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Preparation method of modified silicon dioxide-epoxy resin composite slurry

A technology of epoxy resin and silica, applied in the direction of epoxy resin glue, adhesive type, adhesive additive, etc., can solve the problem of high viscosity of composite slurry, achieve good sphericity, good dispersion, crosslinking high density effect

Inactive Publication Date: 2022-04-08
XILONG SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects in the prior art and provide a method for preparing modified silica-epoxy resin slurry, which uses one pot to complete the preparation of silica and in-situ surface modification to improve the The grafting rate of functional groups on the silicon surface to solve the problem that the existing silica fillers will cause too high viscosity of the composite slurry when the particle size is small and the filling amount is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A. Preparation of modified silica

[0026] Weigh 30g of ammonia water with a concentration of 28wt%, 1000g of ethanol, and 200g of deionized water into a 3L kettle, start stirring, and add 80g of tetraethyl orthosilicate and 0.2g of methyltrimethoxysilane at a constant speed at a stirring speed of 150rpm , the dropping time is 20 minutes, after the dropwise addition is completed, the temperature is raised to 40°C, and the constant temperature is reacted for 3 hours; the temperature is continued to be raised to 60°C, and 50g of bis(3-triethoxysilylpropane) containing 2.5g is added dropwise to the reaction system base) amine and 2.5g of N,N-bis(3-trimethoxysilylpropyl)urea ethanol solution, reacted for 2.5 hours to obtain in-situ modified silica solution, and the modified silica solution was sequentially used Centrifuge in a centrifuge, wash with ethanol / water solvent, repeat the cycle 3 times, and then bake in a drying oven at 120°C for 11 hours to obtain in-situ modifie...

Embodiment 2

[0032] A. Preparation of modified silica

[0033]Weigh 15g of tetramethylammonium hydroxide with a concentration of 25wt%, add 1000g of ethanol, and 200g of deionized water into a 3L kettle, start stirring, and add 80g of tetraethyl orthosilicate and 0.2g of formazan at a constant speed at a stirring speed of 150rpm. Trimethoxysilane, the dropping time is 20 minutes. After the dropping is completed, the temperature is raised to 40°C, and the constant temperature reaction is carried out for 3 hours; the temperature is continued to be raised to 60°C, and 50g silylpropyl)amine and 2.5g of N,N-bis(3-trimethoxysilylpropyl)urea ethanol solution, reacted for 2.5 hours to obtain in-situ modified silica solution, the modified di The silicon oxide solution was centrifuged in a centrifuge, washed with ethanol / water solvent, repeated 3 times, and then baked in a drying oven at 120°C for 11 hours to obtain in-situ modified silicon dioxide powder;

[0034] B. Preparation of modified silica...

Embodiment 3

[0039] A. Preparation of modified silica

[0040] Weigh 30g of tetramethylammonium hydroxide with a concentration of 25wt%, add 1000g of ethanol and 200g of deionized water into a 3L kettle, start stirring, and add 80g of tetraethyl orthosilicate and 0.2g of formazan at a constant speed at a stirring speed of 150rpm. Trimethoxysilane, the dropping time is 20 minutes. After the dropping is completed, the temperature is raised to 40°C, and the temperature is reacted for 3 hours; the temperature is continued to rise to 60°C, and 50g of bis(triethoxysilane base) ethylene and 2.5g of N,N-bis(3-trimethoxysilylpropyl)urea ethanol solution, reacted for 2.5 hours to obtain the in-situ modified silica solution, and the modified silica solution was sequentially used Centrifuge in a centrifuge, wash with ethanol / water solvent, repeat the cycle 3 times, and then bake in a drying oven at 120°C for 12 hours to obtain in-situ modified silica powder;

[0041] B. Preparation of modified silica...

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PUM

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Abstract

The invention provides a preparation method of modified silicon dioxide-epoxy resin slurry, which comprises the following steps: adding an alkaline substance into a mixed solvent of alcohol and water, dropwise adding tetraethoxysilane and methyltrimethoxysilane, then adding at least two biped silane coupling agents, washing and drying to obtain in-situ modified silicon dioxide powder; adding the prepared silicon dioxide powder into an epoxy resin matrix prepared from epoxy resin and ethylene glycol diglycidyl ether, uniformly mixing by using a high-speed mixer, and removing bubbles to obtain the modified silicon dioxide-epoxy resin composite slurry. The preparation and surface in-situ modification of silicon dioxide are completed in one pot, the grafting rate of functional groups on the surface of silicon dioxide is increased, the problem that the viscosity of composite slurry is too high when existing silicon dioxide filler is small in particle size and high in filling amount is solved, and the epoxy resin composite slurry is ideal in the field of electronic packaging.

Description

technical field [0001] The invention belongs to the technical field of polymer composite materials, and in particular relates to a preparation method of a modified silicon dioxide-epoxy resin composite slurry used as an underfill glue in a semiconductor packaging process. Background technique [0002] Silica has excellent characteristics such as low thermal expansion coefficient, small stress, high heat resistance, high moisture resistance, and high hardness, so it is used as a key filler in bottom filling rubber materials. As one of the key electronic materials in the semiconductor packaging process, the underfill can reduce the thermal expansion coefficient mismatch between the chip and the substrate, protect the solder balls, provide adhesion, etc., and provide stress matching after chip packaging, Mechanical protection, reliability, etc. play a vital role. [0003] With the development of society, people's requirements for the performance and size of electronic equipmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J163/00C09J11/04C09J163/02
Inventor 张念椿阳后桂梅园尹彬赵书煌张慕伸兰芳郑鹤立郑安丽
Owner XILONG SCI CO LTD
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