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Low-pinhole-incidence matte black polyimide thin film and preparation method thereof

A technology of black polyimide and incidence rate, which is applied in the field of low pinhole occurrence matte black polyimide film and its preparation, and can solve the problems of bubbles and pinholes, and the easy agglomeration of carbon black etc. to achieve the effect of reducing the generation of film pinholes and bubbles, reducing the generation of pinholes and bubbles, and reducing the specific surface area

Active Publication Date: 2019-01-04
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can ensure that the silane coupling agent is physically attached or chemically bonded to the carbon black surface, preventing the coupling agent from dissociating in the solvent from self-condensation, however, in the drying (baking) process after surface modification, due to the silane coupling The coupling agent is a silicone resin that can be hydrolyzed into a network and has a certain viscosity. Although it is attached to the surface of carbon black, it will also polymerize during the baking process, causing carbon black to easily agglomerate
Therefore, the existing disclosed method of using a coupling agent to treat the surface of carbon black cannot well solve the bubbles and pinholes produced by the agglomeration of carbon black and matting powder

Method used

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  • Low-pinhole-incidence matte black polyimide thin film and preparation method thereof
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  • Low-pinhole-incidence matte black polyimide thin film and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0034] 1) Preparation of black filler dispersion:

[0035] 1.1) Mix 4.2kg carbon black (primary particle size is 5nm) and 38kg DMAc evenly, use high-speed shearing machine to shear and disperse (rotating speed is 2000r / min, dispersion time is 1h), and then use homogenizer to disperse (pressure is 40MPa, and the homogenization time is 30min), to obtain a black dispersion, for subsequent use;

[0036] 1.2) Mix 4.2kg of silicon dioxide (average particle size of 4 μm) and 24kg of DMAc evenly, place in a high-speed shearing machine and shear and disperse at a speed of 3000r / min for 3 hours to obtain a white dispersion, which is set aside;

[0037] 1.3) Mix the black dispersion with the white dispersion, place the resulting mixture in a high-speed shear, add 85g of n-butyl titanate, shear and disperse at a speed of 2000r / min for 10h, and then place it in an ultrasonic device for ultrasonication Disperse for 2 hours to obtain a black filler dispersion;

[0038] 2) Add 0.2mol ODA to...

Embodiment 2

[0041] Repeat Example 1, the difference is:

[0042] In step 1.3), the non-metal alkoxide is ethyl orthosilicate;

[0043] Step 2) in, the total amount of PMDA is 0.1994mol;

[0044] In steps 1) and 2), the polar aprotic solvent is changed to NMP.

Embodiment 3

[0046] Repeat Example 1, the difference is:

[0047] In step 1.1), the primary particle size of carbon black is 300nm;

[0048] In step 1.3), the non-metal alkoxide is ethyl orthosilicate.

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Abstract

The invention discloses a low-pinhole-incidence matte black polyimide thin film and a preparation method thereof. The preparation method comprises the following steps: 1) mixing black dispersion liquid of which the solute is carbon black with white dispersion liquid of which the solute is a matting agent, carrying out shear dispersion and / or ultrasonic dispersion on the obtained mixed solution, adding nonmetallic alkoxide, and carrying out shear dispersion and / or ultrasonic dispersion to obtain black filler dispersion liquid; 2) adding diamine and dianhydride in a polar aprotic solvent according to the molar ratio of 1: 0.990-0.998 and reacting to obtain a polyamide acid resin solution, adding the black filler dispersion liquid, stirring uniformly and then adding or not adding a stabilizing agent, and stirring uniformly to obtain a matte black polyamide acid resin solution; and 3) preparing the obtained matte black polyamide acid resin solution according to an existing conventional process to obtain the matte black PI thin film. The thin film prepared by the method has good mechanical property, electrical property and glossiness and low pinhole and bubble rate.

Description

technical field [0001] The invention relates to a polyimide film, in particular to a matte black polyimide film with low pinhole occurrence rate and a preparation method thereof. Background technique [0002] In recent years, matte black polyimide (PI) film has the appearance color of black, soft gloss and matte surface, and has become one of the mainstream cover film materials for electronic packaging. But the composition material of matt black PI film comprises black pigment (usually carbon black), matting powder and polyimide, and the addition amount of black pigment and matting powder is large, and the particle size of matting powder is big, its dispersibility and Poor wettability not only directly affects the mechanical properties and electrical strength of the film, but also seriously affects the appearance quality of the film, such as pinholes, bubbles, black spots and impurities in the film, which are important indicators for determining the grade of matte black PI f...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08K3/04C08K3/22C08K3/36C08J5/18C08G73/10
CPCC08G73/105C08G73/1071C08J5/18C08J2379/08C08K3/04C08K3/22C08K3/36C08K2003/2241C08K2201/011
Inventor 青双桂唐必连冯婷婷马纪翔白小庆蒋耿杰
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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