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Preparation method of porous low-dielectric polyimide thin films

A technology of polyimide film and low dielectric is applied in the field of organic film preparation, which can solve the problems of high cost and complicated production of polyimide film, and achieve the effect of simple and easy-to-obtain raw materials.

Active Publication Date: 2015-09-16
HANGZHOU NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problem of complex and high cost of low dielectric constant polyimide film in the prior art, and to provide a low dielectric constant, high strength and strong thermal stability polyimide film. Preparation

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  • Preparation method of porous low-dielectric polyimide thin films

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of calcium carbonate suspension

[0031] Adopt Shanxi Ruicheng Warner Nano Material Co., Ltd. to produce 4.5kg of nano-calcium carbonate with a particle size of 100nm, add it into the aprotic solvent DMAc, under the condition of 40kHz ultrasonic dispersion, stir at a speed of 2000r / min, fully stir for 30min, and make a stable Suspension, ensure that the mass concentration of calcium carbonate suspension is 5%.

[0032] (2) Preparation of polyamic acid composite solution

[0033] Add the suspension obtained above into the polyamic acid polymerization reactor, add a sufficient amount of solvent, control the temperature at 40°C, add 20kg of ODA, and carry out mechanical stirring. After it is completely dissolved, control the temperature at 60°C, divide Add 21.8 kg of PMDA in an equimolar ratio to diamine in small batches, and keep stirring to fully react the diamine and dianhydride to form a polyamic acid composite solution with stable viscosity. The mass...

Embodiment 2

[0039] (1) Preparation of calcium carbonate and silica suspension

[0040] Adopt Shanxi Ruicheng Warner Nano Material Co., Ltd. to produce 2.5kg of nano-calcium carbonate with a particle diameter of 40nm, and 4.5kg of nano-silicon dioxide (produced by West Asia Reagent) with a particle diameter of 40nm, add in the aprotic solvent DMAc, and disperse with 60kHz ultrasonic waves Under the conditions, the stirring speed is 3000r / min and the mixture is fully stirred for 60min to form a stable suspension, ensuring that the mass concentration of nano-calcium carbonate and silicon dioxide is 20%.

[0041] (2) Preparation of polyamic acid composite solution

[0042]Add the suspension obtained above into the polyamic acid polymerization reaction kettle, add solvent, control the temperature at 10°C, add 20kg of ODA, and carry out mechanical stirring. After it is completely dissolved, control the temperature at 50°C, batch by batch Add 21.8 kg of PMDA in an equimolar ratio to the diamine...

Embodiment 3

[0048] (1) Preparation of calcium carbonate and silica suspension

[0049] Adopt Shanxi Ruicheng Warner Nano Material Co., Ltd. to produce 1kg of nano-calcium carbonate with a particle diameter of 20nm and 10kg of nano-silicon dioxide (produced by West Asia Reagent) with a particle diameter of 100nm, add in 160kg of aprotic solvent DMAc, 100kHz ultrasonic dispersion conditions Under 2000r / min stirring speed, fully stirred for 60min to make a stable suspension, ensuring that the mass concentration of calcium carbonate and silicon dioxide is 15%.

[0050] (2) Preparation of polyamic acid composite solution

[0051] Add the suspension obtained above into the polyamic acid polymerization reactor, add a sufficient amount of solvent, control the temperature at 25°C, add 16kg of ODA and 4kg of MDA, and perform mechanical stirring. After it is completely dissolved, control the temperature at 25°C. At 55°C, add 21.8 kg of PMDA in an equimolar ratio to diamine in batches, and keep stir...

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Abstract

The invention belongs to the organic film preparation field, and relates to a preparation method of porous low-dielectric polyimide thin films. The method includes the following steps: (1) preparation of a reinforcing filler suspension; (2) preparation of a polyamide acid compound solution; (3) preparation of polyimide thin films; and (4) obtaining of the porous polyimide thin films. Calcium carbonate is used as a pore-forming agent raw material, the calcium carbonate is removed by dilute hydrochloric acid to obtain the porous thin films, raw materials are simple and are easy to obtained, and complex operations are not needed; at the same time, the pore size and porosity of the thin films can be controlled directly through control of the particle size and content of the calcium carbonate, and various porous low-dielectric polyimide thin films with excellent performance are prepared, can be applied in substrate materials of electrician and electronic industries and are especially suitable for electronic materials of large-scale integrated circuits.

Description

technical field [0001] The invention belongs to the field of organic film preparation, and relates to a preparation method of a porous low-dielectric polyimide film. Background technique [0002] With the rapid development of electronic information technology, the integration of VLSI devices is getting higher and higher, and its feature size is shrinking, which will cause resistance-capacitance delay to increase, signal transmission delay, interference enhancement, and power loss increase. and other issues, which will limit the high-speed performance of the device. One of the important ways to alleviate this problem is to reduce the dielectric constant of the dielectric material—that is, to reduce the parasitic capacitance of the material. Polyimide is widely used in the microelectronics industry because of its outstanding high and low temperature resistance and dielectric properties, such as chip packaging materials, shielding materials, and substrate materials for flexibl...

Claims

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Application Information

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IPC IPC(8): C08J9/26C08G73/10C08K3/36C08J5/18
Inventor 宋艳江吕亮刘顺祯
Owner HANGZHOU NORMAL UNIVERSITY
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