Preparation method for graphene/polyimide composite material

A polyimide and composite material technology, which is applied in the field of graphene/polyimide composite material preparation, can solve the problem that the comprehensive performance of graphene and polyimide composite materials cannot be effectively improved, and the comprehensive performance of composite materials cannot be achieved. Ideal value, poor adhesion between graphene and polyimide matrix, etc., to achieve the effects of easy industrialization, improved stress transfer effect, and easy preparation method

Inactive Publication Date: 2014-02-19
TIANJIN POLYTECHNIC UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the reported comprehensive properties of composite materials after adding graphene have not reached the ideal value, and the mechanical and heat resistance properties cannot be taken into account at the same time.
The reasons are: (1) self-agglomeration of graphe

Method used

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  • Preparation method for graphene/polyimide composite material
  • Preparation method for graphene/polyimide composite material
  • Preparation method for graphene/polyimide composite material

Examples

Experimental program
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preparation example Construction

[0029] (1) Preparation of graphite oxide

[0030] Using natural flake graphite as raw material, graphite oxide was prepared by improved Hummer method. The improved Hummer method for preparing graphite oxide is prior art;

[0031] (2) Preparation of Si-modified graphene

[0032] Ultrasonic the graphite oxide powder prepared in step (1) in an aprotic organic solvent for 0.5 to 2 hours to obtain a 0.5 to 5 mg / mL graphene oxide dispersion; React at 180°C for 1-24 hours; after washing and drying, Si-modified graphene black powder can be obtained; Si-modified graphene obtained through elemental analysis and X-ray photoelectron spectroscopy analysis, wherein the mass content of Si is 2-13 %.

[0033] (3) Preparation of Si-modified graphene / polyimide precursor

[0034] Mixing Si-modified graphene, dianhydride and diamine in the aprotic polar solvent, under the protection of nitrogen, at -10-30°C, in-situ polymerization reaction for 1-36 hours to obtain Si-modified graphene / Polyami...

Embodiment 1

[0047] Step (1) preparation of graphene oxide:

[0048] Using 325 mesh natural flake graphite as raw material, graphite oxide powder was prepared by improved Hummer method.

[0049] Step (2) Preparation of Si-modified graphene:

[0050] Weigh a certain amount of graphite oxide powder prepared in step (1), ultrasonically treat it for 1 hour, and disperse it in N-methylpyrrolidone solvent; add modifier 3-aminopropyltrimethoxysilane in proportion, and the reaction temperature is 50°C, the reaction time is 20 hours, wherein the mass ratio of graphene oxide and siloxane modifier 3‐aminopropyltriethoxysilane is 1:3; after the reaction, the reaction product is washed repeatedly with anhydrous methanol , the black target product was obtained after filtration, and dried in a vacuum oven at 80°C for 24 hours to obtain Si-modified graphene. The thickness of the obtained Si-modified graphene is 0.9 nm, and the particle size is 5-20 μm, detected by the atomic force microscope.

[0051] ...

Embodiment 2

[0057] The difference between this embodiment and Example 1 is that the mass ratio of graphene oxide and siloxane modifier 3-aminopropyltriethoxysilane in step (2) is 1:5, and the others are the same as in Example 1 .

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Abstract

The invention discloses a preparation method of a graphene/polyimide composite material. The preparation method adopts composite materials in percentage by weight and the processes, wherein the composite material comprises the following components in in percentage by weight: 80 to 99.99 percent of polyimide and 20 to 0.01 percent of Si-modified graphene; the preparation method particularly comprises the following steps: (1), preparing graphite oxide; (2), preparing Si-modified graphene: performing ultrasonographic treatment on the obtained graphite oxide powder in an aprotic organic solvent for 0.5 to 2 hours to obtain dispersion liquid with the concentration of 0.5 to 5mg/mL, adding an siloxane modification reagent into the dispersion liquid for reaction for 1 to 24 hours at a temperature of 30 to 180 DEG C, and performing washing and drying to obtain the powder of Si-modified graphene , wherein the mass content of Si is 2 to 13 percent;(3), preparing a precursor of Si-modified graphene/polyimide; (4), preparing the Si-modified graphene/polyimide composite material.

Description

technical field [0001] The invention relates to polyimide composite material technology, in particular to a preparation method of graphene / polyimide composite material. The main feature of the preparation method is the use of Si-modified graphene. Background technique [0002] Polyimide is widely used in cutting-edge technical fields such as aerospace, microelectronics, and communications due to its excellent heat resistance, dielectric properties, and mechanical properties. However, with the continuous development of modern industry, the requirements for various properties of materials are getting higher and higher, not only higher temperature resistance is required, but also high strength and high modulus are required. Traditional polyimide materials can no longer meet the requirements. It is necessary to modify polyimide to obtain polyimide composite materials with higher temperature resistance, high strength and high modulus. Graphene is composed of carbon atoms with ...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08G73/10C08K9/06C08K9/00C08K3/04
CPCC08K9/06C08G73/1007C08J5/18C08J2379/08C08K3/04C08K9/00C08L2203/16C08L79/08
Inventor 石海峰曹利孙青青张兴祥
Owner TIANJIN POLYTECHNIC UNIV
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