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Preparation method of photocured crosslinked polyimide film

A polyimide film and light-curing technology, which is applied in the field of polymer materials, can solve problems such as not exceeding, and achieve the effects of increased tensile strength and elastic modulus, excellent mechanical properties, and good dimensional stability

Active Publication Date: 2019-09-27
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] Photosensitive polyimide has attracted the attention and attention of many scholars, but few people realize that the traditional PI industry has encountered greater challenges: the rapid development and application of flexible circuit boards and flexible displays in today's rapid development of the microelectronics industry , put forward higher and higher requirements for PI materials. For example, when flexible copper-clad laminates are processed into microelectronic devices, PI films are required to have a thermal expansion coefficient of 15 μm / ( m °C); the PI substrate has to experience a high temperature of about 500 °C during the flexible display process, and the thermal expansion coefficient cannot exceed 5 μm / (m °C), while the general thermal expansion coefficient of the PI film is 30 ~ 60 μm / (m ℃), how to significantly reduce the thermal expansion coefficient of this type of PI is a challenge we face

Method used

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  • Preparation method of photocured crosslinked polyimide film
  • Preparation method of photocured crosslinked polyimide film
  • Preparation method of photocured crosslinked polyimide film

Examples

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preparation example Construction

[0065] The invention provides a kind of preparation method of photocuring cross-linked polyimide film, comprises the following steps:

[0066] (1) polymerizing dianhydride, end-blocking monoanhydride and diamine in an aprotic polar solvent to obtain a polyamic acid slurry with a mass percent concentration of 12% to 30% and a viscosity of 3000 to 9000cp, the (two Anhydride + capped monoanhydride) to diamine molar ratio is (100:95) ~ (100:110), where

[0067] The dianhydride includes the first functional dianhydride and the second functional dianhydride, and the molar ratio of the first functional dianhydride, the second functional dianhydride and the blocked monoanhydride is (2~98.95):(97~1 ):(5~0.05)

[0068] The first functional dianhydride is selected from at least one of the following substances:

[0069]

[0070] The second functional dianhydride is selected from at least one of the following substances;

[0071]

[0072] The end-blocking monoanhydride is selected...

Embodiment 1

[0118] A light-cured PI film adding photoinitiator 1173 0.1% (wt) and co-initiator pentaerythritol tetramercaptoacetate 1.0% (wt), wherein the dianhydride includes the first functional dianhydride and the second functional dianhydride, the second The first functional dianhydride is S-BPDA, the second functional dianhydride is BTDA, the blocked monoanhydride is PEPA, and the molar ratio of the first functional dianhydride, the second functional dianhydride and the blocked monoanhydride is 80 / 18 / 2. The diamine is DMB, the molar ratio of diamine to (dianhydride + blocked monoanhydride) is 1:1, the aprotic solvent is NMP, and the solid content is 15%. The specific implementation plan is as follows:

[0119] (1) Pre-treatment of raw materials and solvents: DMB was dried in a vacuum oven at 60°C for 2 hours, S-BPDA and BTDA were dried in a vacuum oven at 120°C for 3 hours, NMP was added with 4A spherical molecular sieves and allowed to stand for 6 hours;

[0120] (2) Accurately we...

Embodiment 2-14

[0133] By comparing Example 1 and Example 1, it can be seen that the glue viscosity and film-forming performance synthesized in Example 1 are better and meet the requirements, and then the adjustment of other parameters is explored based on the preparation scheme of Example 1. The reaction steps and conditions are the same as in Example 1, and the specific material consumption and test results are as shown in Table 1. Since the viscosity of the system increases sharply after photocuring, the refractive index will also change to a certain extent, so it can be judged from the apparent change of the coating film whether it can be photocured.

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Abstract

The invention provides a preparation method of a photocured polyimide film. The crosslinking density between polyimide molecular chains is improved by ultraviolet light curing to greatly reduce the thermal expansion coefficient of a PI film and ensure the comprehensive performances of the PI film. The preparation method comprises the following steps: (1) polymerizing a dianhydride, an end-capped monoanhydride and a diamine in an aprotic polar solvent to obtain a polyamic acid slurry having a mass percentage concentration of 12-30% and a viscosity of 3000-9000 cp, wherein a molar ratio of the dianhydride and the end-capped monoanhydride to the diamine is (100:95) to (100:110); (2) cooling the polyamic acid slurry to room temperature, adding a photoinitiator and a co-initiator, performing mixing until uniformly, and defoaming the obtained mixture for 0.5-24 h, wherein the photoinitiator accounts for 0.1-6% of the mass of the polyamic acid slurry, and the co-initiator accounts for 0.1-10% of the mass of the polyamic acid slurry; (3) performing coating film formation to obtain a wet film; and (4) performing illumination under an ultraviolet curing device for 5-300 s, and performing thermal imidization to obtain the photocured polyimide film.

Description

technical field [0001] The invention relates to the field of macromolecular materials, in particular to a method for preparing a light-cured cross-linked polyimide film. Background technique [0002] Polyimide (PI) refers to the aromatic heterocyclic high molecular polymer containing imide ring (-CO-N-CO-) group in the main chain. It is the polymer material with the highest heat resistance level so far. It can be used at 300°C and can withstand high temperatures of 500°C for a short time. Because of its excellent performance, it has been widely used in aerospace, microelectronics, machinery, high-end filter industry, separation membrane, laser and other fields. Because of its outstanding performance characteristics, polyimide has been fully recognized for its huge application prospects whether it is used as a structural material or as a functional material. It is known as an "expert in solving various problems" and It is believed that "without polyimide, there would be no ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
CPCC08G73/1007C08G73/1042C08G73/1067C08J5/18C08J2379/08
Inventor 尤庆亮阮敏刘继延邹立勇刘志宏高阳光周瑞雪高淑豫刘学清胡成龙胡思前付华
Owner JIANGHAN UNIVERSITY
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