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Preparation method of polyimide ultrathin film

A technology of polyimide and ultra-thin film, which is applied in the field of preparation of polyimide ultra-thin film, can solve the problems of difficult film mechanical properties, poor film-forming continuity, poor film plasticity, etc., to overcome poor film-forming continuity, weakening Excellent internal friction and film-forming continuity

Active Publication Date: 2019-10-18
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above-mentioned coating method and lamination method are difficult to prepare ultra-thin films with uniform thickness and high mechanical properties. The chemical imidization method has expensive equipment and large environmental pollution, while the casting method has little environmental pollution and the prepared resin film has good thickness uniformity and can The PI film with good mechanical properties and high degree of orientation is prepared by biaxial stretching, but when the ultra-thin film is prepared by the conventional casting method (the salivation process and imidization process when the ultra-thin film is prepared by the conventional casting method are: the self-supporting film obtained by the salivation After longitudinal stretching, it is sent to the imine furnace, and it is obtained after preheating, transverse stretching, imidization, and shaping; among them, the temperature of the upper drying tunnel is set at 90°C-130°C during film formation, and the temperature of the lower drying tunnel is The temperature is set at 140°C-160°C, the temperature during longitudinal stretching is 80-120°C, the temperature in the preheating zone of the imine furnace is 150-210°C, the temperature in the transverse stretching zone is 310-320°C, the longitudinal stretching ratio and The transverse stretch ratio is usually 1.05-1.20, the temperature in the imidization zone is 300-370°C, and the temperature in the shaping zone is 330-390°C). Because the film is too thin, the internal solvent evaporates too quickly, which will easily lead to poor film plasticity. The film is easy to break in the imine furnace, the continuity of the film is poor, and it is difficult to stretch the film transversely to improve the mechanical properties of the film

Method used

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  • Preparation method of polyimide ultrathin film
  • Preparation method of polyimide ultrathin film
  • Preparation method of polyimide ultrathin film

Examples

Experimental program
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Effect test

Embodiment 1

[0025]1) Add 51.692 kg of diamine (ODA), 492 kg of dimethylacetamide (DMAC) and 28.154 kg of homoanhydride (PMDA) in the reactor according to the conventional process, stir evenly and add homoanhydride in batches to synthesize a viscosity of 12 10,000 centipoise of polyamic acid resin solution, adding diisobutyl phthalate with a boiling point of 327°C to it, controlling the amount of plasticizer added to be 1% of the weight of the polyamic acid resin solution, stirring evenly, and the resulting mixture Send into the defoaming kettle for defoaming, obtain the polyamic acid resin solution after defoaming;

[0026] 2) Set the temperature of the casting upper drying tunnel to 100°C and the temperature of the lower drying tunnel to 150°C; send the defoamed polyamic acid resin solution to the extrusion die to drool on the steel belt, start the operation of the steel belt, wait for the casting temperature When the specified temperature is reached, the feeding is started, and 70% of t...

Embodiment 2

[0047] Repeat Example 1, the difference is:

[0048] In step 1), the viscosity of the obtained polyamic acid resin solution is controlled to be 140,000 centipoise, and the plasticizer is changed to diisooctyl phthalate with a boiling point of 370° C.

[0049] In step 2), the longitudinal stretching temperature is 121°C, the preheating temperature is 211°C, the transverse stretching temperature is 280°C, and the setting temperature is 520°C. Wherein the stretching ratios of longitudinal stretching and transverse stretching all start from 1, and gradually increase at a rate of 0.02 until the film is broken, count the number of broken films of continuous production for 24h, and measure the thickness, tensile strength and thickness of the gained ultra-thin film The results of elongation at break are shown in Table 2 below.

Embodiment 3

[0051] Repeat Example 1, the difference is:

[0052] In step 1), the viscosity of the obtained polyamic acid resin solution is controlled to be 40,000 centipoise, and the plasticizer is changed to dioctyl phthalate with a boiling point of 386° C.

[0053] In step 2), the transverse stretching temperature in the imine furnace is changed to 300°C, and the temperature in the shaping zone is changed to 400°C. The stretch ratios of longitudinal stretching and transverse stretching all start from 1, and gradually increase at a rate of 0.02 until the film is broken, and the number of film breaks in 24 hours of continuous production is counted, and the thickness, tensile strength and fracture of the obtained ultra-thin film are measured. Elongation, the results are shown in Table 2 below.

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Abstract

The invention discloses a preparation method of a polyimide ultrathin film. The method comprises the following steps: 1) obtaining a polyamic acid resin solution, adding a plasticizer with a boiling point of 320-420 DEG C into the polyamic acid resin solution, performing uniform mixing, and performing defoaming on the obtained mixture to obtain a defoamed polyamic acid resin solution, wherein theaddition amount of the plasticizer is 0.5-1.5% of the weight of the polyamic acid resin solution; and 2) performing casting on the defoamed polyamic acid resin solution to form a film, performing longitudinal stretching, sending the stretched film into an imine furnace, performing preheating, performing transverse stretching, performing imidization and performing shaping to obtain the polyimide ultrathin film, wherein the temperature during longitudinal stretching is 121-150 DEG C, the preheating temperature is 211-250 DEG C, the temperature during transverse stretching is 280-300 DEG C, and the temperature during shaping is 400-520 DEG C. According to the method provided by the invention, the ultrathin film can be longitudinally and transversely stretched at a high ratio, meanwhile, the continuity of film forming in the imine furnace is guaranteed, and the mechanical properties of the obtained ultrathin film are good.

Description

technical field [0001] The invention relates to a preparation method of a polyimide film, in particular to a preparation method of a polyimide ultra-thin film. Background technique [0002] Polyimide (PI) films are widely used in the fields of optics, electronics, and aerospace due to their excellent mechanical properties, high and low temperature resistance, thermal dimensional stability, and electrical insulation properties. According to the thickness, polyimide film can be classified into ultra-thin film (d≤8μm), conventional thin film (8μm<d≤50μm), thick film (50μm<d≤125μm) and ultra-thick film (d>125μm). [0003] Ultra-thinning is an important trend in the development of PI thin films, and its driving force mainly comes from the application requirements of aerospace, electronics and other industries for device weight reduction, thinning and functionalization. Due to the technical difficulty of PI ultra-thin film in the manufacturing process and other aspects, ...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08G73/10C08K5/12C08K5/523C08L79/08
CPCC08J5/18C08G73/1071C08G73/105C08J2379/08C08K5/12C08K5/523
Inventor 蒋耿杰青双桂马纪翔姬亚宁白小庆
Owner GUILIN ELECTRICAL EQUIP SCI RES INST