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A kind of matt black polyimide film with low thermal expansion coefficient and preparation method thereof

A technology of black polyimide and low thermal expansion coefficient, which is applied in the field of low thermal expansion coefficient matt black polyimide film and its preparation, can solve the problems of hindered filler dispersion uniformity, insufficient resin reaction, pinholes, etc. Achieve excellent insulation performance and tensile length, reduce the generation of pinholes and air bubbles, and the effect of low pinhole and air bubble rate

Active Publication Date: 2021-03-05
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is well known to those skilled in the art that the addition of rigid monomers will further reduce the elongation at break of the matt black PI film, thereby affecting the stability of product production.
In addition, the solubility of PPDA in DMAc or NMP at room temperature is much lower than that of ODA. During the reaction process, the incompletely reacted PPDA and filler may interact or coat each other, making the resin insufficiently reacted, or causing the filler to disperse evenly. resistance, resulting in air bubbles and pinholes

Method used

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  • A kind of matt black polyimide film with low thermal expansion coefficient and preparation method thereof
  • A kind of matt black polyimide film with low thermal expansion coefficient and preparation method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0039] 1) Preparation of nanocomposite sol:

[0040] Mix 500g of absolute ethanol and 20g of deionized water evenly, add 80g of ethyl orthosilicate, then adjust the pH of the system to 5 with acetic acid, stir and react for 5h, then add 5g of KH550, continue stirring for 20h to obtain a nanocomposite sol, spare;

[0041] 2) Preparation of black filler dispersion:

[0042] 2.1) Mix 4.0kg carbon black (primary particle size is 20nm) and 34kg 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 50MPa, and the homogenization time is 30min), to obtain a black dispersion, for subsequent use;

[0043] 2.2) Mix 4.0kg of silicon dioxide (average particle size of 4 μm) and 23kg 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;

[0044] 2.3) Mix the black d...

Embodiment 2

[0048] Repeat Example 1, the difference is:

[0049] In step 3), the amount of PDA added is 0.03 mol, the amount of ODA added is 0.17 mol, and the viscosity of the finally obtained matt black polyamic acid resin solution is 80000 mPa·s.

Embodiment 3

[0051] Repeat Example 1, the difference is:

[0052] Step 2.1) in, the consumption of carbon black is 3.9kg;

[0053] In step 2.2), the consumption of silicon dioxide is 3.9kg;

[0054] In step 3), the amount of PDA added is 0.06 mol, the amount of ODA added is 0.14 mol, and the viscosity of the finally obtained matte black polyamic acid resin solution is 60000 mPa·s.

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Abstract

The invention discloses a low thermal expansion coefficient matt black polyimide film and a preparation method thereof. The preparation method includes: 1) mixing non-metal alkoxide, absolute ethanol and water, adjusting pH=5-7, adding a silane coupling agent to react to obtain a nanocomposite sol; 2) making the solute into a carbon black sol; The black dispersion liquid is mixed with the white dispersion liquid whose solute is a matting agent, and the obtained mixed liquid is dispersed and then added into the nanocomposite sol, and then dispersed to obtain a black filler dispersion liquid; Add black filler dispersion liquid to the PAA resin solution with solid content, and then add or not add stabilizer to obtain a matt black PAA resin solution of specific viscosity; 4) The obtained resin solution is further made into a matt black PI film. The film prepared by the above method has lower thermal expansion coefficient and excellent insulating properties and tensile length, better elongation at break and lower pinhole and bubble rate.

Description

technical field [0001] The invention relates to a polyimide film, in particular to a matt black polyimide film with a low thermal expansion coefficient and a preparation method thereof. Background technique [0002] The matt black polyimide (PI) film contains carbon black and large particle matting agent, and the mechanical properties of the PI film are easily reduced due to poor dispersion. Therefore, in order to make the matte black PI film have sufficient flexibility to ensure the stability of the production process, the molecular structure design of the matrix resin is particularly important. The molecular structure of the base resin of the currently disclosed matte black PI film is mostly PMDA-ODA type. Since the molecular structure of the PMDA-ODA type polyamic acid resin contains -O-flexible ether bonds, the molecules are easily entangled, so the film has good flexibility. , High product continuity in the manufacturing process. However, the thermal expansion coeffic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08K9/10C08K3/04C08K3/36C08K3/22C08K5/526C08J5/18C08G73/10
CPCC08G73/1007C08G73/1071C08J5/18C08J2379/08C08K3/04C08K3/36C08K5/526C08K9/10C08K2003/2241
Inventor 青双桂冯羽风白小庆白蕊刘姣马纪翔冯婷婷
Owner GUILIN ELECTRICAL EQUIP SCI RES INST