Preparation method of Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area

A technology of nitrogen-doped carbon and composite materials, applied in the direction of nanotechnology, etc., can solve the problems of being unsuitable for large-scale industrial production, high impurity content, and low specific surface area, and achieve low cost, high specific surface area, and low raw material cost Effect

Inactive Publication Date: 2016-05-04
ZHONGBEI UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, this method also has disadvantages such as low yield, high cost, high impurity cont

Method used

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  • Preparation method of Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area
  • Preparation method of Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area
  • Preparation method of Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area

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Example Embodiment

[0023] Example 1:

[0024] Weigh 3g melamine, 1.1g FeCl 3 ·6H 2 O and 3gZnCl 2 , 500rpm mechanical stirring for 3h; transfer the mixture to a ceramic crucible, place it in a tube furnace, 2 Under protection, pre-carbonized at 500℃ for 1h, then heated at 900℃ to carbonize for 2h; soak the obtained carbon material in 3M HCl solution for 6h, filter, and dry at 120℃ to obtain Fe 3 C nanowires are filled with N-doped carbon nanotube composite materials.

[0025] XRD diffraction pattern of the material ( figure 1 ) Shows that the composite material is composed of carbon and Fe 3 C composition, according to the thermogravimetric curve ( figure 2 ) The composite material Fe 3 C content is 13.2wt%; scanning electron microscope ( image 3 ) And TEM image ( Figure 4 ) Shows that Fe is obtained 3 C nanowires are filled with carbon nanotube composite materials. Pass N 2 Adsorption-desorption equilibrium curve ( Image 6 ), the specific surface area of ​​the composite material is calculated t...

Example Embodiment

[0026] Example 2

[0027] Weigh 3g melamine, 1.6g FeCl 3 ·6H 2 O and 3gZnCl 2 , 500rpm mechanical stirring for 2h; transfer the mixture to a ceramic crucible, place it in a tube furnace, 2 Under protection, pre-carbonized at 400°C for 3h, then heated at 800°C for 2h; soak the obtained carbon material in 2M HCl solution for 5h, filter, and dry at 100°C to obtain Fe 3 C nanowires are filled with N-doped carbon nanotube composite materials.

[0028] According to thermogravimetry and N 2 Adsorption-desorption curve, calculated composite material Fe 3 C content is 14.8wt%, specific surface area is 639.42m 2 g -1 .

Example Embodiment

[0029] Example 3

[0030] Weigh 3g melamine, 3.24g FeCl 3 ·6H 2 O and 3gZnCl 2 , 500rpm mechanical stirring for 1h; transfer the mixture to a ceramic crucible, place it in a tube furnace, 2 Under protection, pre-carbonized at 500°C for 2h, then heated to 700°C for 3h; soak the obtained carbon material in 1M HCl solution for 10h, filter, and dry at 100°C to obtain Fe 3 C nanowires are filled with N-doped carbon nanotube composite materials.

[0031] According to thermogravimetry and N 2 Adsorption-desorption curve, calculated composite material Fe 3 The C content is 16.5wt%, the specific surface area is 411.89m 2 g -1 .

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Abstract

The present invention discloses a preparation method of a Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area, and belongs to the field of new energy materials. The method uses melamine as carbon and nitrogen sources, ferric chloride as a catalyst and a source of iron, and zinc chloride as an activator. The melamine, ferric chloride and zinc chloride are mechanically mixed, and subjected to high temperature carbonization decomposition; iron and zinc compounds on the carbon nanotube surface are removed with dilute hydrochloric acid, so as to obtain the Fe3C nanowire filled and nitrogen doped carbon nanotube composite. The present invention uses inexpensive starting materials and a one-step method for preparation of the Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area, and the specific surface area reaches 1500.21 m<2>/g; and the invention is simple in process and applicable to industrial application.

Description

technical field [0001] The invention relates to a nitrogen-doped carbon nanotube / Fe 3 The invention discloses a preparation method of a C composite material, which belongs to the field of new energy materials. Background technique [0002] Fe 3 C materials are widely used in the fields of catalysis, electrochemistry, gas separation and storage due to their advantages of low price, low toxicity, high hardness, magnetism, good thermal stability and oxidation resistance, and have very high application value. Currently, Fe 3 Research on C-based composites mainly focuses on carbon (graphite)-wrapped nano-Fe 3 The research on C composite materials has excellent magnetic properties and electrochemical properties, and has great application prospects in the fields of sensors, catalysts, and new energy materials. [0003] Carbon nanotube is a one-dimensional carbon nanomaterial with a hollow structure. Its unique hollow tubular structure has a confinement effect in the one-dimensi...

Claims

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Application Information

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IPC IPC(8): C01B31/30C01B31/02B82Y40/00
CPCC01P2002/72C01P2002/85C01P2002/88C01P2004/03C01P2004/04C01P2006/12C01P2006/17
Inventor 王延忠董英鸽张国祥刘炜常青薛超瑞胡胜亮
Owner ZHONGBEI UNIV
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