present invention and are used only to illustrate the invention, not to limit it. Other combinations and various modifications within the scope of the present invention can be made without departing from its spirit or scope.
[0041] Each adhesive was prepared according to the proportions and preparation methods of the raw materials specified in the following examples and comparative examples.
[0042] To facilitate implementation of this invention by those skilled in the art, the manufacturers of some raw materials for the embodiments and comparative examples are described below:
[0043] Bisphenol A type epoxy resin: model E-51;
[0044] Bisphenol F type epoxy resin: model DER354;
[0045] Latent amine curing agent: Model ADEKA EH-4357S;
[0046] The D50 particle size of nano-silica is 50nm and 150nm;
[0047] Unless otherwise specified, all other raw materials can be purchased from the market.
[0048] Preparation Example 1
[0049] The preparation method of the second epoxy resin A includes the following preparation steps:
[0050] Q1. Mix 38g of 3-(methacryloyloxy)propyltrimethoxysilane, 20g of bis(methacryloyloxyethyloxy)diphenylsilane, and 100g of toluene in a reaction vessel and stir until homogeneous. Under nitrogen protection, add 0.3g of azobisisobutyronitrile and 1.2g of n-dodecyl mercaptan, heat to 75°C and keep reacting for 6 hours. Cool to room temperature, precipitate with methanol at -5°C, remove the upper solvent, and dry under vacuum at 85°C to constant weight to obtain the reactant.
[0051] Q2. Mix 10g of reactant obtained in step Q1, 50mL of toluene and 10mL of ethanol, stir well, add 50mL of 2wt% dilute hydrochloric acid solution, stir and control the temperature at 25℃ for 2h, adjust the pH to neutral, separate with a separatory funnel, and distill the organic phase under reduced pressure to obtain organosilicon compounds.
[0052] Q3. Add 1.5g of maleic anhydride and 0.15g of triethylamine to 100g of bisphenol A epoxy resin, stir and react at 90℃ for 1.5h to obtain pretreated bisphenol A epoxy resin.
[0053] Q4. Mix 10g of organosilicon compound obtained in step Q2 with 35g of pretreated bisphenol A epoxy resin obtained in step Q3, stir evenly, then add 0.5g of tetrabutyl titanate and 40g of xylene in sequence. Under nitrogen protection, stir at 400rpm for 10min, heat to 80℃ and react for 1.5h, then heat to 120℃ and react for 4.5h. Distill under reduced pressure to obtain the second epoxy resin A.
[0054] Preparation Example 2
[0055] The preparation method of the second epoxy resin B is the same as that of Preparation Example 1, except that the amount of 3-(methacryloyloxy)propyltrimethoxysilane added in step Q1 is 28g.
[0056] Preparation Example 3
[0057] The preparation method of the second epoxy resin C is the same as that of Preparation Example 1, except that the amount of pretreated bisphenol A type epoxy resin added in step Q4 is 45g.
[0058] Preparation Example 4
[0059] The preparation method of modified filler A includes the following preparation steps:
[0060] P1. The hollow glass microspheres were immersed in acetone and stirred continuously for 12 hours. After filtration, the microspheres were washed twice with deionized water, dried at 85°C for 6 hours, and then placed in a vacuum plasma treatment instrument for 1 hour at a vacuum of 500 Pa and a flow rate of 80 mL / min to obtain plasma-enhanced hollow glass microspheres.
[0061] P2. Mix 30g of nano-silica (50nm), 6g of vinyltriethoxysilane, 900mL of anhydrous ethanol and 100mL of water, adjust the pH to 4, heat to 60℃ and react for 4h, wash twice with anhydrous ethanol, and dry at 85℃ for 6h to obtain silanized silica.
[0062] P3. Mix 6.25g of plasma-enhanced hollow glass microspheres obtained in step P1, 25g of silanized silica obtained in step P2, and 285mL of anhydrous ethanol, stir at 1000rpm for 45min at 25℃, and vacuum dry at 85℃ for 6h to obtain composite filler.
[0063] P4. Mix 20g of composite filler, 2g of DOPO and 0.15g of AIBN obtained in step P3, heat to 95℃ for 6h under nitrogen atmosphere, centrifuge, wash 3 times with toluene, and vacuum dry at 85℃ for 8h to obtain modified filler A.
[0064] Preparation Example 5
[0065] The preparation method of modified filler B is the same as that of preparation example 4, except that the amount of isionized hollow glass microspheres added in step P3 is 1.75g.
[0066] Preparation Example 6
[0067] The preparation method of modified filler C is the same as that of preparation example 4, except that the particle size of nano silica in step P2 is replaced with 150 nm.
[0068] Example 1
[0069] A low-temperature curable, low-modulus, low-stress adhesive for optical modules comprises the following raw materials by weight: 15 parts of bisphenol F type epoxy resin, 10 parts of second epoxy resin A, 70 parts of modified filler A, and 18 parts of latent amine curing agent.
