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

AI Technical Summary

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 mat

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

Example Embodiment

[0027] Example 1

[0028] (1) Dissolve 2.94g 3,3,4',4'-bipyromellitic dianhydride in 55.86g N,N-dimethylformamide (DMF) under the protection of nitrogen at room temperature. The solid content is 5%, stir for 5 hours to obtain 3,3,4',4'-bipyromellitic dianhydride solution;

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

[0030] (3) The diaminopolysiloxane tetrahydrofuran solution was slowly added dropwise to the 3,3,4',4'-bipyromellitic dianhydride solution, and after stirring for 6 hours, 1.82g 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, pressurize it to 0.14 MP...

Example Embodiment

[0038] Example 2

[0039] (1) Dissolve 2.94g 3,3,4',4'-bipyromellitic dianhydride in 14.70g N,N-dimethylacetamide (DMAc) under the protection of nitrogen at room temperature. The solid content is 20%, stirring under nitrogen for 3 hours to obtain 3,3,4',4'-bipyromellitic dianhydride solution;

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

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

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

Example Embodiment

[0046] Example 3

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

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

[0049] (3) The diaminopolysiloxane tetrahydrofuran solution was slowly added dropwise to the aromatic tetraacid dianhydride solution, and after stirring for 4 hours, 3.46g of 2,2-bis[4-(4-aminobenzene) was added. (Oxy)phenyl]propane and 31.14g of 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 to an autoclave, replace ...

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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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