Preparation method of thermally conductive film

A heat-conducting film and organic polymer technology, 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, poor product dispersibility, etc., and achieve wide reaction conditions, The effect of stable reaction process and excellent thermal conductivity

Active Publication Date: 2021-09-28
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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preparation example Construction

[0027] The application provides a method for preparing a thermally conductive film, comprising the following steps:

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

[0029] In one embodiment, 1 to 10 parts of the organic polymer monomer are added to 50 to 200 parts of the aqueous solution, and stirred at 20 to 95° C. for 10 to 60 minutes to disperse the organic polymer monomer evenly to obtain the organic polymer monomer Dispersions. Adding a free radical initiator to the organic high molecular monomer dispersion liquid initiates the polymerization of the organic high molecular monomer, wherein, the number of parts of the organic high molecular monomer polymerization initiated by the free radical initiator is the mass part of the organic high molecular monomer 0.1 to 2.0 wt.‰ of the number of parts; make the organic polymer monomer dispersion added with a free radical initiator polymer...

Embodiment 1

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

[0062] Add 3g of graphite oxide to the first product, 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 methyl propyl butyl ester into 200 ml of distilled water at room temperature, and keep stirring in a water bath at 35° C. 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 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 in several times within 1 hour, and polymerize for 4 hours; then After stirring down to room temperature, quickly adjust the pH value to 7-8 with ammonia solution to obtain the first product.

[0068] Add 8g of graphite oxide to the first product, 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 average sheet diameter of 0.8-10μm is obtai...

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Abstract

The invention provides a method for preparing a heat conduction film, comprising the following steps: prepolymerizing an organic polymer monomer and a free radical initiator in an aqueous solution to obtain a first product; adding graphite oxide to the first product and dispersing the graphite oxide processing to obtain a second product; adding an inorganic acid to the second product, adjusting the pH value of the mixed solution to be less than or equal to 3, causing the second product to flocculate, and separating the obtained flocs to obtain an organic polymer modified graphite oxide precursor slurry; The slurry is applied to the surface of the substrate and dried. After drying, the dried material on the surface of the substrate is peeled off to obtain a dried slurry film; the dried slurry film is subjected to heat treatment and reduction treatment to obtain a thermally reduced film; the thermally reduced film is heated to 1000 °C at a first heating rate under an inert atmosphere. After the heat preservation is completed, the temperature is raised to 2600 to 3000°C at the second heating rate. After the heat preservation is completed, a high-temperature carbonized film is obtained; the high-temperature carbonized film is subjected to physical shaping treatment to obtain a heat-conducting film.

Description

technical field [0001] The invention belongs to the technical field of heat-conducting film preparation, and in particular relates to a method for preparing a graphene heat-conducting film. Background technique [0002] As the electronic industry, new energy vehicles, LED and other industries have higher and higher requirements for safe heat dissipation, traditional thermal interface materials are gradually replaced by new thermal conductive 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 15000cm 2 ·V -1 ·s -1 ), mechanical properties (Young's vector 1TPa, intensity 130GPa under ideal conditions), optical properties (light transmittance in the visible light region is over 97%), hig...

Claims

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Application Information

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Patent Type & Authority Patents(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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