Preparation method of iron filled carbon nano tube and reaction device

A carbon nanotube and reactor technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of low metal filling rate and complex preparation method, and achieve high filling amount, simple process and simplified process. Effect

Inactive Publication Date: 2013-09-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The object of the present invention is to propose a method for preparing iron-filled carbon nanotubes to achieve The advantages of high iron filling rate and simple preparation method

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  • Preparation method of iron filled carbon nano tube and reaction device
  • Preparation method of iron filled carbon nano tube and reaction device
  • Preparation method of iron filled carbon nano tube and reaction device

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[0036] The invention discloses a method for preparing iron-filled carbon nanotubes and a reaction device. The method for preparing iron-filled carbon nanotubes uses an inorganic covalent compound of iron, anhydrous ferric chloride, as a catalyst precursor, and selects different carbon sources. , Nitrogen-doped iron-filled carbon nanotubes and nitrogen-doped iron-filled carbon nanotubes were prepared by planktonic catalytic chemical vapor deposition. The elemental iron formed after the reduction of the catalyst precursor anhydrous ferric chloride used in the present invention can be filled into carbon nanotubes in large quantities while catalyzing the growth of carbon nanotubes, which breaks through the reaction when ferrocene is used as a catalyst precursor. The maximum iron-to-carbon atomic ratio is only limited to 1:10, and the filling degree of iron in carbon nanotubes can be improved by increasing the amount of anhydrous ferric chloride.

[0037] Specifically, when the car...

Embodiment 1

[0058] image 3A schematic structural view of a reaction device for realizing the preparation method of iron-filled carbon nanotubes in Example 1; Figure 4 The transmission electron micrograph of the nitrogen-doped iron-filled carbon nanotubes prepared in Example 1; Figure 8 It is the thermogravimetric curve of embodiment 1, 2 and 3 gained products.

[0059] This embodiment discloses a method for preparing nitrogen-doped iron-filled carbon nanotubes, using image 3 The shown iron-filled carbon nanotube reaction device includes: a tubular resistance furnace 3 with a temperature control device, two porcelain boats 2 for holding solid reactants, and gas inlets 7 and 2 respectively at both ends. The quartz tube reactor 5 of the gas outlet 4, the porcelain boat 2 for holding the solid reactant is placed in the quartz tube reactor 5 near the gas inlet 7, specifically the porcelain boat 2 for holding the solid reactant is placed At 1 / 3 of the total length of the quartz tube reac...

Embodiment 2

[0065] Figure 5 A transmission electron micrograph of the nitrogen-doped iron-filled carbon nanotubes prepared in Example 2;

[0066] This embodiment discloses a method for preparing nitrogen-doped iron-filled carbon nanotubes. Using the same reaction device as in Example 1, the preparation method for nitrogen-doped iron-filled carbon nanotubes includes the following steps:

[0067] Weigh melamine and anhydrous ferric chloride according to a mass ratio of 1:1, place them in two porcelain boats 2, and spread them evenly. Put the two porcelain boats 2 side by side into the quartz tube reactor 5 , and then place the quartz tube reactor 5 in the tubular resistance furnace 3 . Inert protective gas Ar was introduced into the well-sealed quartz tube reactor 5, and at the same time, the temperature of the tubular resistance furnace 3 was programmed to 700 °C, the Ar gas flow rate was adjusted to 200 mL / min, and the quartz tube was pushed to make the ceramic boat enter the tubular re...

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Abstract

The invention provides a preparation method of an iron filled carbon nano tube and a reaction device. The preparation method of the iron filled carbon nano tube comprises the following steps of: preparing the iron filled carbon nano tube by adopting an inorganic covalent compound of iron namely ferric chloride anhydrous as a catalyst precursor and selecting different carbon sources through floating catalysis chemical vapor deposition method, wherein the iron filled carbon nano tube comprises a non-nitrogen-doped iron filled carbon nano tube or a nitrogen-doped iron filled carbon nano tube. The preparation method of the iron filled carbon nano tube disclosed by the invention is simple and scientific in steps and can prepare a high-iron filled carbon nano tube. The invention further discloses a reaction device of the preparation method of the iron filled carbon nano tube. According to the preparation method of the iron filled carbon nano tube and the reaction device, a plurality of disadvantages in the prior art can be overcome; and the advantages that the preparation method is simple and the obtained iron filled carbon nano tube has high iron filling rate are realized.

Description

[0001] technical field [0002] The invention relates to inorganic non-metallic material technology, in particular to a preparation method and reaction device for iron-filled carbon nanotubes. Background technique [0003] Since the discovery of carbon nanotubes (CNTs) in 1991 [Iijima S, et al. Nature, 1991, 354(6348): 56], due to its unique structure and excellent electrical and mechanical properties, researchers have attracted extensive attention. focus on. In recent years, the modification of carbon nanotubes has gradually become a research hotspot. The modification of carbon nanotubes can be divided into two types: external modification of carbon nanotubes and filling of internal cavities of carbon nanotubes. The external modification of carbon nanotubes mainly includes functionalization, loading specific functional groups to improve the water solubility of carbon nanotubes, or doping them to change the crystal structure and electronic structure of carbon nanotubes. ,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C23C16/14B82Y30/00C01B32/162
Inventor 王旭珍范彦如刘洋邱介山
Owner DALIAN UNIV OF TECH
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