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Graphene oxide fiber, preparation method, and preparation method of graphene oxide fiber composite material

A graphene fiber, graphene fiber technology, applied in the field of graphene, can solve the problems of limited application, large diameter of graphene fiber, etc., and achieve the effect of improving tensile strength and good hydrophilicity

Active Publication Date: 2013-11-20
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The diameter of the graphene fiber obtained by the above method is relatively large, about 33 μm in diameter, and only a single fiber can be obtained at a time, which limits its application in industry

Method used

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  • Graphene oxide fiber, preparation method, and preparation method of graphene oxide fiber composite material
  • Graphene oxide fiber, preparation method, and preparation method of graphene oxide fiber composite material

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preparation example Construction

[0024] The embodiment of the present invention discloses a preparation method of graphene oxide fiber, comprising:

[0025] The graphene oxide aqueous solution is freeze-solidified in liquid nitrogen, and then freeze-dried to obtain graphene oxide fibers; the graphene oxide is prepared according to a chemical oxidation method.

[0026] In the process of preparing the graphene oxide fiber skeleton, the present invention first freezes and solidifies the graphene oxide aqueous solution in liquid nitrogen. Graphene oxide is the product of flake graphite after chemical oxidation and exfoliation. There are three methods for preparing graphene oxide: Brodie method, Staudenmaier method and Hummers method. Since the graphene oxide prepared by the Hummers method has a higher degree of oxidation and contains more oxygen-containing functional groups, the graphene oxide aqueous solution of the present invention is preferably prepared according to the Hummers method, which is a method well...

Embodiment 1

[0039] (1) Add 1g of natural graphite and 1.2g of potassium nitrate to 46ml of concentrated sulfuric acid with a concentration of 98wt%, stir for 10 minutes, then add 6g of potassium permanganate, raise the temperature to 40°C, heat and stir for 6h, then add 80ml of deionized water, and raise the temperature to 80°C, heat and stir for 0.5h, then add 200ml of deionized water and 6ml of hydrogen peroxide, the reactant turns golden yellow, and the reaction stops. Finally, under the condition of high-speed centrifugation, it was repeatedly washed with deionized water until the pH of the supernatant was neutral, and the graphene oxide concentrate was obtained.

[0040] (2) Prepare the graphene oxide concentrate in step (1) into an aqueous solution with a concentration of 2 mg / ml, and then take 60 ml of it and pour it into a mold with a length of 20 cm, a width of 10 cm, and a thickness of 3 mm.

[0041] (3) Rapidly immerse the mold in liquid nitrogen to rapidly freeze and solidify ...

Embodiment 2

[0046] (1) A 1.25 mg / ml graphene oxide aqueous solution was prepared by the Hummers method.

[0047] (2) Pour 60ml of the graphene oxide aqueous solution obtained in step (1) into a mold with a length of 20cm, a width of 10cm, and a thickness of 3mm.

[0048] (3) Rapidly immerse the mold in liquid nitrogen to rapidly freeze and solidify the graphene oxide solution in the mold.

[0049] (4) Freeze-dry the graphene oxide aqueous solution solidified in step (3) with a freeze dryer to obtain 75 mg of a complete three-dimensional network graphene oxide fiber skeleton.

[0050] (5) Perform thermal reduction treatment at 50°C for 0.5-5 hours on the skeleton obtained in step (4) to obtain a graphene three-dimensional network skeleton.

[0051] (6) Mix JL-236 high-strength epoxy resin and JH-239 epoxy curing agent evenly in a mass ratio of 10:3, and then mix it with the graphene three-dimensional network skeleton obtained in step (5) in a mass ratio of 500 : 1 curing compound. Curin...

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Abstract

The invention provides a graphene oxide fiber, a preparation method of the graphene oxide fiber, and a preparation method of a graphene oxide fiber skeleton based composite material. The preparation method of the graphene oxide fiber comprises the following steps: carrying out quenching setting of an aqueous graphene oxide solution in liquid nitrogen, extruding the graphene oxide between nanometer ice crystals to form a fiber skeleton having a tridimensional network structure, and lyophilizing for sublimating the ice crystals between the graphene oxide in order to realize the in-situ preservation of the fiber skeleton having a tridimensional network structure. The fiber diameter of the prepared graphene oxide fiber skeleton is 100-500nm, and the tensile strength of the graphene oxide fiber compounded with an epoxy resin is 85% higher than that of the graphene oxide fiber, and is 38% higher than that of carbon fiber non-crimp fabric reinforced epoxy resin having a same matrix and a same mass fraction.

Description

technical field [0001] The invention relates to the technical field of graphene, in particular to a graphene oxide fiber, a preparation method thereof and a preparation method of a composite material thereof. Background technique [0002] Graphene is a two-dimensional crystal composed of a single layer of carbon atoms. It has excellent properties such as ultra-high specific surface area, excellent electrical and thermal conductivity, and ultra-high mechanical strength, so it has good application prospects in many fields, such as : Field-effect transistors, high-frequency devices, super microprocessors and single-molecule detectors, controllable gas-permeable membranes, anisotropic ion conductors, supercapacitors and other fields. However, a major obstacle to the application of graphene is the assembly of graphene macrostructures. At present, there are many successful cases in graphene film and block assembly, but in terms of fiber, there are only two methods: spinning and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K7/06C08K3/04C08K9/00C08L63/00C08J5/06
Inventor 周旭峰刘兆平张良忠
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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