Preparation method of high-modulus high-thermal-conductivity polyimide film

A polyimide film, polyamic acid technology, applied in the direction of semiconductor/solid-state device manufacturing, semiconductor devices, semiconductor/solid-state device components, etc. Conductivity improvement is limited and other issues

Active Publication Date: 2020-10-20
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a preparation method of high modulus and high thermal conductivity polyimide film, to overcome the modulus and thermal conductivity of polyimide film prepared by blending modification technology in the prior art The defects of limited improvement and difficulty in large-scale development

Method used

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  • Preparation method of high-modulus high-thermal-conductivity polyimide film
  • Preparation method of high-modulus high-thermal-conductivity polyimide film
  • Preparation method of high-modulus high-thermal-conductivity polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042](1) Under nitrogen protection, in a three-necked flask, add 50mL of NMP, 2.76g (0.0133mol) of anthracene-2,6-diamine (Beijing Dingsheng Brothers Technology Co., Ltd., purity 99%), 4.12g ( 0.014mol) of 3,3',4,4'-biphenyltetraacid dianhydride (BPDA) (Changzhou Sunshine Pharmaceutical Co., Ltd., 99.5%), fully stirred and reacted for 12 hours, and controlled the reaction temperature at 2°C to obtain anhydride-terminated polymer Amic acid oligomer-I solution. Under nitrogen protection, in a three-necked flask, successively add 50 mL of NMP, 2.98 g (0.0133 mol) of 5-amino 2-(4-aminophenyl)-benzimidazole (BIA) (Changzhou Sunshine Pharmaceutical Co., Ltd., Purity 99%), 3.70g (0.0126mol) of 3,3',4,4'-biphenyl tetraic acid dianhydride (BPDA) (Changzhou Sunshine Pharmaceutical Co., Ltd., 99.5%), fully stirred for 12 hours, and controlled the reaction temperature to At 2°C, an amino-terminated polyamic acid oligomer-II solution was obtained. Stir and mix the oligomer-I solution an...

Embodiment 2

[0046] (1) The preparation of the anhydride-terminated polyamic acid oligomer-I solution is the same as in Example 1. According to Example 1, change "2.98g (0.0133mol) of 5-amino 2-(4-aminophenyl)-benzimidazole (BIA)" to "2.99g (0.0133mol) of 5-amino 2-( 4-aminophenyl)-benzoxazole (BOA) (Changzhou Sunshine Pharmaceutical Co., Ltd., purity 99%)", and the rest are the same as in Example 1 to obtain amino-terminated polyamic acid oligomer-II solution. Stir and mix the oligomer-I solution and the oligomer-II solution in a nitrogen atmosphere, and react at 5°C for 12 hours to obtain a block-structured polyamic acid precursor solution with an apparent viscosity of 4980cP·s (25°C) , molecular structure such as image 3 shown.

[0047] (2) The polyamic acid precursor solution in step (1) was cast into a film under the same conditions as in Example 1 to obtain a cured polyamic acid precursor film. Continue thermal cyclization and bidirectional thermal drawing treatment on the cured ...

Embodiment 3

[0050] (1) According to Example 1, change "2.76g (0.0133mol) of anthracene-2,6-diamine" to "3.16g (0.0133mol) of 2,6-diamino-anthraquinone (Cobant Chemical Industry (Hangzhou) Co., Ltd., purity 99%) ", all the other are identical with embodiment 1, obtain anhydride-terminated polyamic acid oligomer-I solution. According to Example 1, change "2.98g (0.0133mol) of 5-amino 2-(4-aminophenyl)-benzimidazole (BIA)" to "2.99g (0.0133mol) of 5-amino 2-( 4-aminophenyl)-benzoxazole (BOA) (Changzhou Sunshine Pharmaceutical Co., Ltd., purity 99%)", and the rest are the same as in Example 1 to obtain amino-terminated polyamic acid oligomer-II solution. Stir and mix the oligomer-I solution and the oligomer-II solution in a nitrogen atmosphere, and react at 5°C for 12 hours to obtain a block-structured polyamic acid precursor solution with an apparent viscosity of 4280cP·s (25°C) , molecular structure such as Figure 4 shown.

[0051] (2) The polyamic acid precursor solution in step (1) wa...

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Abstract

The invention relates to a preparation method of a high-modulus high-thermal-conductivity polyimide film. The preparation method comprises the following steps: mixing diamine containing anthryl or anthraquinone units, a dianhydride monomer and a solvent, and carrying out a polymerization reaction to obtain an anhydride structure-terminated oligomer-I solution; mixing diamine containing a benzimidazole or benzoxazole unit, a dianhydride monomer and a solvent, and carrying out a polymerization reaction to obtain a diamine-terminated oligomer-II solution; mixing the oligomer-I solution with the oligomer-II solution, carrying out a polymerization reaction, casting the obtained polyamide acid solution with a block structure to form a film, and then carrying out thermal cyclization and bidirectional stretching. The method can realize continuous preparation, is simple to operate and environment-friendly in process, is beneficial to large-scale preparation of the intrinsic high-modulus high-thermal-conductivity polyimide film, and has a good industrialization prospect.

Description

technical field [0001] The invention belongs to the field of polyimide film preparation, in particular to a preparation method of a polyimide film with high modulus and high thermal conductivity. Background technique [0002] In recent years, with the rapid development of flexible optoelectronic technology, polyimide films are widely used in flexible optoelectronic devices and flexible printed circuit boards as flexible polymer substrates and dielectric insulating materials. During the processing of electronic devices or circuit boards, polyimide films usually need to be bonded or laminated to the surface of other metal sheets (such as copper plates) or inorganic materials (such as silicon chips). In order to ensure the quality of optoelectronic devices, polyimide films are usually required to have high modulus characteristics to avoid serious problems such as deformation and warping during processing. In addition, with the continuous improvement of the integration of micro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18H01L51/50H01L23/373C08L79/08
CPCC08G73/1085C08G73/1007C08J5/18H01L23/3737C08J2379/08H10K77/111H10K50/00Y02E10/549
Inventor 张清华董杰赵昕郑森森甘锋
Owner DONGHUA UNIV
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