Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing polyimide film from polyamide acid slurry

A technology of polyimide film and polyamic acid, which is applied in the field of preparing polyimide film with polyamic acid slurry, can solve the problems of inability to obtain comprehensive performance PI film, poor performance, and performance difference of PI film, and achieve improvement Application range and prospect, improvement of production efficiency, effect of shortened time

Active Publication Date: 2021-05-25
武汉柔显科技股份有限公司
View PDF6 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Different processing conditions will affect various properties of PI films, and different film-forming processes will affect the movement of molecular segments, which will lead to significant differences in the properties of PI films.
[0004]Current studies have found that the curing rate and curing temperature will have an important impact on the structure and properties of the film, but the reaction path of each stage of the curing process is still unclear, which is As a result, in the prior art, the effect of improving the performance of the PI film by adjusting the curing program such as the heating program is not good, and the PI film with more excellent comprehensive properties cannot be obtained.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing polyimide film from polyamide acid slurry
  • Method for preparing polyimide film from polyamide acid slurry
  • Method for preparing polyimide film from polyamide acid slurry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0098] Preparation of polyamic acid slurry: 1,4-phenylenediamine (PPD) is selected as the diamine monomer, and 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA) and 3,3'4,4'-Diphenyl ether tetracarboxylic dianhydride (ODPA), the solvent is 1-methyl-2-pyrrolidone (NMP). The molar ratio of diamine monomer to dianhydride monomer is 1:0.982, and the dianhydride mixed component is composed of 95mol% s-BPDA and 5mol% ODPA. First add PPD to the solvent NMP under the protection of an inert atmosphere at room temperature and stir to dissolve it. After the three-necked flask becomes a clear liquid, quickly add s-BPDA and ODPA, and use the remaining NMP to rinse the weighing cup and react. The inner wall of the flask. NMP accounts for 13-16 wt% of the total mass of the slurry. The resulting slurry was carried out at a reaction temperature of 40°C under the protection of an inert atmosphere, and continued to stir for 12 hours to obtain a solid content of 14.5wt%, a viscosity of 554...

Embodiment 2

[0103] The same method as in Example 1 was used to prepare a polyimide film. The difference from Example 1 is that the high-temperature heat treatment (OVEN) process adopts a four-stage heating program: at a heating rate of 2.1 °C / min, the temperature is raised from 100 °C to 220 °C , kept at 220°C for 30 minutes; at a heating rate of 4.5°C / min, from 220°C to 300°C, and at 300°C for 45 minutes; at a heating rate of 5.8°C / min, from 300°C to 350°C, at Keep warm at 350°C for 30 minutes; heat up from 350°C to 400°C at a heating rate of 7.2°C / min, and keep warm at 400°C for 20 minutes.

[0104] Gained brown-yellow polyimide film thickness 9.97 μm, figure 1 For the obtained polyimide film physical figure, from figure 1 It can be seen that the film-forming property is good and the color of the film is uniform. Figure 7 It is the XRD spectrum pattern of gained polyimide film.

Embodiment 3

[0106] A polyimide film was prepared in the same manner as in Example 2, except that the vacuum pretreatment (HVCD) process lasted 30 minutes to obtain a semi-dry and semi-wet film with a solvent removal rate of 63.2%. The obtained polyimide film has a thickness of 10.36 μm and good film-forming properties.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
thicknessaaaaaaaaaa
thermal decomposition temperatureaaaaaaaaaa
tensile strengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for preparing a polyimide film from polyamide acid slurry, belonging to the technical field of high polymer materials. The method comprises vacuum pretreatment and high-temperature heat treatment. In the vacuum pretreatment, the solvent evaporation rate of the polyamide acid slurry is 0.088-0.42 g / (min * m<2>), and a solvent removal rate is 50-95 wt.%; the temperature of the high-temperature heat treatment is from vacuum pretreatment temperature to a highest curing temperature, and segmented heating is adopted; and the vacuum pretreatment temperature is 50-150 DEG C, the highest curing temperature is 350-500 DEG C, and the heating rate of each section is 1-10 DEG C / min and is sequentially increased. According to a film preparation process provided by the invention, the polyimide film with more excellent comprehensive performance can be obtained, and the application range and prospect of the PI film in the photoelectron industry are improved; and meanwhile, heat treatment time is shortened, energy is saved, and production efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for preparing a polyimide film from a polyamic acid slurry. 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 highest heat-resistant high-molecular material so far. It is used in aerospace, microelectronics, machinery, high-end filter industry, separation membrane, laser and other fields. Because of its outstanding performance, polyimide, whether as a structural material or as a functional material, has been fully recognized for its huge application prospects. It is known as a "problem-solving expert" and believes that " Without polyimide, there would be no microelectronics technology today." [0003] With the development of electronic device technology, the demand for high-performance polyimide film is becoming more and more urgent. High...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
CPCC08J5/18C08G73/1071C08G73/1007C08J2379/08
Inventor 阮敏肖桂林付华鲁丽平朱双全
Owner 武汉柔显科技股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com