Preparation method for transparent polyimide/silicon dioxide hybrid film

A technology of transparent polyimide and silicon dioxide, which is applied in the field of polymer materials, can solve the problems that it is difficult to meet the basic requirements of transparent materials, limit the application of polyimide, and low light transmittance, and achieve excellent light transmittance, High light transmittance, high dispersion effect

Inactive Publication Date: 2012-08-01
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These polyimide / silicon dioxide hybrid films are generally dark in color, and the light transmittance is still low, which is difficult to meet the basic requirements of transparent materials, which greatly limits the application of polyimide in the field of optoelectronics.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] The preparation method of the transparent polyimide / silicon dioxide hybrid film that the present invention proposes comprises the following steps:

[0014] (1) equimolar 2,2'-bis(trifluoromethyl)diaminobiphenyl and 4,4'-bis(3-aminophenoxy)diphenylsulfone are dissolved in a polar solvent, and Stir to dissolve at room temperature, then add 4,4'-(hexafluoroisopropylene) diphthalic anhydride, the addition ratio is: 4,4'-(hexafluoroisopropylene) diphthalic anhydride and 2,2'-bis(trifluoro The molar ratio of methyl) diaminobiphenyl is (2.1~2.8): 1, stirring reaction 12 hours, obtain polyamic acid solution, wherein the consumption of polar solvent is 20wt% by the solid content in the polyamic acid solution calculate;

[0015] (2) Add 3-aminopropyltriethoxysilane in the polyamic acid solution of the above-mentioned step (1), and the addition ratio is: the content of the 3-aminopropyltriethoxysilane is as high as that in the above-mentioned step (1). 4, 5 mol% to 50 mol% of th...

Embodiment 1

[0020] Dissolve 2.88g (0.009mol) of 2,2'-bis(trifluoromethyl)diaminobiphenyl and 3.89g (0.009mol) of 4,4'-bis(3-aminophenoxy)diphenylsulfone in In 75g of N-methyl-2-pyrrolidone, after being completely dissolved, add 10g (0.023mol) 4,4'-(hexafluoroisopropene) diphthalic anhydride to the above solution at room temperature, stir for 12 hours, add 1.99g ( 0.009mol) 3-aminopropyltriethoxysilane, stirred for 6 hours to obtain a polyamic acid solution containing siloxane end groups, then added 2.86g orthosilicate ethyl ester and 1.88g of 0.1mol / L hydrochloric acid, continue to stir and react for 6 hours to obtain a mixed solution. After the reaction, spread the mixed solution on a flat plate, then dry at 80°C for 2 hours, cure at 150°C for 1 hour, cure at 250°C for 1 hour, and cure at 300°C for 1 hour. Hours, after cooling down to room temperature, the plate was placed in water to peel off the film to obtain a transparent polyimide / silicon dioxide hybrid film.

[0021] The polyimid...

Embodiment 2

[0023] Dissolve 2.88g (0.009mol) of 2,2'-bis(trifluoromethyl)diaminobiphenyl and 3.89g (0.009mol) of 4,4'-bis(3-aminophenoxy)diphenylsulfone in In 75g of N,N-dimethylformamide, after being completely dissolved, add 10g (0.023mol) 4,4'-(hexafluoroisopropylene) diphthalic anhydride to the above solution at room temperature, stir for 12 hours, add 1.99g (0.009mol) 3-aminopropyltriethoxysilane, stirred for 6 hours to obtain a polyamic acid solution containing siloxane end groups, then added 5.72g orthosilicate ethyl ester and 1.88g of 0.1mol / L hydrochloric acid, continue to stir and react for 6 hours to obtain a mixed solution. After the reaction, spread the mixed solution on a flat plate, then dry at 80°C for 2 hours, cure at 150°C for 1 hour, cure at 250°C for 1 hour, and cure at 300°C After cooling down to room temperature for 1 hour, the plate was placed in water to peel off the film to obtain a transparent polyimide / silicon dioxide hybrid film.

[0024] The polyimide / silico...

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Abstract

The invention relates to a preparation method for a transparent polyimide / silicon dioxide hybrid film, which belongs to the technical field of high polymer materials. The method includes the steps: dissolving 2, 2'-bis(trifluormethyl) benzidine and 4, 4'-bis(3-aminophenoxy) diphenyl sulfone, which serve as diamine monomer, into polar solvent; adding 4, 4'-(hexafluoroisopropylidene) diphthalic anhydride serving as dianhydride monomer; mixing to carry out polycondensation at the room temperature; then adding 3-aminopropyltriethoxysilane for continuous reaction to obtain siloxane-terminated polyamide acid solution; adding tetraethyl orthosilicate and hydrochloric acid into the solution for sol-gel reaction; and subjecting the mixed solution to film spreading and gradual curing to obtain thetransparent hybrid film. Silicon dioxide in the polyimide / silicon dioxide hybrid film is high in dispersity and avoids phase separation, and the transparent polyimide / silicon dioxide hybrid film is excellent in light transmission, mechanical property and heat resistance, and is suitable for use as protecting films for flexible display screens and optical devices and substrate materials for transparent conducting films.

Description

technical field [0001] The invention relates to a preparation method of a transparent polyimide / silicon dioxide hybrid film, belonging to the technical field of polymer materials. Background technique [0002] Polyimide has excellent mechanical properties, heat resistance, low temperature resistance, flame retardancy, solvent resistance and electrical properties, and can be used as structural composite materials, electrical insulation materials, adhesives and coating materials, and is widely used in electronic micro Electronics, aerospace, optics, electromechanical and other fields. Especially in the field of microelectronics, polyimide is often used as a dielectric layer for interlayer insulation, as a buffer layer to reduce stress, as a protective layer to reduce environmental damage, and as a shielding layer to reduce device errors. Used in various electronic components such as substrates of flexible printed wiring circuits and alignment films for liquid crystal displays...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08K3/36
Inventor 王晓工王兴元和亚宁金成九
Owner TSINGHUA UNIV
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