Method for preparing polyimide/ silicon dioxide hollow micro-sphere composite film

A technology of silica and hollow microspheres, which is applied in the field of organic-inorganic hybrid material preparation, can solve the problems of difficult processing, easy hydrolysis, large thermal expansion coefficient, etc., and achieves the effect of reducing the dielectric constant

Inactive Publication Date: 2008-02-20
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it has disadvantages such as too high melting point, insoluble in most organic solvents, difficult processing, easy hydrolysis, large thermal expansion co...

Method used

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  • Method for preparing polyimide/ silicon dioxide hollow micro-sphere composite film
  • Method for preparing polyimide/ silicon dioxide hollow micro-sphere composite film
  • Method for preparing polyimide/ silicon dioxide hollow micro-sphere composite film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of silica hollow microspheres:

[0025] Add 5g of styrene, 1.5g of polyvinylpyrrolidone (PVP), 5g of water, 0.2g of azobisisobutyronitrile (AIBN) and 22.5g of ethanol into a 250mL four-necked flask, and stir for 30 minutes under nitrogen protection. After raising the temperature to 70-80°C for 1-2 hours, quickly add 5g of styrene, 22.5g of ethanol and 1-4g of methacryloyloxyethyltrimethylammonium chloride (MTC), under nitrogen protection After reacting for 25 hours, cool to 50°C, then add 6-12g tetraethyl orthosilicate (TEOS) and 1-4mL ammonia water to react for 1 hour, and centrifuge to obtain hollow silica microspheres with a particle size of 200-1000nm.

[0026] Fig. 1 and Fig. 2 are the electron micrographs of the silica hollow microspheres prepared by this method, and it can be clearly seen that the silica microspheres prepared by this method are indeed hollow. The hollow microspheres introduced in this way utilize the dielectric constant of air to be ...

Embodiment 2

[0028] Preparation of polyimide / silica hollow microsphere composite film:

[0029] 10 g of silicon dioxide hollow microspheres were added to 105 ml of ethanol solution with a mass concentration of 95%. Use 50W, 40kHz ultrasonic to disperse for 20 minutes every hour, then add 2g of silane coupling agent, stir and react at 60°C for 5h, stirring speed is 500-1000 rpm, centrifuged at 4500 rpm 10 minutes, wash, dry.

[0030] 0.52g of 2,2-bis[4-(3',4'-dicarboxyphenoxy)phenyl]propane dianhydride (BPADA) and 0.438g of bis[3,5-dimethyl-4 -(4-Amino)phenol]methane (BDAPM) was added to 8.622 g of N-methyl-2-pyrrolidone (NMP) to prepare a solution with a solid content of 10% (wt / wt). Add 0.1064g of silica hollow microspheres modified by a silane coupling agent, the silica hollow microspheres being 10% of the mass of the composite film, into the above NMP solution, disperse with 50W, 40kHz ultrasound, and at room temperature The reaction was continuously stirred for 24 hours to obtain a ...

Embodiment 3

[0032] 10 g of silicon dioxide hollow microspheres were added to 105 ml of ethanol solution with a mass concentration of 95%. After ultrasonic dispersion, 2 g of silane coupling agent was added, stirred and reacted at 80°C for 5 hours at a stirring speed of 500-1000 rpm, centrifuged at 4500 rpm for 10 minutes, washed and dried.

[0033]0.444g of 4,4'-(hexafluoropropylene)bis-phthalic anhydride (6FDA) and 0.438g of BDAPM were added to 7.938g of NMP to prepare a solution with a solid content of 10% (wt / wt). Add 0.378g of silica hollow microspheres modified by a silane coupling agent, the silica hollow microspheres being 30% of the mass of the composite film, into the above NMP solution, disperse with 50W, 40kHz ultrasound, and at room temperature The reaction was continuously stirred for 24 hours to obtain a polyamic acid viscous liquid. Take an appropriate amount of polyamic acid viscous solution and pour it on the glass plate mold. Place the mold at 80° C. for 2 hours in vac...

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Abstract

The invention discloses a method for preparing polyimide/silicon dioxide hollow microballoon laminated film which has low dielectric constant and keeps thermal property, and steps of reaction are that: silicon dioxide hollow microballoon is put into ethanol solution, amino-containing silane coupling agent is added after ultra sonic dispersion, stirred for reaction, separated centrifugally, washed and dried; then under the protection of nitrogen flow, the dianhydride and the diamine with a mole-ratio 1:1 are added into the high boiling polarity aprotic solvent to prepare solvent containing 10 percent (wt/wt) of solid-content; the silicon dioxide hollow microballoon modified by silane coupling agent is put into the solvent, and the weight of the silicon dioxide hollow microballoon modified by the silane coupling agent is 2-50 percent of the weight of laminated film, the polyamide acid viscous fluid is prepared upon ultra sonic dispersion and a reaction of twenty-four hours at room temperature; the polyamide acid viscous fluid is taken and poured into the glass plate mould; finally the mould is put in vacuum to dry, the temperature is heated up continuously after the solvent is removed for cyclic reaction. Thus, the polyimide/silicon dioxide hollow microballoon laminated film is prepared..

Description

technical field [0001] The invention belongs to the field of preparation of organic-inorganic hybrid materials, in particular to the preparation of polyimide / silicon dioxide composite film. Background technique [0002] Polyimide (PI) is a kind of polymer material with high temperature resistance, low temperature resistance, radiation resistance, excellent chemical stability and good mechanical strength. It has been widely used in aerospace, electrical and electronic and other high-tech fields. However, it has disadvantages such as high melting point, insoluble in most organic solvents, difficult processing, easy hydrolysis, large coefficient of thermal expansion, high cost and the like. However, PI with a general dielectric constant of about 3.1-3.5 is far from meeting the dielectric constant value required by submicron devices. [0003] Nano-hybrid materials are the fourth generation of materials after single-component materials, composite materials, and shaved functional...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08K9/06C08J5/18C08K3/36C08K5/541C08K5/09
Inventor 林保平袁媛
Owner SOUTHEAST UNIV
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