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Preparation method of size-stable polyimide film

A polyimide film, dimensionally stable technology, applied in the field of preparation of dimensionally stable polyimide film, can solve the problems of easy formation of small cracks, pulling fine lines, abnormal matching of longitudinal stretching process parameters, etc. Achieve the effect of improving production yield, reducing production energy consumption, and excellent dimensional stability

Active Publication Date: 2020-04-24
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Though this method can obtain the polyimide film that meets the thermal shrinkage rate of relevant requirement, low coefficient of thermal expansion, because in the actual production of longitudinal stretching (longitudinal stretching process is by oil heating roller and control roller speed, The gel film passing through the roller is stretched and shaped longitudinally at a certain temperature (usually 60-150°C), and the gel film with a large solvent content is easily deformed, so that there are many defects in the longitudinal stretching process. Problems, for example, the orientation and deformation of the gel film with uneven thickness are different when stretching in the longitudinal direction, which intensifies the deformation of the gel film in the subsequent transverse stretching, resulting in poor dimensional stability, poor appearance flatness, and uneven tension of the film. The problem of equalization; the extreme edge of the gel film is easy to form small cracks when it is heated, and when it is subjected to longitudinal tension, it will tear and break the film or even wrap the roll; changes in the ambient temperature during the production process, solvent recovery efficiency, etc. will affect the solvent content of the gel film , small changes in the solvent content of the gel film will make the matching degree of the longitudinal stretching process parameters abnormal, resulting in abnormal problems such as white spots, pulling fine lines, and scratch marks on the gel film surface
The above problems lead to low product yield

Method used

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  • Preparation method of size-stable polyimide film
  • Preparation method of size-stable polyimide film
  • Preparation method of size-stable polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Add 320kg of DMAc solvent in the reactor, then add 9kg of PDA and 25kg of ODA, stir for 0.5h, then add 45.6kg of PMDA (adding in 3 times), react for 5h at normal temperature, and obtain a viscosity of 100pa·s Polyamic acid resin solution; transporting it to a defoaming tank for defoaming to obtain a defoamed polyamic acid resin solution.

[0036] 2) The polyamic acid resin solution after defoaming is poured through the die to form a liquid film on the steel strip, and the solvent is removed by heating with hot air in the temperature range of T1, T2 and T3, and finally the imide with a solvent content of 27% is obtained. A gel film with a conversion rate of 85%; where,

[0037] T1 temperature is 80°C, and the processing time under T1 temperature condition is 50s; T2 temperature is 200°C, and the processing time under T2 temperature condition is 120s; T3 temperature is 300°C, and the processing time under T3 temperature condition is 20s .

[0038] 3) The resulting ge...

Embodiment 2

[0055] 1) with embodiment 1.

[0056] 2) The polyamic acid resin solution after defoaming is poured through the die to form a liquid film on the steel strip, and the solvent is removed by heating with hot air in the temperature range of T1 and T2 in turn, and finally the solvent content is 28%, and the imidization rate is 28%. is 83% gel film; among them,

[0057] T1 temperature is 90°C; T2 temperature is 180°C; T3 temperature is 290°C.

[0058] 3) with embodiment 1.

[0059] 4) With embodiment 1.

[0060] 5) With embodiment 1.

[0061] For the tensile strength and elongation at break of the obtained longitudinally stretched gel film in step 2) of the present embodiment, the results are shown in Table 1 below.

[0062] The CTE (coefficient of thermal expansion) and thermal shrinkage of the film obtained in step 4) of this embodiment were detected, and the results are shown in Table 2 and Table 3 below, respectively.

[0063] The thermal shrinkage rate of the film obtained...

Embodiment 3

[0066] 1) with embodiment 1.

[0067] 2) The polyamic acid resin solution after defoaming is poured through the die to form a liquid film on the steel strip, and the solvent is removed by heating with hot air in the temperature range of T1, T2 and T3 in sequence, and finally the imide with a solvent content of 24% is obtained. A gel film with a conversion rate of 80%; where,

[0068] T1 temperature is 100°C, and the processing time under T1 temperature condition is 100s; T2 temperature is 150°C, and the processing time under T2 temperature condition is 300s; T3 temperature is 290°C, and the processing time under T3 temperature condition is 40s .

[0069] 3) with embodiment 1.

[0070] 4) With embodiment 1.

[0071] 5) With embodiment 1.

[0072] For the tensile strength and elongation at break of the obtained longitudinally stretched gel film in step 2) of the present embodiment, the results are shown in Table 1 below.

[0073] The CTE (coefficient of thermal expansion) a...

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Abstract

The invention discloses a preparation method of a size-stable polyimide film. The preparation method comprises the following steps: 1) obtaining a defoamed polyamide acid resin solution; (2) casting the obtained resin solution onto a support body to form a liquid film, and sequentially heating the liquid film by hot air within the temperature ranges of T1, T2 and T3 to obtain a gel film, wherein the solvent content of the gel film is less than or equal to 35 percent and the imidization rate is more than or equal to 60 percent; 3) longitudinally stretching the obtained gel film through at leastsix rollers under a specific roller speed ratio condition without heating to obtain a longitudinally stretched gel film; 4) feeding the obtained longitudinally-stretched gel film into an imine furnace, and carrying out transverse stretching, imidization and a shaping treatment to obtain a polyimide film; and 5) feeding the obtained polyimide film into a gradient heating treatment at 150-400 DEG Cunder a condition of no stress, and then performing gradient cooling treatment at 400-50 DEG C. The provided method can guarantee a good heat shrinkage rate and low thermal expansion, and at the sametime, improves the continuity and yield of production.

Description

technical field [0001] The present invention relates to polyimide film, be specifically related to a kind of preparation method of dimensionally stable polyimide film. Background technique [0002] With the rapid development of electronic technology, the output of flexible copper-clad laminates has grown steadily, and the production scale has continued to expand. Especially, the demand and growth trend of flexible copper-clad laminates with polyimide film as the base material are more prominent. Polyimide (PI) film is combined with copper foil as an important insulating substrate of flexible printed circuit boards, and the film is required to have a thermal expansion coefficient similar to that of copper foil (18×10 -6 / K), lower thermal shrinkage rate (<0.05%), that is, high dimensional stability, to reduce the thermal stress accumulation of the two and cause problems such as peeling, cracking, and warping. At present, domestic polyimide films can only be used in the lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08G73/10C08L79/08
CPCC08G73/1007C08G73/1042C08G73/1071C08J5/18C08J2379/08
Inventor 白小庆青双桂潘钦鹏刘姣郑汉明
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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