Prepn of lateral hydroxyl group containing polyimide/SiO2 hybrid film

The technology of hydroxyl side polyimide and hydroxyl side polyamic acid is applied in the field of synthesis and preparation of organic-inorganic hybrid materials, and can solve the problem of enlargement, mutual agglomeration, the transparency of hybrid materials, the decline of mechanical properties, etc. problem, to achieve the effect of improved dimensional stability, improved tensile strength, and improved Young's modulus

Inactive Publication Date: 2003-08-20
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] Previous research results have shown that when the content of silicon dioxide in ordinary polyimide / silica hybrid materials is greater than 8%, the hybrid film is no longer transparent due to phase separation, and the size of the inorganic phase reaches several microns; The particle size of the silica phase increases further with the increase of the content of inorganic components, and there is a tendency to agglomerate with each other, and obvious phase separation occurs, which further reduces the transparency and mechanical properties of the hybrid material.

Method used

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Examples

Experimental program
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Effect test

Embodiment

[0030] 1. Add 274 grams of 1,3-di(4-amino)phenoxy-2-propanol into an appropriate amount of N-methylpyrrolidone, stir to dissolve it, then add 220 grams of pyromellitic dianhydride, Control the mass percent concentration of the solution to about 6%, protect it under nitrogen, and stir in an ice bath at -5 to 0°C for 10 hours to obtain a light yellow viscous liquid, which is a polyamic acid solution containing alcoholic hydroxyl side groups.

[0031] Add 23.6 grams of glycidoxypropyltrimethoxysilane and 1 gram of N,N-dimethylbenzylamine to the above polyamic acid solution containing hydroxyl side groups, react at 120°C for 4 hours, cool to room temperature, and then Add 250 grams of tetraethoxysilane, stir for 6 hours, and use the casting method to coat the film. Under the negative pressure of 0.09-0.1atm, treat at 60°C for 12 hours, 160°C for 2 hours, and 200°C for 2 hours. After treatment at 260°C for 1 hour and at 300°C for 0.5 hour, a polyimide / silicon dioxide hybrid film co...

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PUM

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Abstract

The preparation process of lateral hydroxyl group containing polyimide/SiO2 hybrid film includes dissolving polyamido acid containing lateral hydroxyl group or polyimide in 1-1400 portions in solvent to compound 5-15 % concentration solution, adding silane coupling agent containing epoxy radical in 0-250 portions for reaction at 120-150 deg.c in the presence of catalyst in 0.1-10 portions of 2-4 hr; cooling to room temperature, adding n-silicate ester in 1-1000 portions through stirring for 6-24 hr, flow casting to form film, and processing at 0.1 atm negative pressure and 60 deg.c for 12 hr, and 160 deg.C for 2 hr, at 200 deg.c for 2 hr, at 260 deg.c for 1 hr and at 300 deg.c for 0.5 hr to obtain the lateral hydroxyl group containing polyimide/SiO2 hybrid film.

Description

1. Technical field [0001] The invention relates to a method for preparing a polyimide / silicon dioxide hybrid film containing hydroxyl side groups, and belongs to the field of synthesis and preparation of organic-inorganic hybrid materials. 2. Background technology [0002] In recent years, with the wide application of large-scale integrated circuits and ultra-large-scale integrated circuits, electronic and electrical products are developing towards miniaturization, integration, high power and high reliability, and higher requirements are placed on the performance of polyimide. In addition to the characteristics of high temperature resistance, small dielectric constant, good electrical insulation, and good film-forming properties, materials are also required to have low thermal expansion, low water absorption, low polarization, high strength, high modulus, and chemical resistance. Good performance. The overall performance of ordinary polyimide is difficult to meet the above ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08K3/34C08L79/08
Inventor 顾宜黄毅王劲刘习奎汤嘉陵盛兆碧
Owner SICHUAN UNIV
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