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Preparation method of atomic oxygen-resistant polyimide hybrid films containing POSS (polyhedral oligomeric silsesquioxanes) structures

An anti-atomic oxide polyimide and thin film preparation technology, applied in the direction of silicon organic compounds, can solve the problems of uneven thermal expansion coefficient of coating and film, difficult large-scale production of thin film, and discounted service life of thin film, etc., to achieve effective It is beneficial to large-scale industrial production, improving the anti-atomic oxygen performance, and the effect of improving the anti-atomic oxygen performance

Inactive Publication Date: 2012-10-17
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method avoids the erosion of the base layer film by atomic oxygen to a certain extent, the impact of microfluidics and high-energy charged particles on the coating in space will cause cracks and even fall off the film surface. Once the coating is lost, the base layer The film is exposed, and under the attack of atomic oxygen, serious "corrosion" phenomenon occurs, which greatly reduces the service life of the film.
Secondly, the coating is easily damaged during processing, folding, loading and unloading, etc., and limited by the current spraying process, it is difficult to mass-produce a large-area film; thirdly, the coating is an inorganic component, so the film and coating There is an interface layer in the layer, and good adhesion is difficult to achieve, and the thermal expansion coefficient of the coating and the film is not uniform, and it is easy to generate internal stress at the interface, thereby deteriorating the performance of the film

Method used

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  • Preparation method of atomic oxygen-resistant polyimide hybrid films containing POSS (polyhedral oligomeric silsesquioxanes) structures
  • Preparation method of atomic oxygen-resistant polyimide hybrid films containing POSS (polyhedral oligomeric silsesquioxanes) structures
  • Preparation method of atomic oxygen-resistant polyimide hybrid films containing POSS (polyhedral oligomeric silsesquioxanes) structures

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Add 250mL of ethanol, 12mL of distilled water and 3mL of TEAOH (methanol solution with a mass fraction of 25%) in sequence into a container equipped with an electric stirrer, a condenser and a thermometer, and at the same time start stirring and raise the temperature of the system. When the temperature rose to 50°C, a mixture of 5.50 mL of γ-aminopropyltriethoxysilane and 14.18 mL of phenyltriethoxysilane was added to the system in Step 1 within 2 hours. After the addition, keep the reaction conditions unchanged and continue to stir for 50h. After the reaction, the solvent was evaporated, the product was washed 3 to 5 times with distilled water, centrifuged, and freeze-dried to obtain a white powdery solid, that is, diamine POSS.

Embodiment 2

[0035] Example 2: Add 210mL of methanol, 10mL of distilled water and 2.5mL of TMAOH (methanol solution with a mass fraction of 25%) to a container equipped with an electric stirrer, a condenser tube and a thermometer in sequence, and at the same time start stirring and raise the temperature of the system. When the temperature rose to 40°C, a mixture of 4.06 mL of γ-aminopropyltrimethoxysilane and 10.74 mL of phenyltrimethoxysilane was added to the system in Step 1 within 2 hours. After the addition, keep the reaction conditions unchanged and continue to stir for 40h. After the reaction, the solvent was evaporated, the product was washed 3 to 5 times with distilled water, centrifuged, and freeze-dried to obtain a white powdery solid, that is, diamine POSS.

Embodiment 3

[0036] Example 3: Add 220mL of methanol, 10mL of distilled water and 2.5mL of TEAOH (methanol solution with a mass fraction of 25%) into a container equipped with an electric stirrer, a condenser tube and a thermometer in sequence, start stirring and raise the temperature of the system at the same time. When the temperature rose to 45°C, a mixture of 4.15 mL of γ-aminopropyltrimethoxysilane and 14.18 mL of phenyltriethoxysilane was added to the system in Step 1 within 2 hours. After the addition, keep the reaction conditions unchanged and continue to stir for 45h. After the reaction, the solvent was evaporated, the product was washed 3 to 5 times with distilled water, centrifuged, and freeze-dried to obtain a white powdery solid, that is, diamine POSS.

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Abstract

The invention relates to a preparation method of atomic oxygen-resistant polyimide hybrid films containing POSS structures. The preparation method comprises the following steps: reacting phenyl-containing monomers with aminopropyl-containing silane monomers in an alcohol / water cosolvent system under the action of a catalyst, volatilizing the solvent, washing, lyophilizing to obtain diamine POSS, modifying a polyimide material with the diamine POSS to prepare polyamide acid containing the POSS structure, and carrying out thermal imidization to obtain a series of polyimide hybrid films with different contents of the diamine POSS. Reaction conditions for synthesizing the diamine POSS are mild, the cost is low, and the POSS structure is introduced to the main chain of a polyimide molecule in a chemical bond manner, so the polyimide material has an excellent intrinsic atomic oxygen resistance, the hybrid films have excellent comprehensive performances, and the atomic oxygen resistances of the hybrid films are 6 times higher than that of unmodified Kapton polyimide films, thereby the hybrid films of the invention have important meanings to the development of the aviation and space industry.

Description

technical field [0001] The invention relates to a method for preparing an anti-atomic oxygen polyimide hybrid film containing a POSS structure, and relates to the preparation of bisaminopropylhexaphenyl octapolycage silsesquioxane (diamine POSS) and the preparation of POSS-containing Fabrication of Structural Antiatomic Oxygen Polyimide Hybrid Films. Background technique [0002] With the rapid development of science and technology, the development of space technology puts forward more and more requirements for materials. The spacecraft must have excellent anti-atomic oxygen performance if it is to operate in an environment with high atomic oxygen content such as low earth orbit (LEO) without being damaged. Polyimide has become an important class of materials in the aerospace industry due to its excellent thermal properties, mechanical properties, solvent resistance and dielectric properties, but the erosion of atomic oxygen makes the service life of unmodified polyimide ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10C07F7/21
Inventor 张秋禹雷星锋张和鹏厉向杰张宝亮范新龙陈营李伟
Owner NORTHWESTERN POLYTECHNICAL UNIV
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