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Preparation method of nitrogen doped super-large cavity carbon nanotube composite material

A carbon nanotube and composite material technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of uneven thickness of two-dimensional carbon nanosheet materials, low ion and electron transfer rate, and difficult to control the composition and structure. , to achieve the effects of good reactivity and catalytic activity, simple process, and enhanced electrical conductivity

Inactive Publication Date: 2017-12-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The conventional methods mentioned in current patents can only obtain micro-nanoparticles or two-dimensional carbon nanosheet materials derived from metal-organic framework compounds, but due to the limitation of structural characteristics, the specific surface area of ​​micro-nanoparticle materials is small (120-170m 2 g -1 ), the ion and electron transport rates are low; the thickness of the two-dimensional carbon nanosheet material is uneven (2-500nm), the composition and structure are difficult to control, and the too thick sheet has the disadvantages of less exposed catalytic active sites.

Method used

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  • Preparation method of nitrogen doped super-large cavity carbon nanotube composite material
  • Preparation method of nitrogen doped super-large cavity carbon nanotube composite material
  • Preparation method of nitrogen doped super-large cavity carbon nanotube composite material

Examples

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Effect test

Embodiment 1

[0039]Disperse 0.78g of halloysite nanotubes in 80mL cobalt nitrate ethanol solution (0.125M), first stir for 30 minutes and then sonicate for 30 minutes, then add 80mL dimethylimidazole methanol solution (0.5M), stir for 30 minutes and then static at room temperature After leaving for 24 hours, the reaction was completed, and the product was centrifuged and washed three times with ethanol, and dried at 60°C to obtain a ZIF-67-coated halloysite composite material. The composite material was heated to 800 °C in nitrogen flow, and the heating rate was controlled at 5 °C min -1 , and calcined for 2 hours to obtain a black solid powder. Finally, soak the material in hydrofluoric acid, filter and separate after reacting for 12 hours, wash with deionized water three times, and dry at 60°C to obtain ZIF-67 metal organic framework compound derived cobalt / nitrogen doped ultra-thin tube wall carbon nano tube (denoted as NCNT-1), its specific surface area is as high as 541m 2 g -1 , t...

Embodiment 2

[0041] Disperse 0.78g of halloysite nanotubes in 80mL of zinc nitrate (0.125M) ethanol solution, first stir for 30 minutes and then sonicate for 30 minutes, then add 80mL of dimethylimidazole methanol solution (0.5M), stir for 30 minutes and then static at room temperature Set aside for 24 hours; after the reaction, the product was centrifuged and washed 3 times with ethanol, and dried at 60° C. to obtain ZIF-8 coated halloysite powder material. The powder material was heated to 800°C in a nitrogen stream, calcined for 2 hours, and the heating rate was controlled at 5°C min -1 , to obtain black solid powder. Finally, soak the powder in excess hydrofluoric acid, react for 12 hours, filter and separate, wash 3 times with deionized water, and dry at 60°C to obtain ZIF-8 metal-organic framework compound-derived nitrogen-doped ultra-thin tube-walled carbon nano Tube (marked as NCNT-2). Figure 4 Shown is the TEM photograph of NCNT-2. It can be seen from the figure that, compared...

Embodiment 3

[0043] Disperse 1.56g halloysite nanotubes in 80mL zinc nitrate (0.0625M) and cobalt nitrate (0.0625M) mixed ethanol solution, stir for 30 minutes, ultrasonic for 1 hour, then add 80mL dimethylimidazole methanol solution (0.5M), After stirring for 30 minutes, stand at room temperature for 24 hours; after the reaction, the product was centrifuged, washed with ethanol three times, and dried at 60°C to obtain a Zn / Co-ZIF-coated halloysite composite. The material was heated to 800°C in a nitrogen stream, calcined for 2 hours, and the heating rate was controlled at 5°C min -1 . Finally, soak the carbonized black solid powder in hydrofluoric acid, filter and separate after reacting for 12 hours, wash 3 times with deionized water, and dry at 60°C to obtain Zn / Co-ZIF metal organic framework compound derived cobalt / nitrogen doped Miscellaneous ultra-thin walled carbon nanotubes (referred to as NCNT-3). Figure 5 It is the TEM image of NCNT-3. It can be seen that the carbon nanotubes ...

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Abstract

The invention provides a preparation method of a nitrogen doped super-large cavity carbon nanotube composite material, belonging to the technical field of preparation of nano composite catalysis materials. Based on a metal organic framework compound, electrostatic adsorption, directional nucleation growth, limited carbonization and acid corrosion for removing a template are performed on the surface of a tubular inorganic template one-dimensional nanotube, so as to obtain a metal-modified nitrogen doped carbon nanotube composite material. The prepared composite material has a large cavity and a thin wall, and has the characteristics of rich electrochemical activity sites and efficient electronic transmission. The preparation method has the characteristics of being easy to operate, being low-cost, and being easy for industrial production, and has a bright application prospect in energy storage and environment-friendly catalysis.

Description

technical field [0001] The invention relates to a synthesis method for preparing a metal-modified nitrogen-doped ultra-thin tube wall and super-large lumen carbon nanotube composite material from a metal-organic framework compound, and belongs to the technical field of new materials. Background technique [0002] Among nanomaterials, carbon nanotubes are known as "super nanomaterials". As a typical one-dimensional (1D) nanostructure material, carbon nanotubes exhibit novel physical and chemical properties, especially high thermal stability and surface carrier mobility, making carbon nanotubes widely used in new energy, sensors, and supercapacitors. and other fields have been widely used. The huge research and application value of carbon nanotubes has also aroused the upsurge of researchers in doping and compounding carbon nanotubes. At present, carbon nanotubes are doped with various heteroatoms, such as boron, nitrogen, phosphorus, sulfur and other heteroatoms. Due to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J21/18B01J35/10B82Y30/00
CPCB82Y30/00B01J21/185B01J27/24B01J35/617B01J35/615
Inventor 王旭珍李芮董琰峰赵宗彬邱介山
Owner DALIAN UNIV OF TECH
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