Preparation method for black polyimide (PI) film

A technology of black polyimide and polyamic acid, which is applied in the field of preparation of black polyimide film, to achieve the effects of stable thermal performance, good insulation performance and excellent mechanical performance

Active Publication Date: 2012-11-21
江苏南方贝昇光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The film preparation process of this method is simple and easy, and it is convenient for mass production, but there is also the problem of halogenated polyimide black film

Method used

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  • Preparation method for black polyimide (PI) film
  • Preparation method for black polyimide (PI) film
  • Preparation method for black polyimide (PI) film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Stir well-dried 5.9287g of carbon black, 0.3016g of silane coupling agent (KH550), and 100g of absolute ethanol at 20°C, and react ultrasonically for 3 hours at a frequency of 40KHz. After the reaction, the filler particles are washed, ground, and dried. stand-by.

[0038] Weigh 11.9657g of 4,4'-diaminodiphenyl ether (ODA), dissolve it in 75.0027g of N,N'-dimethylacetamide (DMAc), stir evenly at 20°C, and then add ODA in 3 batches The pyromellitic anhydride (PMDA) of molar weight is altogether 13.0342g, continues to stir, and along with the continuous dissolving of dianhydride monomer, the viscosity of polymer also constantly increases, after monomer all dissolves, continue to stir at normal temperature 3h, prepare A PAA solution with a solid content (mass fraction) of 25% was obtained. Weigh 5.0097 g of the above-mentioned treated carbon black and add it into the PAA solution, stir and sonicate at 15° C. for 0.5 h at a frequency of 80 KHz.

[0039] Dip-coat the compo...

Embodiment 2

[0041] Stir well-dried 5.9880g of carbon black, 0.436g of silane coupling agent (KH570) and 120g of absolute ethanol at 10°C, and ultrasonically react for 5 hours at a frequency of 20KHz. After the reaction, the filler particles are washed, ground, and dried. stand-by.

[0042] Weigh 5.2004g of carbon black into 79.9986g of N,N'-dimethylacetamide (DMAc) solvent, stir ultrasonically at 18°C ​​for 3h at ultrasonic frequency 25KHz, add 5.6723g of 4,4'-diaminodiphenyl ether ( ODA), after it is completely dissolved, add a total of 9.1277g of dianhydride monomer 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA) in an equimolar amount to ODA in 5 batches, and continue stirring for 2h , to prepare a PAA / carbon black composite solution with a solid content (total mass of filler and PAA) of 20%.

[0043] Dip-coat the PAA / carbon black composite solution on a glass plate, put it into a vacuum oven to raise the temperature step by step, and the heating rate is 4°C / min (100°C×60min, 210°C...

Embodiment 3

[0045] Stir 5.606g of fully dried graphite, 0.1128g of silane coupling agent (KH560) and 140g of absolute ethanol at 0°C, and ultrasonically react for 4 hours at an ultrasonic frequency of 60KHz. After the reaction, the filler particles are washed, ground, and dried. use.

[0046] Weigh 3.9605g graphite into 88.0012g N,N'-dimethylacetamide (DMAc) solvent, stir ultrasonically for 0.5h at 28°C, ultrasonic frequency 100KHz, add 4.7208g octylated diphenylamine (ODPA), wait After it was completely dissolved, a total of 3.3192 g of dianhydride monomer pyromellitic anhydride (PMDA) in an equimolar amount to ODPA was added in 7 batches, and stirring was continued for 12 hours to obtain a solid content (total mass of filler and PAA) of 12%. PAA / carbon black composite solution.

[0047] Dip-coat the PAA / filler composite solution on a stainless steel casting plate, put it into a vacuum oven to raise the temperature step by step, and the heating rate is 3°C / min (120°C×30min, 180°C×90min,...

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Abstract

The invention provides a preparation method for a black polyimide (PI) film. Diamine, dianhydride and black stuffing are taken as raw materials. An addition method is provided with two, one method is that the black stuffing after being processed by coupling agent is added into polyamide acid solution for fully and uniformly mixing up, and the mixture is subjected to a tape casting method to form a film; and the other method is that polyamide acid (PAA) black composite solution is prepared via an in-situ polymerization method, and black PI film is obtained after the solution is subjected to a heat imidization treatment. The prepared PI black film has the advantages of simpleness in operation, excellent process, uniform color and remarkable uniformity of the product. The black PI film can be used as a black covering film, a black static electricity prevention film, a black anti-shielding material and the like, and has wide application in fields of a light-emitting diode (LED), a flexible printed circuit board and the like.

Description

technical field [0001] The invention relates to a method for preparing a black polyimide film, in particular to preparing a black covering film by adding black fillers. Background technique [0002] Black PI film has a long history and is widely used. For example: black tape, black anti-static tape, black reinforcing plate, black cover film, black speaker voice coil, black label, black gasket, black light-shielding sheet, black anti-shielding material, black sound diaphragm, LCD module binding and Substituting a large number of black PEI films, etc. Black cover film is one of the series products of black PI film. Compared with ordinary cover film, it is opaque, does not reflect backlight, has good confidentiality, uniform color, and excellent product consistency. It can be used for LED lighting, interference printed circuit boards, etc. . [0003] As far as the preparation technology of the black cover film is concerned, there are two commonly used methods: one is to coat...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08K9/06C08G73/10
Inventor 黄培吕亮
Owner 江苏南方贝昇光电材料有限公司
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