Optimized preparation method of polyimide film

A polyimide film and polyamic acid technology, applied in the chemical industry, can solve the problems of low thermal expansion coefficient, low glass transition temperature, and inability to meet the temperature requirements of flexible substrates.

Inactive Publication Date: 2017-07-07
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the defects of the prior art that the glass transition temperature is too low to meet the strict temperature requirements in the production process of flexible substr

Method used

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  • Optimized preparation method of polyimide film
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  • Optimized preparation method of polyimide film

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Weigh 6.73g of 2-(4-aminophenyl)-5-aminobenzimidazole and 6.55g of pyromellitic anhydride into a 250mL three-necked flask, blow Ar gas under an ice-water bath and stir mechanically. Add 60 mL of anhydrous N,N-dimethylacetamide as a solvent, and increase the viscosity as time goes on, adding 95 mL of solvent in total, and the final solid content is 8.4%wt. After a reaction time of 10 hours, remove the reaction device and seal the bottle mouth, and place it in a refrigerator at -20°C for 1 day to defoam to obtain a uniform yellow PAA glue.

[0047] Put the PAA glue solution taken out of the refrigerator at room temperature and let it return to room temperature, and the temperature of the operating table of the film coating machine rises to 70 ℃ , and place a clean and flat glass piece on the table for coating. The thickness of the film applicator is controlled at 500 μm. Transfer the coated glass sheet to a blast oven, and pre-bake it according to the temperature rise p...

Embodiment 2

[0057] Weigh 6.73g of 2-(4-aminophenyl)-5-aminobenzimidazole, 2.62g of pyromellitic anhydride and 5.30g of 3,3',4,4'-biphenyltetracarboxylic anhydride (pyromellitic anhydride Formic anhydride: 3,3',4,4'-biphenyltetracarboxylic anhydride = 2:3) was added into a 250 mL three-necked flask, and Ar gas was introduced under an ice-water bath and stirred mechanically. Add 60mL of anhydrous N,N-dimethylacetamide as a solvent, the viscosity becomes larger as time goes on, add 80mL of solvent in sequence, and the final solid content is 9.8%wt. After a reaction time of 14 hours, the reaction device was removed and the bottle mouth was sealed, and it was placed in a refrigerator at -20°C for 1 day to defoam, and a uniform yellow PAA glue was obtained.

[0058] Put the PAA glue solution taken out of the refrigerator at room temperature and let it return to room temperature, and the temperature of the operating table of the film coating machine rises to 70 ℃ , and place a clean and flat gl...

Embodiment 3

[0068] Weigh 4.51g of 2-(4-aminophenyl)-5-aminobenzimidazole and 5.89g of 3,3',4,4'-biphenyltetracarboxylic anhydride into a 150mL three-neck flask, Ar gas, add the solvent anhydrous N,N-dimethylacetamide 60mL. The solid content was 15.6%wt. After 12 hours of reaction time, the reaction device was removed and the bottle mouth was sealed, and it was placed in a refrigerator at -20°C for 1 day to remove bubbles, and a uniform yellow PAA glue was obtained.

[0069] Put the PAA glue solution taken out of the refrigerator at room temperature and let it return to room temperature. The temperature of the operating table of the film coating machine is raised to 70°C, and a clean and flat glass sheet is placed on the table for coating. The thickness of the film applicator is controlled at 500 μm. Transfer the coated glass sheet to a blast oven, and pre-bake it according to the temperature rise program of 70°C / 2h, 90°C / 2h, 110°C / 2h, 130°C / 2h, 150°C / 2h, 180°C / 2h to remove solvent. Aft...

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Abstract

The invention relates to an optimized preparation method of a polyimide film. The optimized preparation method comprises the following steps: dissolving diamine monomers and dianhydride monomers which have benzimidazole and benzothiazole structures into a non-protonic solvent, so as to obtain yellow homogeneous-phase sticky polyamide acid (PAA) low-temperature glue liquid; and coating a film with the PAA low-temperature glue liquid, removing the solvent according to an optimized heating process, and carrying out amination, so as to obtain the polyimide film. The glass-transition temperature of the polyimide film is 309-482 DEG C, the 1% thermal decomposition temperature of the polyimide film is 448-520 DEG C, and the thermal expansion coefficient of the polyimide film at 50-250 DEG C is 4.213ppm/K-(-)2.054ppm/K. The polyimide film having relatively high heat stability and dimensional stability can meet bearing conditions of polyimide as a flexible substrate and is an ideal OLED substrate material.

Description

technical field [0001] The invention relates to a technology in the field of chemical industry, in particular to an optimized preparation method of a polyimide film with low thermal expansion coefficient and high temperature resistance. Background technique [0002] The realization of flexible OLED technology largely depends on the design and development of new materials. With the development of OLED devices from unbreakable → bendable → rollable → foldable, polymer film substrates show strong advantages. Polyimide (Polyimide: PI) is an aromatic heterocyclic polymer whose main chain structure unit contains imide characteristic groups. Due to its semi-ladder and ladder main chain structure and the resonance of the aromatic ring, it has excellent Thermal stability, chemical stability, good dielectric properties, high insulation and excellent mechanical strength and other characteristics. At present, it is widely used in aerospace, electronic and electrical, precision machiner...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08G73/10
CPCC08J5/18C08G73/1085C08J2379/08
Inventor 路庆华廉萌
Owner SHANGHAI JIAO TONG UNIV
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