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Cross-linked polyimide film, preparation method and applications thereof

A polyimide film, cross-linked technology, applied in the field of cross-linked polyimide film and its preparation, can solve the problems of low dielectric constant, high strength and high modulus, etc. Effects of electrical constant, lower thermal expansion coefficient, and higher strength

Active Publication Date: 2020-01-31
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a new cross-linked polyimide film in order to overcome the problem that the low thermal expansion coefficient, low dielectric constant and high strength and high modulus of the polyimide film in the prior art cannot be combined. Thin film and its preparation method

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  • Cross-linked polyimide film, preparation method and applications thereof
  • Cross-linked polyimide film, preparation method and applications thereof
  • Cross-linked polyimide film, preparation method and applications thereof

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preparation example Construction

[0019] The invention provides a kind of preparation method of cross-linked polyimide film, and this method comprises the following steps:

[0020] (1) In the presence of a solvent, the dianhydride and the diamine are subjected to polycondensation reaction to obtain a linear polyamic acid solution;

[0021] (2) under the conditions of the polycondensation reaction, adding an amino compound to the linear polyamic acid solution to obtain a cross-linked polyamic acid solution, the amino compound has more than 3 amino groups;

[0022] (3) the cross-linked polyamic acid solution is formed into a polyamic acid film;

[0023] (4) carry out imidization reaction with described polyamic acid film, obtain cross-linked polyimide film;

[0024] Wherein, based on the total molar weight of the dianhydride, diamine and amino compound, the molar fraction of the amino compound is 0.01%-3%.

[0025] In the present invention, in step (1), the molar ratio of the acid anhydride groups in the dianh...

Embodiment 1

[0056] Weigh 0.9862g (4.925mmol) of ODA, dissolve it in 20mL N'N-dimethylacetamide, and add 2.2434g (5.05mmol) 6FDA to the aforementioned system in six batches for polycondensation reaction at 0°C, wherein , each feeding time interval is 10min, total reaction 12h, until the intrinsic viscosity of the solution is 1.3dL / g, add 0.5% TAPOB accounting for the total moles of reaction monomers, continue the reaction for 1h, and prepare a cross-linked polyamic acid solution .

[0057] The cross-linked polyamic acid solution was left to defoam, evenly coated on the glass substrate, dried at room temperature, and then heated to 300 °C at a heating rate of 5 °C / min to obtain a cross-linked polyimide film, recorded as 6FDA / ODA / TAPOB-PI-0.5%-300.

Embodiment 2-6

[0061] Weigh 0.1002g (5mmol), 0.9862g (4.925mmol), 0.9712g (4.85mmol), 0.9561g (4.775mmol), 0.9111g (4.55mmol) ODA respectively, dissolve in 20mL N'N-dimethylacetamide At 0°C, 1.1015g (5.05mmol) PMDA was added into the aforementioned system in six batches for polycondensation reaction. The time interval between each feeding was 10min, and the total reaction was 12h. After the solution had a certain viscosity, the linear polyamic acid solution The intrinsic viscosity is 1.2-2dL / g, and TAPOB is added at 0.01%, 0.5%, 1%, 1.5%, 3% of the total molar weight of the reaction monomers, and the reaction is continued for 1 hour to prepare a cross-linked polyamic acid solution.

[0062] The cross-linked polyamic acid solution was left to defoam, evenly coated on the glass substrate, dried at room temperature, and heated to 320 °C at a heating rate of 1 °C / min to obtain 5 kinds of cross-linked polyimide films, respectively recorded PMDA / ODA / TAPOB-PI-0.01%-320, PMDA / ODA / TAPOB-PI-0.5%-320, ...

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Abstract

The invention relates to the field of high-performance film materials, and discloses a cross-linked polyimide film, a preparation method and applications thereof. The preparation method comprises: ina reaction system formed by condensation polymerization of dianhydride and diamine, adding an amino compound, and carrying out a continuous reaction to obtain a cross-linked polyamic acid solution, wherein the amino compound has more than 3 amino groups; forming a polyamic acid film from the obtained cross-linked polyamic acid solution; and carrying out an imidization reaction to obtain the cross-linked polyimide film. According to the invention, the cross-linked polyimide film prepared by the method has properties of high strength, high modulus, low expansion coefficient and low dielectric constant.

Description

technical field [0001] The invention relates to the field of high-performance film materials, in particular to a cross-linked polyimide film and its preparation method and application. Background technique [0002] Polyimide (PI) has excellent high temperature resistance, mechanical properties, insulation properties, corrosion resistance, radiation resistance and other performance characteristics due to its unique aromatic heterocyclic rigid structure. The resins and films produced from it as raw materials , fibers, composite materials, etc. have been widely used in the fields of electronics, machinery manufacturing, aerospace and other fields. In recent years, with the rapid development of miniaturization, thinning, multi-layering, high integration and special functionalization of electronic and optoelectronic display devices, higher requirements have been put forward for PI films: such as high strength, high modulus , high dimensional stability, low dielectric constant an...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08G73/10C08L79/08
CPCC08J5/18C08G73/1071C08G73/1039C08J2379/08
Inventor 田国峰周涵武德珍齐胜利
Owner BEIJING UNIV OF CHEM TECH
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