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Preparation method of heat conduction film

A heat-conducting film and organic polymer technology, which is applied in the field of graphene heat-conducting film preparation, can solve the problems of inability to peel off graphene aggregate powder, high temperature peeling temperature, unfavorable slurry preparation, etc., and achieve wide reaction conditions , stable reaction process, large size effect

Active Publication Date: 2020-12-04
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, graphite oxide is dried and exfoliated into few-layer graphene powder. The disadvantage of this preparation method is that the high-temperature exfoliation temperature is high, the energy consumption is large, and after thermal exfoliation, the dispersibility of the product is poor, and the graphene powder is dispersed. It has been agglomerated before, and it is impossible to separate the graphene aggregate powder after redispersion, which is not conducive to the preparation of subsequent slurry.

Method used

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Examples

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preparation example Construction

[0027]This application provides a method for preparing a thermally conductive film, which includes the following steps:

[0028]Step S1: polymerizing the organic polymer monomer and free radical initiator in an aqueous solution to obtain a first product.

[0029]In one embodiment, add 1 to 10 parts of organic polymer monomer to 50 to 200 parts of aqueous solution and stir at 20 to 95°C for 10 to 60 minutes to disperse the organic polymer monomer uniformly to obtain the organic polymer monomer Dispersions. Adding a free radical initiator to the organic polymer monomer dispersion to initiate polymerization of the organic polymer monomer, wherein the number of parts by which the free radical initiator initiates the polymerization of the organic polymer monomer is the mass part of the organic polymer monomer 0.1 to 2.0wt.‰ of the number; make the organic polymer monomer dispersion with the free radical initiator polymerize in a water bath at 20 to 90°C for 1 to 8 hours, and then add ammonia t...

Embodiment 1

[0061]Add 1.2 ml of acrylic acid and 1.25 g of acrylamide mixed organic polymer monomer to 100 ml of distilled water at room temperature, and heat and stir in a 35° C. water bath for 15 minutes to obtain a uniformly mixed organic polymer monomer dispersion. Weigh 0.02g each of potassium persulfate and sodium bisulfite, and add 2ml of distilled water to prepare an aqueous initiator solution. Take out 1 / 3 of each of the initiator aqueous solution, slowly drop it into the organic polymer monomer dispersion, stir and raise the temperature to 45°C, add the remaining initiator aqueous solution multiple times within 1 hour, and polymerize for 4 hours; After stirring down to room temperature, the pH value is quickly adjusted to 7-8 with an aqueous ammonia solution to obtain the first product.

[0062]Add 3g of graphite oxide to the first product, and use a high-pressure homogenizer for homogeneous dispersion, crushing and peeling, until graphene oxide with an average thickness of 0.4-0.7nm and...

Embodiment 2

[0067]Add 1.5 g of acrylic acid and 1.0 g of organic polymer monomer mixed with 1.0 g of methyl propyl butyl in 200 ml of distilled water at room temperature, and heat and stir in a 35° C. water bath for 15 minutes to obtain a uniformly mixed organic polymer monomer dispersion. Weigh 0.04 g of ammonium persulfate and add 4 ml of distilled water to prepare an aqueous initiator solution. Take out 1 / 3 of each of the initiator aqueous solution, slowly drop it into the organic polymer monomer dispersion, stir and raise the temperature to 45°C, add the remaining initiator aqueous solution multiple times within 1 hour, and polymerize for 4 hours; After stirring down to room temperature, the pH value is quickly adjusted to 7-8 with an aqueous ammonia solution to obtain the first product.

[0068]Add 8g of graphite oxide to the first product, and use a high-pressure homogenizer for homogeneous dispersion, crushing and peeling, until graphene oxide with an average thickness of 0.4-0.7nm and an a...

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Abstract

The invention provides a preparation method of a heat conduction film. The preparation method comprises the following steps: pre-polymerizing an organic polymer monomer and a radical initiator in an aqueous solution to obtain a first product; adding graphite oxide into the first product, and carrying out dispersion treatment on the graphite oxide to obtain a second product; adding an inorganic acid into the second product to adjust the pH value of the mixed solution to be less than or equal to 3 to flocculate the second product, and separating the obtained flocculate to obtain organic polymermodified graphite oxide precursor slurry; and coating the surface of a base material with the slurry, and drying; after drying, stripping the dried substance on the surface of the base material to obtain a slurry dry film; carrying out heat treatment and reduction treatment on the slurry dry film to obtain a thermal reduction film; heating the thermal reduction film to 1000-1200 DEG C at a first heating rate in an inert atmosphere, heating the thermal reduction film to 2600-3000 DEG C at a second heating rate after heat preservation is completed, and obtaining a high-temperature carbonized film after heat preservation is completed; and carrying out physical shaping treatment on the high-temperature carbonized film to obtain the heat conduction film.

Description

Technical field[0001]The invention belongs to the technical field of thermal conductive film preparation, and specifically relates to a method for preparing a graphene thermal conductive film.Background technique[0002]As the electronics industry, new energy vehicles, LED and other industries have increasingly higher requirements for safe heat dissipation, traditional thermal interface materials are gradually being replaced by new thermal materials due to their own limitations. Graphene is a material with a single-atom layered structure composed of carbon atoms in a hexagonal honeycomb lattice. As a new type of two-dimensional nano-carbon material, graphene has excellent properties and characteristics, such as electrical properties (electron mobility at room temperature) Up to 15000cm2·V-1·S-1), mechanical properties (in ideal conditions, Young’s vector 1TPa, intensity 130GPa), optical properties (visible light region transmittance of more than 97%), high specific surface area (2630m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19C09K5/14C08F220/06C08F220/14C08F220/18C08F220/56
CPCC01B2204/24C08F220/06C08F220/56C09K5/14C01B32/19C08F220/14C08F220/1804
Inventor 杜鸿达褚晓东姚有为陈威康飞宇李宝华
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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