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A kind of polyimide film material with high adhesion and low linear expansion coefficient and preparation method thereof

A technology of polyimide film and linear expansion coefficient, which is applied in the field of polymer material synthesis, can solve the problems of low polyimide, poor bonding, and can only achieve low thermal expansion coefficient and improve adhesion performance , the effect of good dimensional stability

Inactive Publication Date: 2017-11-07
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the application process of polyimide, it is often encountered that polyimide falls off from the surface of the substrate (substrate), and situations such as poor bonding occur, which seriously affects the service life of the polyimide material, and Some unnecessary economic losses have been caused. In order to solve such problems, heteroatoms such as O, S, N, P, etc. can be introduced into the polyimide main chain; cyano group; it can also appropriately increase the proportion of flexible groups in the main chain of polyimide to properly improve the adhesion problem, while ensuring other excellent properties of polyimide, such as thermal stability, chemical stability, mechanical performance etc. is not compromised
[0004] In recent years, polyimide has begun to show its potential and wide application value in the field of flexible printed circuit board (FPC) and self-adhesive tape (TAB) technology and flexible solar cell substrate, while its core flexible copper clad laminate requires polymer It has high adhesion to the substrate and its own low linear expansion coefficient, but so far no polyimide with high adhesion and low linear expansion coefficient has been reported
According to existing literature reports, two types of biphenyls, 1,4-bis(2-cyano-4-aminophenoxy)benzene and 1,4-bis(4-aminophenoxy)biphenyl, have been synthesized. Amine monomers, and polymerized with a series of anhydride monomers to form polyimides with different properties, but according to the performance of the test, the former diamine monomer has a strong adhesion GB 0 level, but for linear expansion The improvement of the coefficient (CTE) is not obvious (CTE>80ppm / K), although the latter diamine monomer can moderately reduce the value of the linear expansion coefficient (CTE≥40ppm / K), but the adhesion can only reach GB 2 and below

Method used

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  • A kind of polyimide film material with high adhesion and low linear expansion coefficient and preparation method thereof
  • A kind of polyimide film material with high adhesion and low linear expansion coefficient and preparation method thereof
  • A kind of polyimide film material with high adhesion and low linear expansion coefficient and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0053] 1) Preparation of nitro compounds

[0054] Add biphenol 18.6207g (0.1mol), 2-chloro-5-nitrobenzonitrile 38.3384g ( 0.21mol), anhydrous K2CO 3 16.5847g (0.12mol), 141ml of DMF (the percentage of the total weight of raw material monomers to the weight of the whole material is 30%, that is, the solid content) and 20ml of toluene, the initial reaction temperature is 135 ~ 140 ° C, with water for 2 ~ 3 hours, gradually increase the temperature When the reaction temperature is 150-155°C, continue the reaction for 4-6 hours, filter while it is hot and discharge it into ice ethanol to obtain a large amount of bright yellow precipitate. After filtering, wash the crude product in deionized water for 3-4 times until the filtrate is almost Reflux in hot ethanol for 2 to 3 hours to remove organic impurities, recrystallize in DMSO solvent, filter, cool and dry in a vacuum oven for 24 hours to obtain bright yellow nitro compound 1,4-bis(4-nitro- 2 cyanophenoxy) biphenyl 46g, yield 8...

Embodiment 2

[0061] According to the operation prepared by the nitro compound in Example 1, the anhydrous K 2 CO 3 The input amount is increased to 20.7g (0.15mol), all the other conditions are constant, obtain product 1,4-bis (4-nitro-2 cyanophenoxy group) the characterizing result of biphenyl and the nitro compound of embodiment 1 The characterization results are consistent.

Embodiment 3

[0063]According to the operation of the preparation of the nitro compound in Example 1, only the addition of DMF is changed to 112ml (the solid content of the system is increased from 30% to 35%) to obtain the product 1,4-two (4-nitro-2 cyano) The characterization result of phenoxy)biphenyl is consistent with the characterization result of the nitro compound in Example 1.

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Abstract

The invention relates to a high-adhesion-property low-linear-expansion-coefficient polyimide film material and a preparation method thereof, belonging to the technical field of high polymer material synthesis. The main chain of the polyimide contains cyano group, and is a homopolymerized or copolymerized polyimide polymer of a rigid chain; and thus, the polyimide has higher adhesion property and low linear expansion coefficient. The preparation method comprises the following steps: synthesizing cyano-introduced amino monomer containing rigid structure; and carrying out polycondensation on the synthesized amino monomer or with other diamine monomers containing rigid structure and acid anhydride monomer to obtain the polyimide film. The polyimide film material has higher adhesion property and lower linear expansion coefficient, so that the adhesion property and linear expansion coefficient are optimal, and the mechanical property and heat stability of the polyimide are obviously improved. The polyimide film material can be used in field of high-adhesion-property materials and provide low linear expansion coefficient.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and in particular relates to the preparation of polyimide with high adhesion and low coefficient of linear expansion. Background technique [0002] Polyimide is a promising polymer material. After decades of development, it has a wide variety and various forms. Compared with other heterocyclic compounds, polyimide has a wide range of raw material sources and diverse synthetic routes. , more comprehensive functions, etc., and because of its outstanding thermal properties, polyimide meets the needs of aerospace technology for high temperature resistant, lightweight structural materials, in addition, polyimide also has excellent mechanical properties , good chemical stability, extremely low temperature resistance, good film-forming properties, various synthesis methods, safety, and non-toxic properties. These properties make polyimides have a wide range of applications, involving ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08G73/10
CPCC08G73/1003C08J5/18C08J2379/08C08L79/08C08L2201/08C08L2203/16
Inventor 刘佰军沈艳超井丽巍姜振华
Owner JILIN UNIV