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A kind of matte black polyimide film with low pinhole occurrence rate and preparation method thereof

A technology of black polyimide and occurrence rate is applied in the field of low pinhole occurrence rate matt black polyimide film and its preparation, which can solve the problem that bubbles and pinholes and carbon black are prone to agglomeration. and other problems, to reduce the generation of pinholes and bubbles in the film, reduce the generation of pinholes and bubbles, and achieve the effect of good mechanical properties

Active Publication Date: 2021-06-15
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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  • A kind of matte black polyimide film with low pinhole occurrence rate and preparation method thereof
  • A kind of matte black polyimide film with low pinhole occurrence rate and preparation method thereof
  • A kind of matte black polyimide film with low pinhole occurrence rate and preparation method thereof

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Experimental program
Comparison scheme
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 matte black polyimide film with low pinhole occurrence rate and a preparation method thereof. The preparation method comprises the following steps: 1) mixing a black dispersion in which the solute is carbon black and a white dispersion in which the solute is a matting agent, performing shear dispersion and / or ultrasonic dispersion on the resulting mixed solution, adding non-metal alkoxide, Then carry out shear dispersion and / or ultrasonic dispersion to obtain a black filler dispersion; 2) In a polar aprotic solvent, add diamine and dianhydride in a molar ratio of 1:0.990-0.998 to react to obtain a polyamic acid resin solution, then add the black filler dispersion, stir well and then add or not add stabilizer, stir well to obtain a matt black polyamic acid resin solution; 3) The obtained matt black polyamic acid resin solution is prepared according to the existing conventional process Matt black PI film. The film prepared by the method of the invention has good mechanical properties, electrical properties and glossiness, and low pinhole rate and air bubble rate.

Description

technical field [0001] The invention relates to a polyimide film, in particular to a matte black polyimide film with low pinhole incidence and a preparation method thereof. Background technique [0002] In recent years, matt 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. However, the composition of matt black PI film includes black pigment (usually carbon black), matting powder and polyimide, and the addition of black pigment and matting powder is large, and the particle size of matting powder is large, and its dispersibility and Poor wettability not only directly affects the mechanical properties and electrical strength of the film, but also seriously affects the appearance of the film, such as pinholes, bubbles, black spots and impurities in the film, which are important indicators for the grade of matt black PI film. As people's requirements for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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