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Preparation method of graphene/carbon nanotube composite material

A technology of carbon nanotubes and composite materials, applied in the directions of carbon nanotubes, multi-walled carbon nanotubes, graphene, etc., can solve the problems of high experimental cost, harsh experimental conditions, complex preparation process, etc. The effect of controllable parameters and simple process

Active Publication Date: 2018-02-16
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the above-mentioned preparation method has the disadvantages of harsh experimental conditions, complicated preparation process and high experimental cost.

Method used

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  • Preparation method of graphene/carbon nanotube composite material
  • Preparation method of graphene/carbon nanotube composite material
  • Preparation method of graphene/carbon nanotube composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 3g of graphite powder and 2g of sodium nitrate into the beaker, slowly add 70mL of concentrated sulfuric acid along the beaker and keep stirring; under the condition of ice bath, add 30g of potassium permanganate solid powder into the beaker in five times and keep stirring 1h. Stirring was continued for 2 h in a water bath at 35 °C to obtain a mixed solution. Slowly add 140mL deionized water into the solution and keep stirring for 15min, then the temperature of the system rises to about 95°C, and continue stirring for 3h; dropwise add 30% H 2 o 2 until the solution turned bright yellow. The reaction solution was filtered while hot, and washed with dilute hydrochloric acid to remove excess metal ions. Graphene oxide was prepared by centrifuging and washing to pH 7, freeze-drying for 48 hours, vacuum degree 8-pa, temperature: -10°C, and its crystal plane structure was confirmed by X-ray diffractometer, refer to the attached figure 1 . The XRD results show that th...

Embodiment 2

[0037] The preparation method of the graphene / carbon nanotube composite material, the operation steps are as follows: (1) graphene oxide is prepared by oxidation reaction of natural graphite powder; Hydrothermal reaction to prepare graphene / carbon nanotube composites.

[0038] Step (1) The operating steps are the same as in Example 1.

[0039] Step (2) The operation steps are as follows: Add graphene oxide and deionized water into a beaker for ultrasonic dispersion for 1 h, then add Ni(NO3)2·6H2O and hexamethylenetetramine (HMTA) and stir well; the solution is transferred to React at a constant temperature in a 100mL reactor; after the reaction, add excess hydrochloric acid with a concentration of 1mol / L to dissolve nickel hydroxide, take a black solid after suction filtration, wash and dry in vacuum to obtain a graphene / carbon nanotube composite material.

[0040] The freeze-drying time is 30-50 hours, the temperature is -18°C, and the vacuum degree is 9 Pa.

[0041] In the s...

Embodiment 3

[0048] The preparation method of graphene / carbon nanotube composite material is characterized in that operation steps are as follows: (1) natural graphite powder prepares graphene oxide through oxidation reaction; (2) graphene oxide and nickel nitrate hexahydrate, hexamethylenetetrafluoroethylene Amines undergo ultrasonic hydrothermal reaction to prepare graphene / carbon nanotube composites.

[0049] Step (1) The operating steps are the same as in Example 1. The different process parameters are: the freeze-drying time is 50 hours, the temperature is -40° C., and the vacuum degree is 10 Pa.

[0050] The operation steps of the step (2) are as follows: take graphene oxide and deionized water and add them to a beaker for ultrasonic dispersion for 1.5h, then add Ni(NO3)2·6H2O and hexamethylenetetramine (HMTA) and stir well; The solution was transferred to a 100mL reactor for constant temperature reaction; after the reaction was completed, an excess concentration of 1mol / L hydrochlo...

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Abstract

The invention discloses a method for preparing a graphene / carbon nanotube composite material. Graphene oxide can be obtained from graphite powder as a raw material by a modified Hummers method; the graphene oxide and deionized water are added into a beaker for ultrasonic dispersion, then nickel nitrate hexahydrate and hexamethylenetetramine are added and evenly fully mixed; the solution is transferred into a reaction kettle for a period of time of reaction at constant temperature, after the reaction is finished, enough hydrochloric acid with the concentration of 1mol / L is added for dissolution of nickel hydroxide, and after filteration by suction, a black solid is taken, and dried in vacuum to obtain the graphene / carbon nanotube composite material. Lens results show that the carbon nano tube size distribution is in 15-40nm, the carbon nano tube lengthis micron-scale, and the carbon nano tubes are dispersed in the system so as to realize the graphene and carbon nano tube homogeneous compounding.

Description

technical field [0001] The invention relates to a composite material, in particular to a preparation method of a graphene / carbon nanotube composite material. It belongs to the technical field of functional materials. Background technique [0002] As a typical one-dimensional quantum carbon material, carbon nanotubes have a special structure. It is mainly a hollow coaxial tube composed of carbon atoms arranged in a hexagonal shape. Because of the unevenness of the local area of ​​carbon nanotubes, its structure is not completely straight. And showing a certain curvature. The pipe diameter distribution is generally maintained at a dozen to tens of nanometers, and the length distribution is at the micron level. Graphene is a single-layer two-dimensional crystal, in which carbon atoms are also arranged in sp2 mixed orbitals, so carbon nanotubes can be regarded as graphene coils. Both have high electrical conductivity, large specific surface area, and good mechanical propertie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184C01B32/166B82Y40/00B82Y30/00
CPCB82Y30/00C01B2202/06C01B2202/22C01B2202/34C01B2202/36C01P2002/01C01P2002/72C01P2004/03C01P2004/04C01P2004/80
Inventor 邢宏龙王磊孙翔刘振峰
Owner ANHUI UNIV OF SCI & TECH
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