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Method for in-situ preparation of iron carbide filled doped carbon nanotube

A technology for in-situ preparation of carbon nanotubes, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the cumbersome preparation process, low precursor utilization rate, low iron utilization rate, etc. problem, to achieve the effect of high utilization rate, low precursor cost, and low equipment requirements

Inactive Publication Date: 2016-01-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This invention needs to place the iron salt and the carbon source respectively at the inlet end of the reactor. The catalyst and the carbon source need to be gasified first, and then brought into the high-temperature zone of the reactor by the carrier gas for chemical vapor deposition reaction, and the reactants are dispersed throughout the reactor. The reaction zone, so the preparation process is cumbersome and the equipment is complicated. At the same time, a large amount of iron salts are not gasified but iron oxides are formed during the iron salt gasification process, and the utilization rate of iron is not high.
[0004] In summary, the existing methods for preparing iron-filled doped carbon nanotubes have the disadvantages of low iron filling rate in the prepared iron-filled carbon nanotubes, complex preparation methods, harsh preparation conditions, and low precursor utilization.

Method used

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  • Method for in-situ preparation of iron carbide filled doped carbon nanotube
  • Method for in-situ preparation of iron carbide filled doped carbon nanotube
  • Method for in-situ preparation of iron carbide filled doped carbon nanotube

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Effect test

Embodiment 1

[0036] Preparation of iron carbide filled nitrogen-doped carbon nanotubes:

[0037] Dissolve and disperse 1.5g of ferric chloride hexahydrate and 1.5g of melamine in 100mL of ethanol solution. After ultrasonication for half an hour, put them in an oven at 110°C for 12h. Grind the dried mixed powder evenly, put it into a porcelain boat, and put it in the high temperature zone of the tube furnace. Introduce Ar into the tube furnace at a rate of 160 mL / min, raise the temperature to 800 °C at a rate of 10 °C / min, keep it for 2 h, and naturally cool to room temperature to obtain a black powder. The black powder was pickled in 200mL, 2mol / L hydrochloric acid solution for 6h, filtered and dried to obtain nitrogen-doped carbon nanotubes filled with iron carbide. The weight of the sample was 0.4g, and the filling amount of iron was about 27%.

[0038]The SEM image of the obtained iron carbide filled nitrogen-doped carbon nanotube sample is shown in figure 1 shown, from figure 1 It c...

Embodiment 2

[0042] Preparation of iron carbide-filled nitrogen-boron co-doped carbon nanotubes:

[0043] Dissolve 1.5g of ferric chloride hexahydrate, 1.5g of melamine, and 0.2g of boric acid in 100ml of ethanol solution, ultrasonicate for half an hour, and dry in an oven at 110°C for 12h. Grind the dried mixed powder evenly, put it into a porcelain boat, and put it in the high temperature zone of the tube furnace. Introduce Ar into the tube furnace at a rate of 160 mL / min, raise the temperature to 800 °C at a rate of 10 °C / min, keep it for 2 h, and naturally cool to room temperature to obtain a black powder. The black powder was pickled in 200mL, 2mol / L hydrochloric acid solution for 6 hours, filtered and dried to obtain iron carbide-filled nitrogen-boron-doped carbon nanotubes. The weight of the sample was 0.4g, and the iron filling amount was about 20%.

[0044] The SEM image of the obtained iron carbide filled nitrogen-boron co-doped carbon nanotube sample is as follows Figure 6 As...

Embodiment 3

[0046] Preparation of iron carbide filled nitrogen and phosphorus co-doped carbon nanotubes:

[0047] Dissolve and disperse 0.5g of ferric chloride hexahydrate, 1.5g of melamine, and 0.2mL of phosphoric acid in 100ml of ethanol solution. After ultrasonication for half an hour, dry in an oven at 110°C for 12h. Grind the dried mixed powder evenly, put it into a porcelain boat, and put it in the high temperature zone of the tube furnace. Introduce Ar into the tube furnace at a rate of 160 mL / min, raise the temperature to 900 °C at a rate of 10 °C / min, keep it for 2 h, and naturally cool to room temperature to obtain a black powder. The black powder was pickled in 200mL, 2mol / L hydrochloric acid solution for 6h, filtered and dried to obtain iron carbide-filled nitrogen-phosphorus-doped carbon nanotubes. The weight of the sample was 0.4g, and the iron filling amount was about 20%.

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Abstract

The invention discloses a method for in-situ preparation of an iron carbide filled doped carbon nanotub. The method includes: mixing an iron salt, a cyanamide nitrogenous organic compound precursor and a doping precursor evenly, then conducting high temperature pyrolysis in a tube furnace, and carrying out pickling to remove impurities, thus obtaining the iron carbide filled doped carbon nanotub. Compared with the traditional method, the method provided by the invention uses cheap precursor, reaches high utilization ratio, lower equipment requirement, improves the safety of the preparation process, and can be used for large-scale preparation, The prepared iron carbide filled doped carbon nanotub has uniform size, iron carbide is filled evenly, the filling content is high, and the product yield is high.

Description

technical field [0001] The invention relates to a method for filling doped carbon nanotubes with iron carbide, in particular to a method for preparing iron carbide filled and doped carbon nanotubes in situ. Background technique [0002] As a new type of carbon nanomaterial, carbon nanotubes have attracted worldwide attention due to their unique mechanical, electronic and chemical properties. a wide range of applications. The modification of carbon nanotubes can obviously change their properties, and has gradually become one of the hotspots in the field of carbon materials research in recent years. The modification of carbon nanotubes can be divided into the following categories: external modification of carbon nanotubes, doping of carbon nanotubes and filling of internal cavities of carbon nanotubes. The external modification of carbon nanotubes is mainly to insert other organic or oxygen-containing functional groups on the outer surface of carbon nanotubes, which is gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/30B82Y30/00
Inventor 王红娟钟国玉彭峰余皓
Owner SOUTH CHINA UNIV OF TECH
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