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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has disadvantages such as low yield, high cost, high impurity content and low specific surface area, and is not suitable for large-scale industrial production.

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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Experimental program
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Effect test

Embodiment 1

[0024] Weigh 3g melamine, 1.1gFeCl 3 ·6H 2 O and 3gZnCl 2 , 500rpm mechanical stirring for 3h; the mixture was transferred to a ceramic crucible, placed in a tube furnace, under N 2 Under protection, pre-carbonize at 500°C for 1 hour, then carbonize at 900°C for 2 hours; soak the obtained carbon material in 3M HCl solution for 6 hours, filter, and dry at 120°C to obtain Fe 3 C nanowires filled N-doped carbon nanotube composites.

[0025] The XRD diffraction pattern of the material ( figure 1 ) indicates that the composite material consists of carbon and Fe 3 C composition, according to the thermogravimetric curve ( figure 2 ) to get the composite material Fe 3 C content is 13.2wt%; SEM ( image 3 ) and TEM images ( Figure 4 ) show that Fe 3 C nanowires filled in carbon nanotube composites. by N 2 Adsorption-desorption equilibrium curve ( Figure 6 ), the calculated specific surface area of ​​the composite material is 1026.26m 2 g -1 .

Embodiment 2

[0027] Weigh 3g melamine, 1.6gFeCl 3 ·6H 2 O and 3gZnCl 2 , 500rpm mechanical stirring for 2h; the mixture was transferred to a ceramic crucible, placed in a tube furnace, under N 2 Under protection, pre-carbonize at 400°C for 3h, and then carbonize 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 filled N-doped carbon nanotube composites.

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

Embodiment 3

[0030] Weigh 3g melamine, 3.24gFeCl 3 ·6H 2 O and 3gZnCl 2 , 500rpm mechanical stirring for 1h; the mixture was transferred to a ceramic crucible, placed in a tube furnace, under N 2 Under protection, pre-carbonize at 500°C for 2 hours, and then heat up to 700°C for carbonization for 3 hours; soak the obtained carbon material in 1M HCl solution for 10 hours, filter, and dry at 100°C to obtain Fe 3 C nanowires filled N-doped carbon nanotube composites.

[0031] According to TGA and N 2 Adsorption-desorption curve, the calculated composite material Fe 3 The C content is 16.5wt%, and 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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