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Method for preparing graphene/carbon nanotube composites by solid-phase cracking technology

A technology of carbon nanotubes and composite materials, applied in the manufacture of hybrid capacitor electrodes, hybrid/electric double layer capacitors, etc., can solve the problems of high cost, poor quality, low efficiency, etc., and achieve energy saving, high safety, cracking The effect of low temperature

Active Publication Date: 2017-10-17
SICHUAN HUANTAN TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing graphene / carbon nanotube composite materials in one step by using solid phase cracking technology to solve the problems of high cost, low efficiency and poor quality in the existing graphene / carbon nanotube composite material preparation technology. question

Method used

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  • Method for preparing graphene/carbon nanotube composites by solid-phase cracking technology
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  • Method for preparing graphene/carbon nanotube composites by solid-phase cracking technology

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Using 30.0 grams of self-made nickel phthalocyanine (the amount of nickel chloride precursor is 0.5 grams) as the starting material, in a quartz tube furnace, under the protection of high-purity argon, the argon flow rate is controlled at 50cm 3 min -1 , cracked under the following heating scheme to obtain about 23 grams of the final graphene / carbon nanotube composite material. That is, the temperature is raised to 300 degrees at a slow heating rate of 5 degrees per minute, and 300 degrees is stable for 1 hour; the temperature is raised to 350 degrees at 5 degrees per minute, and 350 degrees is stable for 1 hour; hour; the temperature is raised to 500 degrees at 3 degrees per minute, and 500 degrees is stable for 4 hours; the temperature is raised to 800 degrees at 2 degrees per minute, and 800 degrees is stable for 8 hours, and finally it is naturally lowered to room temperature. Its XRD pattern is as figure 1 shown.

Embodiment 2

[0035] Using 30.0 grams of self-made nickel phthalocyanine (1.65 grams of nickel chloride precursor) as the starting material, in a quartz tube furnace, under the protection of high-purity argon, the argon flow rate is controlled at 50cm 3 min -1 , cracked under the following heating scheme to obtain about 22 grams of the final graphene / carbon nanotube composite material. That is, the temperature is raised to 300 degrees at a slow heating rate of 5 degrees per minute, and 300 degrees is stable for 1 hour; the temperature is raised to 350 degrees at 5 degrees per minute, and 350 degrees is stable for 1 hour; hour; the temperature is raised to 500 degrees at 3 degrees per minute, and 500 degrees is stable for 4 hours; the temperature is raised to 800 degrees at 2 degrees per minute, and 800 degrees is stable for 8 hours, and finally it is naturally lowered to room temperature. Its Raman spectrum is as follows figure 2 shown.

Embodiment 3

[0037] Using 30.0 grams of self-made nickel phthalocyanine (1.0 grams of nickel chloride precursor) as the starting material, in a quartz tube furnace, under the protection of high-purity argon, the argon flow rate is controlled at 50cm 3 min -1 , and obtain about 20 grams of final graphene / carbon nanotube composite material by pyrolysis under the following heating scheme. That is, the temperature is raised to 300 degrees at a slow heating rate of 5 degrees per minute, and 300 degrees is stable for 1 hour; the temperature is raised to 350 degrees at 5 degrees per minute, and 350 degrees is stable for 1 hour; hour; the temperature is raised to 500 degrees at 3 degrees per minute, and 500 degrees is stable for 4 hours; the temperature is raised to 800 degrees at 2 degrees per minute, and 800 degrees is stable for 8 hours, and finally it is naturally lowered to room temperature. Its SEM and TEM images are as follows image 3 , as shown in 4.

[0038] The sample of Example 3 wa...

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Abstract

The invention discloses a method for preparing a graphene / carbon nanotube composite material by solid-phase cracking technology. The heating method is to raise the temperature to the pyrolysis autocatalysis temperature, and obtain the final graphene / carbon nanotube composite material by one-step pyrolysis. Using nickel phthalocyanine compound and its derivatives as the only starting material, one-step solid-phase cracking to obtain azagraphene / carbon nanotube composite materials; the cracking temperature is low, saving energy consumption; using inert gas protection, it can be used in a non-hydrogen atmosphere environment The final material is obtained by medium pyrolysis, which has high safety; the nitrogen atoms of the molecular skeleton of the raw material compound remain in the final graphene / carbon nanotube composite skeleton after high temperature pyrolysis, becoming a better conductive material.

Description

technical field [0001] The invention belongs to the field of high-tech material preparation, and in particular relates to a method for preparing graphene / carbon nanotube composite materials in one step by using solid-phase cracking technology. Background technique [0002] Carbon nanotubes (CNTs) and graphene (Graphene) were discovered in 1991 and 2004, respectively, and have been attracting attention since the day they were discovered. Carbon nanotube is a one-dimensional quantum material with a special structure. Its radial dimension can reach nanometer level, and its axial dimension is micron level. Both ends of the tube are generally sealed, so it has great strength and huge The aspect ratio is expected to make it into carbon fiber with excellent toughness. Graphene is a carbon atom with sp 2 The hexagonal honeycomb lattice composed of hybrid orbitals is a planar film, a two-dimensional carbon material with a thickness of only one carbon atom. Zero-dimensional fullere...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G11/32H01G11/36H01G11/44H01G11/86
CPCY02E60/13
Inventor 薛卫东赵睿
Owner SICHUAN HUANTAN TECH
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