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Preparation method of polyimide film with low thermal expansion coefficient

A technology of polyimide film and low thermal expansion coefficient, which is applied in the field of preparation of polyimide film, can solve problems such as unfavorable size stability, and achieve the effect of balanced performance, good flexibility and good bonding performance

Active Publication Date: 2017-11-07
安徽统唯新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Polyimides with traditional structures are mainly synthesized from dibasic anhydrides and dibasic amines. The source of raw materials is wide and the synthesis is relatively easy.
There are many kinds of dianhydrides and diamines, and polyimides with different properties can be obtained by different combinations. The CTE of polyimide films with traditional structures generally ranges from 40 to 65ppm / K. Compared with copper foil and silicon wafers, the CTE CTE16~17ppm / K is too high, which is not conducive to the dimensional stability of the laminated copper foil

Method used

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  • Preparation method of polyimide film with low thermal expansion coefficient

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Comparison scheme
Effect test

Embodiment 1

[0019] The preparation method of polyimide film with low thermal expansion coefficient comprises the following steps:

[0020] (1) Under normal pressure conditions full of nitrogen in the kettle body at 45°C, pyromellitic dianhydride and p-phenylenediamine are placed in dimethylacetamide solvent for polycondensation reaction, pyromellitic dianhydride and p-phenylenediamine The molar ratio of phenylenediamine is 1:1.005. When performing polycondensation reaction, first dissolve p-phenylenediamine in dimethylacetamide solvent (stirring speed 70r / min, time not less than 2h), and then add in 4 times Pyromellitic dianhydride (stirring speed 115r / min), and in the process of adding pyromellitic dianhydride, the time interval between two adjacent times is 60 minutes, and each addition in the first three times accounts for 54% of the balance. %, after adding pyromellitic dianhydride, react for another 180 minutes to obtain polyamic acid glue A with a solid content of 20wt%;

[0021] (...

Embodiment 2

[0025] The preparation method of polyimide film with low thermal expansion coefficient comprises the following steps:

[0026] (1) Under normal pressure conditions full of nitrogen in the kettle body at 35°C, pyromellitic dianhydride and p-phenylenediamine are placed in dimethylacetamide solvent for polycondensation reaction, pyromellitic dianhydride and p-phenylenediamine The molar ratio of phenylenediamine is 1:1.002. When carrying out polycondensation reaction, first dissolve p-phenylenediamine in dimethylacetamide solvent (stirring speed 70r / min, time not less than 2h), and then add in 4 times Pyromellitic dianhydride (stirring speed 115r / min), and in the process of adding pyromellitic dianhydride, the time interval between two adjacent times is 40 minutes, and each addition in the first three times accounts for 45% of the balance. %, after the addition of pyromellitic dianhydride, react for another 200 minutes to obtain polyamic acid glue A with a solid content of 17wt%; ...

Embodiment 3

[0031] The preparation method of polyimide film with low thermal expansion coefficient comprises the following steps:

[0032] (1) Under normal pressure conditions full of nitrogen in the kettle body at 55°C, pyromellitic dianhydride and p-phenylenediamine are placed in dimethylacetamide solvent for polycondensation reaction, pyromellitic dianhydride and p-phenylenediamine The molar ratio of phenylenediamine is 1:1.008. When conducting polycondensation reaction, first dissolve p-phenylenediamine in dimethylacetamide solvent (stirring speed 70r / min, time not less than 2h), and then add in 4 times Pyromellitic dianhydride (stirring speed 115r / min), and in the process of adding pyromellitic dianhydride, the time interval between two adjacent times is 80 minutes, and each addition in the first three times accounts for the wt of the balance %, after adding pyromellitic dianhydride, react for another 160 minutes to obtain polyamic acid glue A with a solid content of 23wt%;

[0033]...

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Abstract

The preparation method of the low thermal expansion coefficient polyimide film of the present invention comprises the following steps: (1) placing pyromellitic dianhydride and p-phenylenediamine in a dimethylacetamide solvent for polycondensation reaction to obtain polyamic acid Glue A; (2) 2,3',3,4'-biphenyltetracarboxylic dianhydride and 4,4'-diaminodiphenyl ether were placed in dimethylacetamide solvent for polycondensation reaction to obtain poly Amic acid glue B; (3) polyamic acid glue A and polyamic acid glue B are mixed, and high-speed stirring reaction is obtained polyamic acid glue C; (4) polyamic acid solution C is made by casting process Form a film, and finally send the film into an imidization furnace for treatment to obtain the polyimide film with low thermal expansion coefficient. The CTE of the low thermal expansion coefficient polyimide film prepared by the invention is 15-17ppm / K, and it also has performance advantages such as high strength, high stability and high electric strength.

Description

technical field [0001] The invention relates to the field of preparation of polyimide films, in particular to a preparation method of polyimide films with low thermal expansion coefficient. Background technique [0002] Polyimide refers to a class of polymers containing imide rings (-CO-NH-CO-) in the main chain. It is one of the organic polymer materials with the best comprehensive performance and has been widely used in aviation and aerospace. , microelectronics, nanometer, liquid crystal, separation membrane, laser and other fields. When polyimide is used as a base film on a flexible circuit board, the dimensional stability of the film is highly required, so the coefficient of thermal expansion (CTE) is an important parameter to investigate the dimensional stability of the film. [0003] Polyimides with traditional structures are mainly synthesized from dibasic anhydrides and dibasic amines, with wide sources of raw materials and relatively easy synthesis. There are man...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 王超
Owner 安徽统唯新材料科技股份有限公司
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