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Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof

A silicon oxidation polyimide, polyimide technology, applied in the direction of chemical instruments and methods, flat products, other household appliances, etc., can solve the problem of increased material adhesion, cold welding phenomenon has not been better resolved, and affects Problems such as the normal function of the spacecraft mechanism, to achieve the effect of excellent product performance and controllable process conditions

Active Publication Date: 2018-03-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The occurrence of cold welding seriously affects the normal function of the spacecraft mechanism, and even leads to flight accidents
[0004] In recent years, Japan has developed polyimide-co-siloxane anti-atomic oxygen materials, which exhibit excellent anti-atomic oxygen properties, but due to the introduction of siloxane, the adhesion of the material has been greatly increased. The phenomenon of cold welding has not been better resolved

Method used

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  • Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof
  • Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof
  • Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) At room temperature and under the protection of nitrogen, 2.94g 3,3,4',4'-biphenyltetraacid dianhydride was dissolved in 55.86g N,N-dimethylformamide (DMF), and the solid content was 5%, stirred for 5 hours to obtain 3,3,4',4'-biphenyltetraacid dianhydride solution;

[0029] (2) Under nitrogen protection, 0.78 g of diaminopolysiloxane with a molecular weight of 860 was dissolved in 14.82 g of tetrahydrofuran with a solid content of 5%, and stirred for 5 hours to obtain a diaminopolysiloxane tetrahydrofuran solution;

[0030] (3) Slowly add the diaminopolysiloxane tetrahydrofuran solution dropwise into the 3,3,4',4'-biphenyltetraacid dianhydride solution, stir for 6 hours and then add 1.82g of 4,4 '-diaminodiphenyl ether and 34.58g N,N-dimethylformamide (DMF), stirred for 4 hours to obtain oligomeric polyamic acid siloxane solution 1;

[0031] (4) Transfer the oligomeric polyamic acid-co-siloxane solution 1 into an autoclave, replace the air with nitrogen, pressuriz...

Embodiment 2

[0039] (1) Dissolve 2.94g of 3,3,4',4'-biphenyltetralic acid dianhydride in 14.70g of N,N-dimethylacetamide (DMAc) at room temperature and under the protection of nitrogen, with a solid content of 20%, stirred for 3 hours under nitrogen to obtain a solution of 3,3,4',4'-biphenyltetralic acid dianhydride;

[0040] (2) Under the protection of nitrogen, 21 g of diaminopolysiloxane with a molecular weight of 2100 was dissolved in 84 g of tetrahydrofuran with a solid content of 20%, and stirred for 3 hours under nitrogen to obtain a solution of diaminopolysiloxane in tetrahydrofuran;

[0041] (3) Slowly add the diaminopolysiloxane tetrahydrofuran solution dropwise into the aromatic tetraacid dianhydride solution to obtain oligomeric polyamic acid-co-siloxane solution 2;

[0042] (4) Transfer the oligomeric polyamic acid-co-siloxane solution 2 into an autoclave, replace the air with nitrogen, pressurize to 0.14MPa, keep at 60°C for 3 hours, and keep at 100°C for 3 hours, Cool to ro...

Embodiment 3

[0047] (1) At room temperature and under the protection of nitrogen, 2.18g of pyromellitic dianhydride was dissolved in 19.08g of N-methylpyrrolidone (NMP), with a solid content of 10%, and stirred for 4h under nitrogen to obtain a pyromellitic dianhydride solution ;

[0048] (2) Under the protection of nitrogen, 1.48g of diaminopolysiloxane with a molecular weight of 950 was dissolved in 13.32g of tetrahydrofuran with a solid content of 10%, and stirred for 4 hours under nitrogen to obtain diaminopolysiloxane tetrahydrofuran solution ;

[0049] (3) Slowly add the diaminopolysiloxane tetrahydrofuran solution dropwise into the aromatic tetraacid dianhydride solution, stir for 4 hours and add 3.46g of 2,2-bis[4-(4-aminobenzene Oxygen) phenyl] propane and 31.14g N-methylpyrrolidone (NMP), stirred for 4 hours to obtain oligomeric polyamic acid-co-siloxane solution 3;

[0050] (4) Transfer the oligomeric polyamic acid-co-siloxane solution 3 into an autoclave, replace the air with...

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Abstract

The invention discloses a surface silicon oxidation polyimide-co-silane thin film and a preparation method and belongs to the technical field of polyimide preparation. The invention provides the surface silicon oxidation polyimide-co-silane thin film. The preparation method comprises the following steps: firstly, preparing polyimide-co-silane by adopting a temperature raising and pressurizing method on the basis of a traditional two-step preparation method; and secondly, forming a glass-like functional layer on the surface by controlling conditions and adopting atomic oxygen equipment. The surface silicon oxidation polyimide-co-silane thin film consists of three parts, namely a glass layer, a transition layer and a substrate layer, wherein the glass layer consists of a silicon-oxygen structure, the transition layer consists of the silicon-oxygen structure and the polyimide-co-silane and the substrate layer consists of the polyimide-co-silane. The surface silicon oxidation polyimide-co-silane thin film, disclosed by the invention, has the advantages of excellent atomic oxygen resistance and capability of self-healing. The glass-like functional layer avoids the occurrence of a cold welding phenomenon.

Description

technical field [0001] The invention relates to the technical field of polyimide preparation, in particular to a surface silicon oxidation polyimide-co-siloxane film and a preparation method thereof. Background technique [0002] After the completion of the space shuttle mission in 1981, a special phenomenon was discovered during the visual inspection of the staff: a significant change occurred on the surface of the thermal control pad of a TV camera made of polyimide film material. The glossy, transparent amber film prior to flight turns a translucent pale yellow. After research, it was found that it was the result of atomic oxygen erosion. Atomic oxygen has begun to attract the attention of the aerospace industry. Researchers from various countries have conducted a lot of research on the mechanism of interaction between atomic oxygen and materials, and have developed different types of anti-atomic oxygen materials. [0003] Silicone resin-based coating materials have exc...

Claims

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Application Information

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IPC IPC(8): B32B17/10B32B9/04B32B27/28C08G77/455C08J3/28B29D7/01
Inventor 陈春海王春博姜勃弛周宏伟赵晓刚王大明
Owner JILIN UNIV
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