[0070] The method for preparing the adhesive in this embodiment includes the following steps:
[0071] S1. Add the first epoxy resin and the second epoxy resin A to the reactor and stir evenly. Then add the modified filler A, stir evenly, degas, and obtain the mixture.
[0072] S2. Add an amine curing agent to the mixture obtained in step S1, stir evenly, degas, and obtain the adhesive.
[0073] Example 2
[0074] A low-temperature curable, low-modulus, low-stress adhesive for optical modules comprises the following raw materials by weight: 10 parts of bisphenol F type epoxy resin, 5 parts of second epoxy resin A, 60 parts of modified filler A, and 5 parts of latent amine curing agent.
[0075] The method for preparing the adhesive in this embodiment is the same as in Embodiment 1.
[0076] Example 3
[0077] A low-temperature curable, low-modulus, low-stress adhesive for optical modules comprises the following raw materials by weight: 20 parts of bisphenol F type epoxy resin, 15 parts of second epoxy resin A, 80 parts of modified filler A, and 30 parts of latent amine curing agent.
[0078] The method for preparing the adhesive in this embodiment is the same as in Embodiment 1.
[0079] Example 4
[0080] A low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method are disclosed. The specific implementation method is the same as in Example 1, except that an equal amount of second epoxy resin B is used to replace second epoxy resin A.
[0081] Example 5
[0082] A low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method are disclosed. The specific implementation method is the same as in Example 1, except that an equal amount of second epoxy resin C is used to replace second epoxy resin A.
[0083] Example 6
[0084] A low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method are disclosed. The specific implementation method is the same as in Example 1, except that an equal amount of modified filler B is used instead of modified filler A.
[0085] Example 7
[0086] A low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method are disclosed. The specific implementation method is the same as in Example 1, except that an equal amount of modified filler C is used instead of modified filler A.
[0087] Comparative Example 1
[0088] A low-temperature curable, low-modulus, low-stress adhesive for optical modules and its preparation method are disclosed. The specific implementation method is the same as in Example 1, except that an equal amount of filler is used to replace the modified filler A. The filler is composed of commercially available hollow glass microspheres and nano-silica (50nm) mixed in a mass ratio of 1:4.
[0089] Effect evaluation:
[0090] The adhesives prepared in Examples 1-7 and Comparative Example 1 were tested and analyzed. The specific results are shown in Table 1. The adhesives prepared in Examples 1-3 were tested and analyzed for shear strength. The specific results are shown in Table 2.
[0091] Performance testing:
[0092] (1) Curing volume shrinkage rate: Referring to GB / T 24148.9-2014 "Plastic Unsaturated Polyester Resin (UP-R) Part 9: Determination of Total Volume Shrinkage Rate", the test was conducted according to the company's internal testing standard XB-QCT-017, specifically as follows:
[0093] a. Prepare solid glue blocks with a single weight of 1g using adhesive. Weigh the glue blocks in air and in distilled water respectively using the density balance method, w(fl), where ρ(fl) is the liquid density of the adhesive.
[0094] b. Use the formula ρv = w(a) / (w(a) - w(fl)) to calculate the density of the solid glue block.
[0095] c. Calculate the volume shrinkage rate of the adhesive Sv = (ρv-ρ(fl))ρv*100;
[0096] (2) Coefficient of thermal expansion: Referring to GB / T 36800.2-2018 "Thermomechanical Analysis of Plastics (TMA) Part 2: Determination of linear coefficient of thermal expansion and glass transition temperature", the test was conducted according to the company's internal testing standard XB-QCT-019, specifically as follows:
[0097] a. Apply the adhesive sample into the customized mold, cure at 120℃@30min, and then polish to ensure that the upper and lower surfaces are flat;
[0098] b. Test the sample using TMA equipment;
[0099] c. Calculate the linear thermal expansion coefficient α = ΔL / (L0·ΔT) using software, where α represents the linear expansion coefficient, ΔL is the length change, L0 is the initial length, and ΔT is the temperature change;
[0100] Table 1
[0101]
[0102] (3) Shear strength: Referring to GB / T 7124-2008 "Determination of Tensile Shear Strength of Adhesives (Rigid Material to Rigid Material)", the initial shear strength, PCT (110℃, 100%RH)@24h shear strength, and 120℃@1000h shear strength were tested according to the company's internal testing standard XB-QCT-016. Specifically:
[0103] a. The test substrate is an AL-AL lap joint. A standard aluminum sheet (100mm*27.9mm*1.5mm) is polished and then the surface to be bonded is cleaned with a cleaning solvent.
[0104] b. Weigh 8mg of adhesive sample onto the bonding surface, place a 100μm copper wire as a spacer to set the adhesive layer thickness, then cover it with another aluminum sheet, press it tightly, and finally fix it with a clip. Curing is carried out at 120℃@30min, and then left at room temperature for 24h.
[0105] c. Use a microcomputer universal testing machine to test the shear force of the sample. After the aluminum sheet is pulled apart, use a micrometer to measure the actual area of the adhesive layer.
