Porous polyimide nanometer composite film and preparation method thereof

A polyimide and nanocomposite technology, applied in the field of porous polyimide nanocomposite film and its preparation, can solve the problems of increasing equipment cost and environmental problems, and achieve the effect of avoiding agglomeration

Inactive Publication Date: 2013-12-25
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition of organic solvents improves the ability of polyimide to absorb physical blowing agents, but the introduction of organic solvents in the preparation process will cause environmental problems and increase the cost of equipment

Method used

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  • Porous polyimide nanometer composite film and preparation method thereof
  • Porous polyimide nanometer composite film and preparation method thereof
  • Porous polyimide nanometer composite film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Put 100 grams of N,N-dimethylacetamide solution of polyamic acid with a mass percentage concentration of 20% into a three-necked bottle, then add 20 grams of tetraethyl orthosilicate (TEOS), and then add 3 grams of γ-ammonia Propyltriethoxysilane coupling agent, fully stirred and mixed to form a film. Vacuum the film in a vacuum oven at 80°C for 4 hours to remove the organic solvent, then adopt gradient heating method, keep it at 100°C for half an hour, at 140°C for half an hour, at 160°C for half an hour, at 200°C for 1 hour, and at 240°C Half an hour, heat preservation at 280°C for half an hour, heat preservation at 300°C for 2 hours, imidize the film to prepare a polyimide / nano-silicon dioxide composite film. Put the polyimide / nano-silica composite film into the autoclave, inject carbon dioxide gas into the autoclave, set the temperature in the autoclave to 60°C, and the pressure to 20MPa. Quickly release the pressure to normal pressure, then put it into an oil bath...

Embodiment 2

[0065] Put 100 grams of N,N-dimethylacetamide solution of polyamic acid with a concentration of 20% by mass into a three-necked bottle, then add 16 grams of tetraethyl orthosilicate (TEOS), stir well and mix well to form a film . Vacuum the film in a vacuum oven at 80°C for 4 hours to remove the organic solvent, then adopt gradient heating method, keep it at 100°C for half an hour, at 140°C for half an hour, at 160°C for half an hour, at 200°C for 1 hour, and at 240°C Half an hour, heat preservation at 280°C for half an hour, heat preservation at 300°C for 2 hours, imidize the film to prepare a polyimide / nano-silicon dioxide composite film. Put the polyimide / nano-silica composite film into the autoclave, inject carbon dioxide gas into the autoclave, set the temperature in the autoclave to 30°C, and the pressure to 20MPa. Quickly release the pressure to normal pressure, then put it into an oil bath at 170°C, take it out after 20 seconds of foaming, cool and shape to obtain a p...

Embodiment 3

[0068] First prepare silica sol, add 3.5 grams of tetraethyl orthosilicate (TEOS) to 100 mL of N,N-dimethylacetamide solution and stir for 30 minutes to mix well, then add 0.5 grams of deionized water, and then add hydrochloric acid Adjust the pH value of the mixed solution to 2-3, and reflux the above mixed solution at 80° C. for 2 hours to obtain a uniform and transparent silica sol.

[0069] Put 100 grams of N,N-dimethylacetamide solution of polyamic acid with a concentration of 10% by mass into a three-necked bottle, then add the above-mentioned silica sol into the polyamic acid solution, stir and mix well film forming. Vacuum the film in a vacuum oven at 80°C for 4 hours to remove the organic solvent, then adopt gradient heating method, keep it at 100°C for half an hour, at 140°C for half an hour, at 160°C for half an hour, at 200°C for 1 hour, and at 240°C Half an hour, heat preservation at 280°C for half an hour, heat preservation at 300°C for 2 hours, imidize the film...

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Abstract

The invention discloses a porous polyimide nanometer composite film and a preparation method of the film. The preparation method is characterized by comprising the following steps of: preparing the polyimide composite film by using a sol-gel method, an in-situ polymerization method, a solution direct doping method, and an intercalation hybrid method, placing the composite film into a high-pressure kettle filled with inert gas, and dissolving the gas into the composite film in the presence of the inert gas while keeping the temperature at 30-150 DEG C and the pressure of 5-60MPA for 0.5-12 hours; and rapidly releasing the pressure to the normal pressure to form a lot of foam nuclei on the polyimide / inorganic nanometer particle composite film, and foaming the foam nuclei at the temperature of 150-330 DEG C for 1-60 seconds to obtain the porous polyimide nanometer composite film. The inorganic nanometer particles function as the nucleating agent in the polyimide substrate, not only is the nucleation barrier of the gas reduced, but also the number of the nucleation points is increased, as well as the nucleation points are distributed in the polyimide substrate more uniformly and more stably, so that the obtained micro-pores are smaller in size and more uniform in distribution.

Description

technical field [0001] The invention relates to a porous polyimide nanocomposite film and a preparation method thereof, belonging to the processing field of polymer materials. Background technique [0002] With the rapid development of the microelectronics industry, the functions of microelectronic components continue to increase while the volume continues to decrease, resulting in the continuous reduction of the size of VLSI, while the resistance, capacitance, and delay of metal interconnections continue to increase, resulting in signal transmission. Delay and crosstalk directly affect the performance of the device. In order to reduce the increase in power consumption caused by signal transmission delay and dielectric loss, and to meet the high-speed transmission of signals, the insulating material between the dielectric layers is required to have a lower dielectric constant. [0003] Polyimide has excellent dielectric properties, mechanical properties, radiation resistanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K3/36C08K3/22C08K3/04C08K3/34C08K3/24C08K3/26C08J9/12C08J5/18
Inventor 刘鹏波李晓文吴东森邹华为
Owner SICHUAN UNIV
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