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Polyimide high dielectric composite material and preparation method thereof

A technology of composite material and polyimide, which is applied in the field of polyimide high dielectric composite material and its preparation, can solve problems such as the degradation of the internal structure and performance of composite materials, and achieve improved dielectric properties, easy removal, and reduced volume fractional effect

Active Publication Date: 2013-09-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the non-modified nano-barium titanate filled polymer reaches a certain amount, it will inevitably lead to defects in the internal structure of the composite material and a decrease in performance.

Method used

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  • Polyimide high dielectric composite material and preparation method thereof
  • Polyimide high dielectric composite material and preparation method thereof
  • Polyimide high dielectric composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method of polyimide high dielectric composite material, comprising the following steps:

[0044] (1) Modification of graphene oxide

[0045] ① Take 100mg of graphite oxide and add it to the mixed solution of 20ml thionyl chloride and 0.5ml anhydrous dimethylformamide, peel it off by ultrasonic for 30min; under the protection of nitrogen, under the temperature condition of 70℃, react gently for 24 hours , obtain the acid chloride product of graphite oxide;

[0046] Excess thionyl chloride was removed by distillation under reduced pressure.

[0047]② Add 50ml of anhydrous dimethylformamide to the reaction product obtained in step (1)①, seal it and ultrasonically disperse it for later use; dissolve 0.5g of p-phenylenediamine in 10ml of anhydrous dimethylformamide and inject it into the reaction device. Reacted at 120° C. for 24 hours under the protection of nitrogen, suction-filtered, washed, and dried in vacuum at 60° C. for 12 hours to obtain graphene fu...

Embodiment 2

[0056] A preparation method of polyimide high dielectric composite material, comprising the following steps:

[0057] (1) Modification of graphene oxide

[0058] ① Take 200mg of graphite oxide and add it to the mixed solution of 40ml thionyl chloride and 2ml anhydrous dimethylformamide, and peel it off by ultrasonic for 60min; Obtain the acid chloride product of graphite oxide;

[0059] Excess thionyl chloride was removed by distillation under reduced pressure.

[0060] ② Add 100ml of anhydrous dimethylformamide to the reaction product obtained in step (1) ①, seal and ultrasonically disperse for later use; dissolve 1g of p-phenylenediamine in 10ml of anhydrous dimethylformamide and inject into the reactor , reacted at 100° C. for 24 hours under the protection of nitrogen, suction-filtered, washed, and dried in vacuum at 60° C. for 24 hours to obtain graphene functionalized with p-phenylenediamine.

[0061] (2) Preparation of polyamic acid prepolymer

[0062] ① Take 143mg (...

Embodiment 3

[0069] A preparation method of polyimide high dielectric composite material, comprising the following steps:

[0070] (1) Modification of graphene oxide

[0071] ① Add 100mg of graphite oxide to a mixed solution of 20ml of thionyl chloride and 0.5ml of anhydrous dimethylformamide, and peel it off by ultrasonic for 40min; Obtain the acid chloride product of graphite oxide;

[0072] Excess thionyl chloride was removed by distillation under reduced pressure.

[0073] ② Add 50ml of anhydrous dimethylformamide to the reaction product obtained in step (1) ①, seal and ultrasonically disperse for later use; dissolve 1g of p-phenylenediamine in 10ml of anhydrous dimethylformamide and inject into the reactor ; Under the protection of nitrogen, react at 80°C for 48 hours, filter the generated product, wash, and vacuum dry at 70°C for 12 hours to obtain graphene functionalized with p-phenylenediamine.

[0074] (2) Preparation of polyamic acid prepolymer

[0075] ① Take 30mg (0.5wt%) o...

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Abstract

The present invention relates to a polyimide high dielectric composite material, wherein polyimide is adopted as a matrix phase, modified graphene and nanometer barium titanate are adopted as inorganic phases, components comprise, by mass, 0.5-3.0 w% of modified graphene, 9.6-29.8 w% of nanometer barium titanate, and 69.7-87.4 w% of polyimide, the modified graphene is p-phenylenediamine graft modified graphene, and the surface of the modified graphene contains chemically grafted polyimide. The preparation method comprises the following steps: (1) graphene oxide modification, (2) polyamic acid prepolymer preparation, and (3) composite material thermal cross-linking. According to the preparation method, the functionalized graphene and the polyimide molecules can be combined through a covalent bond form, electric conductivity of the graphene can directly affect dielectric property of the composite material, and a volume fraction of the barium titanate can be effectively reduced. In addition, the conventional solution blending technology is adopted, the preparation process is simple, operation is easy, and the method can be widely promoted and applied.

Description

technical field [0001] The invention relates to the technical field of electronic functional materials, specifically, polyimide is jointly modified by graphene and barium titanate, and a polyimide high-dielectric composite material and a preparation method thereof are provided. Background technique [0002] With the continuous development and progress of society, people's demand for energy is increasing, and the most effective use of energy has become a matter of concern to everyone. In terms of effective use of electric energy, in order to store and utilize electric energy quickly and effectively, people have developed supercapacitors. In the manufacture of supercapacitors, dielectric materials are very important. In this regard, polymer-based high-k dielectric composites are ideal capacitor dielectric materials, which can be widely used in fields requiring electrical energy storage materials. [0003] In terms of dielectric materials, graphene is a two-dimensional planar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K9/04C08K3/04C08K3/24C08G73/10C08J5/18C08J3/24
Inventor 庄启昕何剑杰毛晓阳李欣欣钱军刘小云韩哲文
Owner EAST CHINA UNIV OF SCI & TECH
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