[0106] d. Calculate tensile shear strength = breaking force (Newtons) / adhesive layer area (mm²) 2 For PCT (110℃, 100%RH)@24h shear strength, the shear strength is measured after curing and then high temperature and high humidity treatment for 24h, followed by 24h at room temperature, and then measured in the same manner as above; for 120℃@1000h shear strength, the shear strength is measured after curing and then high temperature treatment for 1000h, followed by 24h at room temperature, and then measured in the same manner as above.
[0107] Table 2
[0108]
[0109] As can be seen from the results in Table 1-2, the adhesives prepared in Examples 1-3 have the characteristics of low modulus, low stress and ultra-low coefficient of expansion, good adhesion to microelectronic and optical devices, and still have good shear strength even after high-temperature aging.
[0110] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present application in any way. Although the present application discloses the preferred embodiment as described above, it is not intended to limit the present application. Any changes or modifications made by those skilled in the art without departing from the scope of the technical solution of the present application using the disclosed technical content are equivalent to equivalent implementation cases. Any simple modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the scope of the technical solution of the present invention are still within the scope of the technical solution.
Claims
1. A low-temperature curable, low-modulus, low-stress adhesive for optical modules, characterized in that, By weight, it comprises the following raw materials: 10-20 parts of first epoxy resin, 5-15 parts of second epoxy resin, 60-80 parts of modified filler, and 5-30 parts of amine curing agent; wherein... The first epoxy resin is bisphenol F type epoxy resin and / or bisphenol E type epoxy resin; The second epoxy resin is an organosilicon-modified epoxy resin, and the specific preparation method includes the following steps: Q1. 3-(methacryloyloxy)propyltrimethoxysilane, di(methacryloyloxyethyloxy)diphenylsilane, and toluene are mixed and added to a reaction vessel, stirred, and then azobisisobutyronitrile and n-dodecyl mercaptan are added. The mixture is heated to react, separated, and dried to obtain the reactant. The mass ratio of 3-(methacryloyloxy)propyltrimethoxysilane to di(methacryloyloxyethyloxy)diphenylsilane in step Q1 is (1.6-2.2):
1. Q2. Mix the reactants obtained in step Q1, toluene, and ethanol, stir, add dilute hydrochloric acid solution, stir and control the temperature at 25-30℃ for 1-2 hours, adjust the pH to neutral, and distill under reduced pressure to obtain organosilicon compounds. Q3. Add maleic anhydride and triethylamine to bisphenol A epoxy resin and stir at 80-100℃ for 1-2 hours to obtain pretreated bisphenol A epoxy resin. Q4. Mix the organosilicon compound obtained in step Q2 with the pretreated bisphenol A epoxy resin obtained in step Q3, stir, and then add tetrabutyl titanate and xylene in sequence. Under an inert gas protective atmosphere, heat and react in stages, and then distill under reduced pressure to obtain the second epoxy resin. The method for preparing the modified filler includes the following steps: P1. The hollow glass microspheres are immersed in acetone with continuous stirring during immersion, filtered, washed, dried, and then subjected to plasma treatment to obtain plasma-treated hollow glass microspheres. P2. Mix nano-silica, vinyl silane coupling agent, anhydrous ethanol, and water, adjust the pH to acidic, heat to 50-70℃ and react for 3-5 hours, wash, and dry to obtain silanized silica; P3. Mix the plasma-enhanced hollow glass microspheres obtained in step P1, the silanized silica obtained in step P2, and anhydrous ethanol, stir, and dry to obtain a composite filler. P4. Mix the composite filler obtained in step P3, DOPO, and AIBN, and heat to 80-110℃ for 4-8 hours under an inert gas protective atmosphere. Centrifuge, wash, and dry to obtain the modified filler.
2. The low-temperature curable, low-modulus, low-stress adhesive for optical modules according to claim 1, characterized in that, The mass ratio of the organosilicon compound and the pretreated bisphenol A epoxy resin in step Q4 is 1:(3-4).
3. The low-temperature curable, low-modulus, low-stress adhesive for optical modules according to claim 1, characterized in that, The D50 particle size of the nano-silica mentioned in step P2 is 20-80 nm.
4. The low-temperature curable, low-modulus, low-stress adhesive for optical modules according to claim 1, characterized in that, The mass ratio of silanized silica to plasma-enhanced hollow glass microspheres in step P3 is 1:(0.1-0.4).
5. The low-temperature curable, low-modulus, low-stress adhesive for optical modules according to claim 1, characterized in that, The amine curing agent is a latent amine curing agent.
6. A method for preparing a low-temperature curable, low-modulus, low-stress adhesive for optical modules according to any one of claims 1-5, characterized in that, It includes the following steps: S1. Add the first epoxy resin and the second epoxy resin to the reactor and stir. Then add the modified filler, stir, degas, and obtain the mixture. S2. Add an amine curing agent to the mixture obtained in step S1, stir, degas, and obtain an adhesive.
Citation Information
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