Benzodiacyclic dianhydride and low-dielectric-constant polyimide precursor film

A polyimide precursor, polyimide film technology, applied in the direction of organic chemistry, can solve the problems of mechanical properties and glass transition temperature reduction, difficult to meet 5G high-frequency high-speed communication, affecting performance, etc. Achieve the effects of low thermal expansion coefficient, low dielectric loss, and low water absorption

Inactive Publication Date: 2019-06-21
ZHEJIANG FORST NEW MATERIAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, pure polyimide has a high dielectric constant (3.4), which is difficult to meet the requirements of 5G high-frequency and high-speed communication, so it is necessary to develop new low dielectric constant PI materials
At present, there are many ways to reduce the dielectric constant of PI. For example, Chinese patent CN 105461924B uses fluorine-containing PI to reduce the molar polarizability of molecules and reduce the dielectric constant of PI, but the cost is extremely high; Chinese patent CN 104211980B prepares porous PI film, using the low dielectric constant of air to degrade the dielectric constant of PI film, but the mechanical properties and glass transition temperature are greatly reduced, which affects the performance

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0033] The polyamic acid solution is prepared according to a known method. 1mol of p-phenylenediamine is fully dissolved in N,N dimethylacetamide, and then 0.95mol of dianhydride a is quickly added to the solution, and under the protection of an inert gas React at 25° C. for 1 h, then add 0.5 wt % (accounting for the total mass) of nanoporous silica (50 nm) with surface amination, and stir rapidly for 2 h. The mass fraction of the total solid content of the final diamine, dianhydride and silicon dioxide is 25wt%. The preparation process of the polyimide film is as follows: a) film coating, the polyamic acid precursor solution is coated on the copper foil substrate by spin coating. b) Imidization, dry the coated substrate at 60°C for 12 hours; then program the temperature rise, and treat it at 150°C, 200°C, and 250°C for 60 minutes; finally raise the temperature to 350°C for 10 minutes, and the imidization reaction It needs to be carried out under nitrogen atmosphere. c) Stre...

Embodiment 2

[0035] The polyamic acid solution was prepared according to a known method, 1mol of 2,2'-bis(trifluoromethyl)benzidine was fully dissolved in N,N dimethylacetamide, and then 1mol of dianhydride a was quickly added to solution, and reacted at 30° C. for 0.5 h under the protection of an inert gas, and then added 0.2 wt % (accounting for the total mass) of nanoporous silicon dioxide (25 nm) with surface fluorination, and stirred rapidly for 4 h. The mass fraction of the total solid content of the final diamine, dianhydride and silicon dioxide is 20wt%. The preparation process of the polyimide film is as follows: a) film coating, the polyamic acid precursor solution is coated on the copper foil substrate by spin coating. b) Imidization, dry the coated substrate at 50°C for 12 hours; then program the temperature rise, and treat it at 150°C, 200°C, and 250°C for 60 minutes; finally raise the temperature to 350°C for 15 minutes, and the imidization reaction It needs to be carried ou...

Embodiment 3

[0037]The polyamic acid solution is prepared according to a known method, 1mol of 3,4-diaminodiphenyl ether is fully dissolved in N,N dimethylacetamide, and then 0.99mol of dianhydride b is quickly added to the solution, And react at 20°C for 1h under the protection of inert gas. The mass fraction of the total solid content of the final diamine, dianhydride and silicon dioxide is 25wt%. The preparation process of the polyimide film is as follows: a) film coating, the polyamic acid precursor solution is coated on the copper foil substrate by spin coating. b) Imidization, dry the coated substrate at 60°C for 10 hours; then program the temperature rise, and treat it at 150°C, 200°C, and 250°C for 75 minutes; finally raise the temperature to 350°C for 20 minutes, and the imidization reaction It needs to be carried out under nitrogen atmosphere. c) Stress relief, control the cooling rate to 5°C / min until room temperature. Finally, the polyimide film was peeled off from the coppe...

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Abstract

The invention discloses a benzodiacyclic dianhydride and low-dielectric-constant polyimide precursor film. The preparation method comprises the following steps: completely dissolving diamine into an aprotic polar solvent; adding benzodiacyclic dianhydride and performing reaction at the temperature of -10 to 35 DEG C for 0.5 to 5 hours under the protection of nitrogen or inert gas to obtain a polyimide precursor solution; coating a base material with the polyimide precursor solution, and performing imidization and stress relief to prepare the low-dielectric-constant polyimide precursor film. The polyimide precursor film prepared by the method has low dielectric constant, low dielectric loss and low water-absorbing rate, and still has low dielectric constant and low dielectric loss after absorbing water; furthermore, the polyimide precursor film has excellent heat stability and mechanical property and can meet the requirement on dielectric materials by 5G communication and high-frequencyhigh-speed electronic industry.

Description

technical field [0001] The invention relates to the field of polymer materials, and relates to a novel polyimide precursor resin with low dielectric constant, a film and its application in the electronic industry. Background technique [0002] With the rapid development of electronic equipment in recent years, the size of printed circuit boards tends to be light, thin, short, and small. Due to the high-speed and high-frequency of 4G and 5G communication products, high-frequency substrates with fast information transmission rates have gradually become the focus of development. As the materials used in 5G communication high-frequency communication substrates, electromagnetic information must be transmitted quickly, and signal loss and interference are required to be very low during transmission to ensure the reliability of signal transmission. [0003] In order to reduce the time delay and loss of signal transmission, the dielectric constant and dielectric loss of the basic di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04C08L79/08C08G73/10C08J5/18
Inventor 曹春李伟杰周光大林建华
Owner ZHEJIANG FORST NEW MATERIAL RES INST CO LTD
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