Method for preparing high thermal conductivity graphite film by using graphene-doped polyamic acid resin

A technology of polyamic acid resin and high thermal conductivity graphite, which is applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc. It can solve the problems of low production efficiency, poor thermal conductivity of carbonized film, and unexamined thermal conductivity of graphite film, etc. , to achieve the effect of reducing production cost and production cycle, significant economic and social benefits, and shortening graphitization time

Active Publication Date: 2017-06-16
株洲时代华鑫新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production of polyimide film in my country adopts the thermal imidization film-making process. Compared with the foreign chemical imidization film-making process, the production efficiency is low (about 1/6 of the chemical imidization method), and the thermal dimensional stability is poor. Low strength and low thermal stability. The precursor PI base film produced by this process is cracked during high temperature carbonization, the surface is wrinkled and dull, the thermal conductivity is low, and it is not resistant to folding, which cannot meet the film production requirements of high thermal conductivity graphite film process.
[0007] CN103080005A Chinese patent document discloses a method for preparing a graphite film with less graphite powder from a polyimide film. This method belongs to the traditional sintering of a polyimide film to prepare a graphite film. Amine film sintered graphite fi

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  • Method for preparing high thermal conductivity graphite film by using graphene-doped polyamic acid resin

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Embodiment 1

[0033] A kind of method utilizing graphene-doped polyamic acid resin of the present invention to prepare high thermal conductivity graphite film may further comprise the steps:

[0034] (1) Graphene (graphene is graphene oxide or graphene oxide obtained by the Humers method) is added to the strong polar organic solvent DMAc, ultrasonically dispersed for 60min, and the concentration obtained is prepared as a 0.1wt% graphene dispersion;

[0035] (2) Diamine ODA and dianhydride PMDA are added respectively in the graphene dispersion liquid that step (1) makes in equimolar ratio and carry out stirring reaction, and specific operation mode is: first diamine ODA monomer is once added to In the graphene dispersion, after being fully dissolved, the dianhydride PMDA monomer is added in batches as the stirring reaction proceeds, and the reaction is stirred for 6 hours in an ice-water bath and under the protection of an inert gas to obtain an in-situ polymerization with a solute concentrat...

Embodiment 2

[0040] A kind of method utilizing graphene-doped polyamic acid resin of the present invention to prepare high thermal conductivity graphite film may further comprise the steps:

[0041] (1) Graphene (graphene is graphene oxide or graphene oxide obtained by the Humers method) is added in the strong polar organic solvent DMF, ultrasonically dispersed for 60min, and the prepared concentration is 2wt% graphene dispersion;

[0042] (2) Diamine PDA and dianhydride BPDA are added respectively in the graphene dispersion liquid that step (1) makes in equimolar ratio and carry out stirring reaction, and specific operation method is: first diamine PDA monomer is once added to In the graphene dispersion, after being fully dissolved, the dianhydride BPDA monomer is added in batches along with the stirring reaction, and the reaction is stirred for 6 hours in an ice-water bath and under the protection of an inert gas to obtain an in-situ polymerization with a solute concentration of 20wt%. G...

Embodiment 3

[0047] A kind of method utilizing graphene-doped polyamic acid resin of the present invention to prepare high thermal conductivity graphite film may further comprise the steps:

[0048] (1) Graphene (graphene is graphene oxide or graphene oxide obtained by the Humers method) is added in the strong polar organic solvent DMF, ultrasonically dispersed for 60min, and the prepared concentration is 5wt% graphene dispersion;

[0049] (2) Diamine PDA, ODA and dianhydride ODPA, BPDA are respectively added to the graphene dispersion prepared in step (1) in an equimolar ratio to carry out stirring reaction. The specific operation method is: first equimolar diamine Add PDA and ODA monomers to the graphene dispersion at one time. After fully dissolving, add equimolar dianhydride ODPA and BPDA monomers in batches as the stirring reaction proceeds. Under the protection of ice-water bath and inert gas, Stirring and reacting for 6h to obtain an in-situ polymerized graphene-doped polyamic acid ...

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Abstract

The present invention discloses a method for preparing a high thermal conductivity graphite film by using a graphene-doped polyamic acid resin. The method comprises: adding graphene to a strongly polar organic solvent, and carrying out ultrasonic dispersion to prepare a graphene dispersion; respectively adding diamine and dianhydride to the graphene dispersion, and carrying out a stirring reaction to obtain a graphene-doped polyamic acid resin solution obtained through in situ polymerization; adding an imidization reagent, sequentially carrying out deaeration and casting film forming, carrying out crystallization orientation by using two-way stretching equipment, and carrying out high temperature imidization treatment to obtain a graphene-doped polyimide composite film; carrying out high temperature carbonization on the film under vacuum, and naturally cooling to a room temperature to obtain a carbonized film; and finally carrying out high temperature graphitization under argon gas protection, and naturally cooling to a room temperature to obtain the high thermal conductivity graphite film.

Description

technical field [0001] The invention relates to a chemical imidization method for preparing a film, in particular to a method for preparing a graphite film by using graphene-doped polyamic acid resin. Background technique [0002] The heat dissipation performance of electronic products is one of the important performances that consumers pay attention to. In recent years, the miniaturization and thickness reduction of electronic products such as notebook computers has become a design trend. With the thinning of smart electronic products, this puts forward more stringent requirements for the heat dissipation of electronic products, and also brings thermal design engineers. This posed a huge challenge, which required new and effective thermal solutions to keep the surface temperature of the notebook even and free of "hot spots". [0003] Carbon materials have ultra-high thermal conductivity. According to molecular dynamics simulation calculations, the thermal conductivity of g...

Claims

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Application Information

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IPC IPC(8): C01B32/205C08G73/10
Inventor 高敬民刘媛彭博江乾张步峰姜其斌
Owner 株洲时代华鑫新材料技术有限公司
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