Preparation method for polyimide thin film

A technology of polyimide film and polyamic acid, which is applied in the field of preparation of partially cross-linked polyimide film, can solve the problems of low thermal conductivity of graphite film and the need to improve the thermal conductivity of graphite film, and achieve simple process, The effect of improving thermal conductivity

Inactive Publication Date: 2016-01-13
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the thermal conductivity of the graphite film obtained after the domestic PI film is graphitized at a high temperature of 3000°C is much lower than that of the DuPont PI film.
[0009] At present, the process of preparing graphite heat dissipation film by sintering polyimide film is becoming more and more mature, but the thermal conductivity of the prepared graphite film still needs to be improved, especially the production technology of domestic polyimide film needs to be developed.

Method used

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  • Preparation method for polyimide thin film
  • Preparation method for polyimide thin film
  • Preparation method for polyimide thin film

Examples

Experimental program
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Effect test

Embodiment 1

[0031](1) Under nitrogen protection at 20-25°C, weigh 6g of 4,4'-diaminodiphenyl ether (ODA) and 0.1337g of 3,3'-diaminobenzidine (TAB) into 50ml of N-methylpyrrolidone (NMP ), dissolved under mechanical stirring. After complete dissolution, lower the reaction system below 5°C, add 3g of pyromellitic anhydride (PMDA) while stirring, and rinse the inner wall of the device with 10ml of NMP. After reacting for 1.5 h, add 3 g of PMDA while stirring, and rinse the inner wall of the device with 10 ml of NMP. After reacting for 1.5 h, add 0.5 g PMDA while stirring, and rinse the inner wall of the device with 10 ml NMP. At this time, the viscosity of the system began to rise. After 2 hours of reaction, 0.2 g of PMDA was added while stirring. After 2 hours, the reaction system formed a viscous polyamic acid solution. At this time, the total amount of the added dianhydride PMDA was 6.7 g. The molar ratio of the amount of tetraamine TAB to the amount of diamine ODA in this system is 0...

Embodiment 2

[0034] (1) Under nitrogen protection at 20-25°C, weigh 6g of 4,4'-diaminodiphenyl ether (ODA) and 0.2049g of 3,3'-diaminobenzidine (TAB) into 50ml of N-methylpyrrolidone (NMP ), dissolved under mechanical stirring. After complete dissolution, lower the reaction system below 5°C, add 3g of pyromellitic anhydride (PMDA) while stirring, and rinse the inner wall of the device with 10ml of NMP. After reacting for 1.5 h, add 3 g of PMDA while stirring, and rinse the inner wall of the device with 10 ml of NMP. After reacting for 1.5 h, add 0.5 g PMDA while stirring, and rinse the inner wall of the device with 10 ml NMP. At this time, the viscosity of the system began to rise, and after 2 hours of reaction, 0.2 g of PMDA was added. After 2 hours, the reaction system formed a viscous polyamic acid solution. At this time, the total amount of the added dianhydride PMDA was 6.7 g. The molar ratio of the amount of tetraamine TAB to the amount of diamine ODA in this system is 0.03:0.94, ...

Embodiment 3

[0043] (1) Under nitrogen protection at 20-25°C, weigh 1.1573g of 4,4'-diaminodiphenyl ether (ODA), 2.50g of p-phenylenediamine (PDA) and 0.11g of 1,3,5-triaminobenzene Dissolve in 50ml N,N-dimethylacetamide (DMAc) under mechanical stirring. After complete dissolution, lower the reaction system below 5°C, add 4g of 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA) while stirring, and rinse the inner wall of the device with 10ml of DMAc. After reacting for 1.5 h, add 2 g of BPDA while stirring, and rinse the inner wall of the device with 10 ml of DMAc. After 1.5 h of reaction, 2.00 g of BPDA was added, and the inner wall of the device was washed with 10 ml of DMAc. After reacting for 2 hours, add 0.6g BPDA, and rinse the inner wall of the device with 10ml DMAc. After 2h, the reaction system formed a viscous polyamic acid solution. At this time, the total amount of dianhydride BPDA added was 8.6 g. The molar ratio of the amount of 1,3,5-triaminobenzene to the amount of di...

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Abstract

The invention discloses a preparation method for a polyimide thin film comprising a local crosslinking structure. The polyimide thin film comprising the local crosslinking structure is prepared by the steps: by selecting an aromatic organic dianhydride monomer and an aromatic organic diamine monomer and matching with a small amount of polyamine monomer, firstly synthesizing polyamide acid comprising partial crosslinking structure; then coating the polyamide acid; and then carrying out thermal imidization. The preparation method disclosed by the invention is simple in process of preparing the polyimide thin film and graphite film. A conventional polyimide thin film preparation process is not changed, a trace amount of polyamine serving as a local crosslinking core is added to an original formula of preparing polyimide to synthesize the polyimide thin film comprising the local crosslinking structure, so that a good effect on the prepared graphite film can be obtained, and therefore, the heat conductivity of the graphite film is improved.

Description

technical field [0001] The invention relates to a method for preparing a partially cross-linked polyimide film, which belongs to a method for preparing a film. Background technique [0002] Due to its many excellent properties, polyimide has become a promising main material in cutting-edge technical fields such as aviation, aerospace, electronics, nuclear power, communications and automobiles. [0003] Traditional polyimide films are generally formed by polycondensation of aromatic diamines and aromatic dianhydrides in extremely strong solvents, followed by imidization. At present, the preparation technology of this polyimide is very mature, but due to the limitation of its molecular structure, the strength and other properties of this type of polyimide film still need to be improved. [0004] With the continuous development of science and technology, heat dissipation has become the key to the development of many fields. Traditional high thermal conductivity materials are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
Inventor 徐勇李宣虞立立李林霜曾皓张晶晶
Owner NANJING UNIV OF SCI & TECH
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