Polyimide/graphite hybrid material with high dielectric constant and preparation method thereof

A high dielectric constant, polyimide technology, used in multilayer capacitors, thin film/thick film capacitors, etc., can solve the problems of flexibility and mechanical properties of composite materials, and maintain flexibility and excellent mechanical properties. The effect of low content and high dielectric constant

Inactive Publication Date: 2013-12-25
TORAY FIBER RES INST(CHINA) CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiencies of polymer composite materials in the prior art, the present invention provides a high dielectric constant polyimide / graphite hybrid material, so as to provide high dielectric constant composite materials while overcoming existing polymer composite materials. The deficiencies in the flexibility and mechanical properties of composite materials due to the high content of inorganic substances

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  • Polyimide/graphite hybrid material with high dielectric constant and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0035] (1) Add 0.053g of natural flake graphite, sodium nitrate, and potassium permanganate into 98% concentrated sulfuric acid placed in an ice bath, keep stirring for 1 hour, and prevent the temperature of the mixture from exceeding 20°C. The ice bath was removed, and the mixture was kept in a water bath at 35°C for 4 hours. Dilute with deionized water and keep the mixture at 90°C for 15 minutes. Then dilute with deionized water, add hydrogen peroxide and filter while hot. Wash with deionized water until SO-free 4 2- ions to obtain 0.10g graphite oxide.

[0036] (2) 0.10g of graphite oxide was dispersed in 81ml of N-methylpyrrolidone, and ultrasonically dispersed for 15 hours at room temperature to make it uniformly dispersed to become a graphite oxide dispersion;

[0037] (3) Under the protection of an inert gas, add 5.0g of 4,4'-diaminodiphenyl ether (ODA) into the above-mentioned graphite oxide dispersion, stir, and slowly add 5.6g of pyromellitic acid to it after dis...

Embodiment 2

[0045] (1) According to the method in the embodiment 1 step (1), 0.082g of natural flake graphite was oxidized and exfoliated to obtain 0.164g of graphite oxide.

[0046] (2) 0.032g of graphite oxide is dispersed in 84ml of N,N-dimethylacetamide, and ultrasonicated for 3 hours at room temperature to make it uniformly dispersed to become a graphite oxide dispersion;

[0047] (3) Under the protection of an inert gas, add 2.7g m-phenylenediamine (MPD) into the above-mentioned graphite oxide dispersion, stir, and slowly add 8.2g 3,3',4,4'-bis benzophenone tetra-acid dianhydride (BTDA); after the addition is completed, react at 27° C. for 15 hours under the protection of an inert gas to obtain a polyamic acid / graphite hybrid solution;

[0048] (4) The obtained polyamic acid / graphite hybrid solution is formed into a film on a stainless steel plate, and after an imidization reaction at 320°C for 3 hours, a polyimide / graphite with a graphite content of 0.75% is obtained hybrid membra...

Embodiment 3

[0055] (1) According to the method in the embodiment 1 step (1), 0.204g of natural flake graphite was oxidized and peeled off to obtain 0.40g of graphite oxide.

[0056] (2) 0.40g of graphite oxide is dispersed in 78ml of N-methylpyrrolidone, and ultrasonicated for 9 hours at room temperature to make it uniformly dispersed to become a graphite oxide dispersion;

[0057] (3) Under the protection of an inert gas, add 2.7g of p-phenylenediamine (PPD) into the above-mentioned graphite oxide dispersion, stir, and slowly add 7.5g of 3,3',4,4'-linked pyromellitic dianhydride (BPDA); after the addition is complete, react at 20°C for 20 hours under the protection of an inert gas to obtain a polyamic acid / graphite hybrid solution;

[0058] (4) The obtained polyamic acid / graphite hybrid solution is formed into a film on a stainless steel plate, and after an imidization reaction at 350°C for 3 hours, a polyimide / graphite with a graphite content of 2% is obtained hybrid membrane.

[0059...

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Abstract

The invention belongs to the field of an organic / inorganic hybrid material and discloses a polyimide / graphite hybrid material with high dielectric constant and a preparation method thereof. The hybrid material consists of dianhydride monomer, diamine monomer and graphite, wherein the mass content of the graphite in the hybrid is 0.1-3%, and the molar ratio of the diamine monomer to the dianhydride monomer is 1:1-1.20. The graphite is uniformly dispersed in a polyimide substrate in a lamellar structure, and the thickness of the graphite lamella is 1-20 nanometers. According to the preparation method, the polyimide / graphite hybrid material with high dielectric constant can be obtained, the content of inorganic substances is low and the original flexibility and excellent mechanical performance of the polyimide substrate is maintained by the hybrid material. The polyimide / graphite hybrid material can be applied to embedded high-capacity film capacitors.

Description

technical field [0001] The invention belongs to the field of organic / inorganic hybrid materials, in particular to a novel high dielectric constant polyimide / graphite hybrid material and a preparation method thereof. Background technique [0002] High dielectric constant materials are one of the core materials for power and electronic devices, and are mainly used in embedded film capacitors. With the gradual shrinking of the VLSI size, embedded capacitors are required to achieve overall packaging, reduce the size of the circuit, and increase the degree of integration. At present, the high dielectric constant materials used in capacitors are mostly inorganic ceramic materials. Although they have extremely high dielectric constants, the process of forming requires high-temperature firing above 700°C. The process is complicated, and the obtained materials are poor in flexibility and easy to crack; and The substrates of embedded capacitors are mostly organic polymer materials, w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08K9/02C08K3/04H01G4/33
Inventor 陈桥吴祯祺吴刚
Owner TORAY FIBER RES INST(CHINA) CO LTD
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