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Method for preparing elemental oxygen-resistant polyimide material by in-situ hydrolysis method

An oxygen polyimide film and polyimide technology are applied in the field of preparing atomic oxygen-resistant polyimide materials by an in-situ hydrolysis method, achieving the effects of easy conditions, wide application range and compact structure

Active Publication Date: 2018-12-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the deficiencies of existing materials and technologies, and provide a method for preparing atomic oxygen-resistant polyimide materials by in-situ hydrolysis

Method used

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  • Method for preparing elemental oxygen-resistant polyimide material by in-situ hydrolysis method
  • Method for preparing elemental oxygen-resistant polyimide material by in-situ hydrolysis method
  • Method for preparing elemental oxygen-resistant polyimide material by in-situ hydrolysis method

Examples

Experimental program
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Effect test

Embodiment 1

[0028]The atomic oxygen resistant polyimide film material of PMDA / ODA system was prepared. (1) Weigh 2.0g of pyromellitic dianhydride (PMDA) and 1.8g of 4,4'-diaminodiphenyl ether (ODA) with a molar ratio of 1:1, and dissolve all ODA in 30ml of N,N - Dimethylformamide (DMF) solvent, mechanical stirring, after ODA is completely dissolved in DMF, under the condition of ice-water bath, add PMDA step by step, after obtaining the polyamic acid (PAA) solution with moderate viscosity, mechanical stirring 2h Finally, add 40wt% tetraethyl orthosilicate (TEOS) based on the weight of the polyamic acid by dropping, and stir to obtain a uniform mixed solution; The compound solution was made into a thin film, and placed at room temperature for 24 hours; (3) the polyamic acid film was placed in a hot furnace, and the temperature was gradually raised to 300 ° C at a heating rate of 5 ° C / min, and kept for 0.5 h; (4) The polyamic acid film is placed in the airtight container that contains a...

Embodiment 2

[0030] The atomic oxygen resistant polyimide film material of PMDA / ODA system was prepared. (1) Weigh 2.0g of pyromellitic dianhydride (PMDA) and 1.8g of 4,4'-diaminodiphenyl ether (ODA) with a molar ratio of 1:1, and dissolve all ODA in 30ml of N,N - Dimethylformamide (DMF) solvent, mechanical stirring, after ODA is completely dissolved in DMF, under the condition of ice-water bath, add PMDA step by step, after obtaining the polyamic acid (PAA) solution with moderate viscosity, mechanical stirring 2h Finally, add tetraethyl orthosilicate (TEOS) based on 60wt% of the polyamic acid weight by dropping, and stir to obtain a uniform mixed solution; (2) adopt the above-mentioned polyamic acid / silicon The compound solution was made into a thin film, and placed at room temperature for 12 hours; (3) the polyamic acid film was placed in a hot furnace, and the temperature was gradually raised to 300 ° C at a heating rate of 3 ° C / min, and kept for 1 h; (4) the The polyamic acid film ...

Embodiment 3

[0032] The atomic oxygen resistant polyimide film material of BPDA / PDA system was prepared. (1) Weigh 2.82g of 3,3'4,4'-biphenyltetracarboxylic dianhydride (BPDA) and 1.02g of p-phenylenediamine (PDA) with a molar ratio of 1:1, and dissolve all the PDA in 30ml of N, N-dimethylacetamide (DMAc) solvent, mechanical stirring, after PDA is all dissolved in DMAc, under the condition of ice-water bath, add BPDA step by step, after obtaining the polyamic acid (PAA) solution with moderate viscosity, After mechanical stirring for 2 hours, add 40wt% tetraethyl orthosilicate (TEOS) based on the weight of polyamic acid by dropwise addition, and stir to obtain a uniform mixed solution; The acid / silicon compound solution was used to form a thin film, and placed at room temperature for 12 hours; (3) the polyamic acid film was placed in a heating furnace, and the temperature was gradually raised to 300°C at a heating rate of 5°C / min, and kept for 0.5h; (4) The polyamic acid film is hydrolyzed...

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Abstract

The invention relates to a method for preparing an elemental oxygen-resistant polyimide material by an in-situ hydrolysis method, the prepared polyimide material is composed of SiO2 and polyimide, andhas structural characteristic of compact SiO2 layer @(SiO2 / PI interpenetrating network layer) @(SiO2 particle / PI hybrid layer), the polyimide material has a three-stage anti-atomic oxygen function, and is excellent in atomic oxygen-resistant performance. The preparation method of the material comprises the following steps: a silicon compound is added to a polyamic acid solution, the materials arestirred to form a uniform mixed solution, and then subjected to casting film formation, pre-cyclization and heat-induced migration aggregation, in-situ hydrolysis and high-temperature heat treatment,and finally the elemental oxygen-resistant polyimide material is obtained. The method of the invention has simple implementation process and convenient conditions, and is suitable for polyimide of all systems, and the obtained elemental oxygen-resistant polyimide film layer material has the advantages of compact structure, no cracking and excellent interfacial bonding property.

Description

technical field [0001] The invention belongs to the technical field of polyimide films, and in particular relates to a method for preparing an atomic oxygen-resistant polyimide material by an in-situ hydrolysis method. Background technique [0002] Polyimide (PI) film is a kind of aromatic heterocyclic polymer material with excellent comprehensive properties. , has become one of the indispensable high-performance materials in the aerospace field, and has been widely used in thermal control materials for space vehicles, flexible substrates for lightweight solar cell arrays, and insulating protective layers for circuit systems. [0003] However, space vehicles such as space stations, spacecraft, space shuttles, and most satellites mainly operate in low earth orbit (Low Earth Orbit, LEO), and one of the main components in this environment is atomic oxygen (atomic oxygen) with strong oxidizing ability. ). The spacecraft is running in LEO at high speed for a long time, so the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K3/36C08J5/18
CPCC08J5/18C08J2379/08C08K3/36
Inventor 齐胜利董国庆王芮晗田国峰武德珍
Owner BEIJING UNIV OF CHEM TECH
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