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Graphene induced polyimide oriented crystallization based high-thermal-conductivity graphite film preparation method

A high thermal conductivity graphite, polyimide technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problem of unsatisfactory thermal conductivity and mechanical properties of graphite film, affecting the thermal conductivity and electrical conductivity, flexibility and mechanical properties of graphite film. Strength can not meet the requirements and other problems, to achieve the effect of reducing amorphous defects, improving thermal conductivity and mechanical properties, and reducing the temperature of graphitization process

Inactive Publication Date: 2019-10-08
ZHEJIANG FORST NEW MATERIAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two main methods of preparing graphite film: one is to press artificial graphite into a film, which is easy to operate, but the prepared graphite film is not ideal in terms of thermal conductivity and mechanical properties, especially the flexibility and strength cannot meet the requirements; The second is to use the graphitization of polymer film to directly prepare graphite film. The graphite film prepared by this method generally has good flexibility and thermal conductivity, but it consumes a lot of energy during the high-temperature graphitization process, and it is easy to produce a large amount of incomplete graphite. Defects in the amorphous state seriously affect the thermal and electrical conductivity of the graphite film

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 88L DMF, 7.5g graphene oxide, 0.15g KH550 to the reaction kettle in sequence, and mechanically stir the reaction at 5°C for 2h. 20mol 1,4,5,8-naphthalenetetracarboxylic dianhydride and 20mol p-phenylenediamine were sequentially added to the above reaction system, and reacted at 5°C for 2h under the protection of nitrogen to obtain a graphene hybrid polyamic acid solution. Add 7.5 g of pyridine to the graphene hybrid polyamic acid solution, stir the solution for 1 hour, and then use a casting machine to cast the graphene hybrid polyamic acid solution at room temperature to form a film, and then bake the film at 40°C. Dry, and react at 70° C. for 5 min to obtain a graphene hybrid polyimide film, and then use a peeling device to peel the graphene hybrid polyimide film from the casting carrier tape. After the obtained graphene hybrid polyimide film is peeled off, it is further subjected to a two-way stress stretching process. The stretching process is: a temperature of 8...

Embodiment 2

[0024] 60L DMF, 100g graphene oxide, 3g KH550 were sequentially added to the reaction kettle, and the reaction was mechanically stirred at 20°C for 6h. In the above reaction system, 20 mol 1,4,5,8-naphthalenetetracarboxylic dianhydride and 20 mol p-phenylenediamine were sequentially added, and reacted at 25° C. for 6 hours under the protection of nitrogen to obtain a graphene hybrid polyamic acid solution. Add 120g of pyridine to the graphene hybrid polyamic acid solution, stir the solution for 1 hour, then use a casting machine to cast the graphene hybrid polyamic acid solution at room temperature to form a film, and then dry the film at 50°C , And then react at 90° C. for 50 minutes to obtain a graphene hybrid polyimide film, and then use a peeling device to peel the graphene hybrid polyimide film from the casting carrier tape. After the obtained graphene hybrid polyimide film is peeled off, it is further subjected to a two-way stress stretching process, the stretching proces...

Embodiment 3

[0026] 30L DMF, 376g graphene oxide, 18.8g KH550 were sequentially added into the reaction kettle, and the reaction was mechanically stirred at 30°C for 12h. 20mol 1,4,5,8-naphthalenetetracarboxylic dianhydride and 20mol p-phenylenediamine were sequentially added to the above reaction system, and reacted at 30°C for 16h under the protection of nitrogen to obtain a graphene hybrid polyamic acid solution. Add 150.4g of pyridine to the graphene hybrid polyamic acid solution, stir the solution for 5 hours, and then use a casting machine to cast the graphene hybrid polyamic acid solution at room temperature to form a film, and then bake the film at 60°C. Dry, and react at 160° C. for 90 minutes to obtain a graphene hybrid polyimide film, and then use a peeling device to peel the graphene hybrid polyimide film from the casting carrier tape. After the obtained graphene hybrid polyimide film is peeled off, it is further subjected to a two-way stress stretching process. The stretching p...

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Abstract

The invention provides a graphene induced polyimide oriented crystallization based high-thermal-conductivity graphite film preparation method. According to the preparation method, a graphene and polyimide composite material serves as graphite film precursor, and in a high-temperature carbonization and graphitization process, graphene serves as an orientation and crystallization inducing agent to promote graphitization of polyimide to prepare a high-thermal-conductivity graphite film. Flaky nano graphene oxide introduced into the graphite film has an intrinsic crystalline graphitized carbon structure and can be used as a graphitized carbon template in a stretching and graphitization process to induce a polyimide molecular orientation and graphitized carbon crystallization process, amorphousform defects in the graphitization process are reduced, and accordingly thermal conductivity and mechanical properties of the graphite film are improved. The high-thermal-conductivity graphite film prepared according to the method is high in graphite crystallization degree, flexibility and thermal conductivity and meets the requirement of high thermal dissipation in the microelectronic industry.

Description

Technical field [0001] The invention relates to the field of thermally conductive films, in particular to a method for preparing a highly thermally conductive graphite film in which graphene induces polyimide orientation crystallization. Background technique [0002] With the rapid development of modern microelectronics industry and high-frequency and high-speed communication technology, electronic equipment and integrated circuits are developing in the direction of miniaturization and high-density. Miniature high-density interconnect (HDI) integrated circuits have become one of the future development trends . In HDI, the density of wires and electronic components is greatly increased, and the locally generated heat rapidly accumulates and increases, which has a negative impact on the service life of electronic components, and at the same time affects the stability and reliability of the components. In addition, in high-frequency and high-speed communication systems, the heat ge...

Claims

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Application Information

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IPC IPC(8): C01B32/205C08L79/08C08K9/06C08K3/04C08J5/18
CPCC01B32/205C08J5/18C08J2379/08C08K3/042C08K9/06
Inventor 曹春李伟杰周光大林建华
Owner ZHEJIANG FORST NEW MATERIAL RES INST CO LTD
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