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Polyimide film and preparation method thereof

A technology of polyimide film and polyamic acid, which is applied in the field of polyimide film and its preparation, can solve problems such as low mechanical properties, particle agglomeration, and decreased mechanical properties, so as to achieve good mechanical properties and improve thermal conductivity , evenly dispersed effect

Active Publication Date: 2013-07-10
株洲时代华鑫新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there are also some problems at the same time. If micron-sized aluminum nitride with a larger particle size is used to fill it, it is easy to realize in technology, and the thermal conductivity of the obtained polyimide film will be improved, but the surface of the prepared film is rough; Grade aluminum nitride filling is prone to particle agglomeration. Although the thermal conductivity of the prepared polyimide film has improved, the mechanical properties will decrease, which is not conducive to popularization and application.
[0004] The Chinese patent with the publication number CN101168598 discloses a method for preparing an ultra-thick polyimide film with high thermal conductivity and low thermal expansion coefficient. The thermal conductivity of the polyimide film is improved by filling aluminum nitride, but its mechanical properties Not high, and the preparation is ultra-thick polyimide film, the applicability is not strong

Method used

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preparation example Construction

[0022] The invention provides a kind of preparation method of polyimide film, comprises the following steps:

[0023] Mix and grind thermally conductive fillers, solvents and coupling agents to obtain slurry;

[0024] Diamine and dianhydride are reacted in a solvent to obtain polyamic acid resin;

[0025] Mixing the slurry and polyamic acid resin, defoaming, and casting to obtain a polyamic acid film;

[0026] Imidating the polyamic acid film to obtain a polyimide film;

[0027] The thermally conductive filler includes a first thermally conductive filler with a particle size of 100nm-200nm, a second thermally conductive filler with a particle size of 50nm-100nm, and a third thermally conductive filler with a particle size of 10nm-50nm.

[0028] In the present invention, the thermally conductive filler, solvent and coupling agent are firstly mixed and ground to obtain a slurry; the thermally conductive filler preferably includes a first thermally conductive filler with a part...

Embodiment 1

[0042] 1kg of 3-aminopropyltriethoxysilane, N, N-dimethylacetamide 100kg, 35kg of aluminum nitride with an average particle diameter of 200nm, 10kg of aluminum nitride with an average particle diameter of 100nm, and an average particle diameter of 5kg of 50nm aluminum nitride, mixed evenly by a high-speed disperser, then transferred to a horizontal sand mill for grinding, and the dispersion and distribution of nano-aluminum nitride were detected by a particle size analyzer. When the polydispersity index is less than 1.05, the grinding is stopped, and the slurry is obtained.

[0043] Stir to dissolve 43.06kg of 4,4'-diaminodiphenyl ether and 360kg of N,N-dimethylacetamide to obtain a mixed solution, then gradually add 46.94kg of pyromellitic dianhydride to the above solution In, obtain the polyamic acid resin that viscosity is 60000CP.

[0044] Add 30 kg of the slurry into the above polyamic acid resin, stir and mix evenly to obtain the polyamic acid resin filled with aluminum...

Embodiment 2

[0047] 1kg of 3-aminopropyltriethoxysilane, N, N-dimethylacetamide 100kg, 35kg of aluminum nitride with an average particle diameter of 200nm, 10kg of aluminum nitride with an average particle diameter of 100nm, and an average particle diameter of 5kg of 50nm aluminum nitride, mixed evenly by a high-speed disperser, then transferred to a horizontal sand mill for grinding, and the dispersion and distribution of nano-aluminum nitride were detected by a particle size analyzer. When the polydispersity index is less than 1.05, the grinding is stopped, and the slurry is obtained.

[0048] Stir to dissolve 43.06kg of 4,4'-diaminodiphenyl ether and 360kg of N,N-dimethylacetamide to obtain a mixed solution, then gradually add 46.94kg of pyromellitic dianhydride to the above solution , Obtaining the polyamic acid resin that viscosity is 50000CP.

[0049] Add 20kg of the slurry into the above polyamic acid resin, stir and mix evenly to obtain the polyamic acid resin filled with aluminum...

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Abstract

The invention provides a preparation method of a polyimide film. The preparation method comprises the following steps of mixing and grinding a heat-conducting padding, a solvent and a coupling agent to obtain slurry; enabling diamine and dianhydride to react in a solvent, so as to obtain polyimide resin; mixing, defoaming and casting the slurry and the polyimide resin to obtain a polyamic acid film; conducting imidization on the polyamic acid film to obtain the polyimide film, wherein the heat-conducting padding includes a first heat-conducting padding of which the particle size is 100-200nm, a second heat-conducting padding of which the particle size is 50-100nm and a third heat-conducting padding of which the particle size is 10-50nm. The heat-conducting padding adopted by the polyimide film is different in particle size, so that the maximal packing degree is formed between the heat-conducting padding; an effective heat-conducting channel is formed; the heat-conducting property of the polyimide film is improved; the heat-conducting padding can be evenly dispersed in the solvent in a grinding manner; the prepared polyimide film is even to disperse, high in stability, and good in mechanical property in the presence of the coupling agent.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a polyimide film and a preparation method thereof. Background technique [0002] Polyimide film is a new type of organic polymer film, which is made of pyromellitic dianhydride (PMDA) and diaminodiphenyl ether (ODA) in a very strong solvent N,N-dimethylacetamide ( DMAC) by polycondensation and casting into a film, and then by imidization. It is currently the best thin film insulating material in the world, with excellent mechanical properties, electrical properties, chemical stability, radiation resistance, high temperature resistance and low temperature resistance. Polyimide film also has low dielectric properties, which can reduce the interconnection delay, crosstalk and energy consumption of VLSI, so it has high research value in packaging materials and dielectric layers. However, the thermal conductivity of polyimide film is only 0.16W / (m·K), which limits its appl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K3/28C08K3/34C08G73/10C08J5/18C08K9/06
Inventor 王文进张步峰廖波周升
Owner 株洲时代华鑫新材料技术有限公司
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