Preparation method of thermal conductive film based on graphene polyimide composite sponge precursor

A polyimide precursor, ene polyimide technology, is applied in the field of preparation of a thermal conductive film based on a graphene polyimide composite sponge precursor, and achieves the effects of reducing grain boundary scattering, improving electrical conductivity, and reducing interface thermal resistance.

Active Publication Date: 2019-12-10
SHENZHEN STRONG ADVANCED MATERIALS RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above technical problems, the present invention discloses a method for preparing a thermally conductive film based on a graphene polyimide composite sponge precursor, which solves the problems existing in the existing graphene composite film in terms of mechanical properties and electrical and thermal conductivity

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  • Preparation method of thermal conductive film based on graphene polyimide composite sponge precursor
  • Preparation method of thermal conductive film based on graphene polyimide composite sponge precursor
  • Preparation method of thermal conductive film based on graphene polyimide composite sponge precursor

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Experimental program
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Effect test

Embodiment 1

[0059] A thermally conductive film based on graphene / polyimide composite sponge precursor is prepared by the following steps, and the schematic diagram of the preparation process is as follows: figure 1 Shown:

[0060] 1. Preparation of graphene oxide aqueous solution: measure 20mL graphene oxide slurry, add deionized water; under the condition of stirring speed of 700r / min, after stirring for 60min; and at a frequency of 100KHz, perform ultrasonic treatment for 30min to obtain Graphene oxide aqueous solution.

[0061] Wherein, the concentration of the graphene oxide slurry is 20 mg / mL; the concentration of graphene oxide in the graphene oxide aqueous solution is 5 mg / mL.

[0062] 2. Preparation of polyimide precursor solution:

[0063] Using an electromagnetic stirrer, 1.98g of monomeric diamine diaminodiphenyl ether (ODA) powder was uniformly dispersed in 83mL of polar solvent dimethylacetamide (DMAc) solution; 2.18g of dianhydride was continuously added to the mixed solut...

Embodiment 2

[0083]A thermally conductive film based on graphene / polyimide composite sponge precursor is prepared by the following steps:

[0084] 1. Preparation of graphene oxide aqueous solution:

[0085] Measure 20 mL of graphene oxide slurry, add deionized water; stir for 60 min at a stirring speed of 700 r / min; and perform ultrasonic treatment for 30 min at a frequency of 100 KHz to obtain a graphene oxide aqueous solution.

[0086] Wherein, the concentration of the graphene oxide slurry is 20 mg / mL; the concentration of graphene oxide in the graphene oxide aqueous solution is 5 mg / mL.

[0087] 2. Preparation of polyimide precursor solution:

[0088] Using an electromagnetic stirrer, 1.98g of monomeric diamine diaminodiphenyl ether (ODA) powder was uniformly dispersed in 83mL of polar solvent dimethylacetamide (DMAc) solution; 2.18g of dianhydride was continuously added to the mixed solution in small amounts Pyromellitic anhydride (PMDA) powder, stirred for 5h to make it fully react...

Embodiment 3

[0106] A thermally conductive film based on graphene / polyimide composite sponge precursor is prepared by the following steps:

[0107] 1. Preparation of graphene oxide aqueous solution:

[0108] Measure 20 mL of graphene oxide slurry, add deionized water; stir for 120 min at a stirring speed of 100 r / min; and perform ultrasonic treatment for 60 min at a frequency of 10 KHz to obtain a graphene oxide aqueous solution.

[0109] Wherein, the concentration of the graphene oxide slurry is 20 mg / mL; the concentration of graphene oxide in the graphene oxide aqueous solution is 4 mg / mL.

[0110] 2. Preparation of polyimide precursor solution:

[0111] Using an electromagnetic stirrer, 1.98g of monomeric diamine diaminodiphenyl ether (ODA) powder was uniformly dispersed in 83mL of polar solvent dimethylacetamide (DMAc) solution; 2.18g of dianhydride was continuously added to the mixed solution in small amounts Pyromellitic anhydride (PMDA) powder, after stirring 5h to make it fully r...

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Abstract

The invention provides a preparation method of a thermal conductive film based on a graphene polyimide composite sponge precursor. The preparation method comprises the following steps that a grapheneoxide water solution is mixed with a polyimide precursor solution to obtain a graphene oxide/polyamide acid mixed solution, then the graphene oxide/polyamide acid mixed solution is frozen to obtain agraphene oxide/polyamide acid frozen sponge, a frozen drying method is adopted for drying to obtain a graphene oxide/polyamide acid composite sponge, the graphene oxide/polyamide acid composite spongeis placed in a hot pressing reactor, hot pressing oxidizing pre-processing is adopted and machinery pressuring is conducted to obtain a reduced graphene oxide/polyamide acid composite film, then vacuum hot processing and machinery pressuring are adopted to obtain a graphene/polyimide carbon film, then the graphene/polyimide carbon film is placed in a high-temperature graphitization furnace, and agradient temperature rising method is adopted to achieve graphitization of the carbon film. According to the technical scheme of the preparation method, the problem of dispersion of graphene is improved, the obtained film has a certain flexibility and high mechanical strength, and has better electrical and thermal conductivity, and the preparation technology is simple.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and in particular relates to a method for preparing a thermally conductive film based on a graphene-polyimide composite sponge precursor. Background technique [0002] Today, with the advancement of science and technology, the lightweight and highly integrated development of modern military equipment is facing increasingly severe thermal management challenges. For example, in electronic weapons, ultra-high-speed aircraft, remote sensing satellites, radars and other equipment, large-scale The high integration of high-power electronic components will cause serious heat concentration problems, which poses a fatal threat to the working stability, safety and reliability of key components of military equipment. At the same time, the complex thermal interface in highly integrated equipment also puts forward unique requirements on the flexibility of thermal management materials. [0003] Wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/524C04B35/622
CPCC04B35/524C04B35/522C04B35/622C04B2235/6562C04B2235/6567C04B2235/96C04B2235/9607
Inventor 彭庆宇祝越赫晓东
Owner SHENZHEN STRONG ADVANCED MATERIALS RES INST CO LTD
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