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Preparation method of three-dimensional network-shaped tungsten carbide-carbon nanotube composite material

A carbon nanotube and composite material technology is applied in the field of preparation of three-dimensional network tungsten carbide-carbon nanotube composite materials, which can solve the problems of easy agglomeration and low catalytic activity of methanol, so as to improve electrical conductivity, reduce reaction time, improve The effect of electrocatalytic effect

Active Publication Date: 2017-07-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the problem that WC materials are easy to agglomerate during preparation and have low catalytic activity to methanol, the invention provides a preparation method of tungsten carbide-carbon nanotube composite material

Method used

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  • Preparation method of three-dimensional network-shaped tungsten carbide-carbon nanotube composite material
  • Preparation method of three-dimensional network-shaped tungsten carbide-carbon nanotube composite material
  • Preparation method of three-dimensional network-shaped tungsten carbide-carbon nanotube composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Weigh 0.2g WCl in the glove box 6 , dissolved in 20mL of absolute ethanol, stirred evenly and placed in the InitiatorEXP microwave synthesizer, the reaction pressure of the microwave reaction was 15bar, and the reaction was carried out at 160°C for 1h. After the reaction was completed, it was cooled to room temperature, washed with deionized water and absolute ethanol for 3 times, and dried in a vacuum oven at 50°C for 6 hours.

[0040] 2. Put the dried sample above into a tube furnace, calcinate at 700°C for 3 hours in a CO atmosphere of 100mL / min, and then cool to room temperature under a nitrogen protective atmosphere to obtain WC-CNTs particles, which are marked as WC-CNTs- 700.

[0041] Depend on figure 1In the XRD pattern of WC-CNTs-700 shown in A, it can be concluded that the diffraction peaks at 2θ diffraction angle positions of 31.5°, 35.6°, 48.3°, 64.0°, 73.1°, and 75.5° belong to WC ( 001), (100), (101), (110), (111), (200) crystal faces (01-072-0097). ...

Embodiment 2

[0044] 1. Weigh 0.2g WCl in the glove box 6 , dissolved in 20mL of absolute ethanol, stirred evenly and placed in the InitiatorEXP microwave synthesizer, the reaction pressure of the microwave reaction was 15bar, and the reaction was carried out at 160°C for 1 hour. After the reaction was completed, it was cooled to room temperature, washed with deionized water and absolute ethanol for 3 times, and dried in a vacuum oven at 50°C for 6 hours.

[0045] 2. Put the dried sample above into a tube furnace, calcinate at 800°C for 3 hours in a CO atmosphere of 100mL / min, and then cool to room temperature under a nitrogen protective atmosphere to obtain WC-CNTs particles with carbon nanotubes grown. Marked as WC-CNTs-800.

[0046] Depend on figure 1 In the XRD pattern of WC-CNTs-800 shown in B, it can be concluded that the diffraction peaks at 2θ diffraction angle positions of 31.5°, 35.6°, 48.3°, 64.0°, 73.1°, and 75.5° belong to WC ( 001), (100), (101), (110), (111), (200) crystal...

Embodiment 3

[0049] 1. Weigh 0.2g WCl in the glove box 6 , dissolved in 20mL of absolute ethanol, stirred evenly and placed in the InitiatorEXP microwave synthesizer, the reaction pressure of the microwave reaction was 15bar, and the reaction was carried out at 160°C for 1h. After the reaction was completed, it was cooled to room temperature, washed with deionized water and absolute ethanol for 3 times, and dried in a vacuum oven at 50°C for 6 hours.

[0050] 2. Put the above-mentioned dried sample into a tube furnace, calcinate at 900°C for 3 hours under 100mL / min CO atmosphere, and then cool to room temperature under a nitrogen protective atmosphere to obtain WC particles with grown carbon nanotubes. Marked as WC-CNTs-900.

[0051] Depend on figure 1 In the XRD pattern of WC-CNTs-900 shown in C, it can be concluded that the diffraction peaks at 2θ diffraction angle positions of 31.5°, 35.6°, 48.3°, 64.0°, 73.1°, and 75.5° belong to WC ( 001), (100), (101), (110), (111), (200) crystal ...

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Abstract

The invention discloses a preparation method of a three-dimensional network-shaped tungsten carbide-carbon nanotube composite material. The preparation method comprises the steps of dissolving a tungsten source in a solvent in a microwave tube, placing the microwave tube in a microwave synthesis device after uniform stirring, and performing reaction for 40-60 minutes under 160-180 DEG C to obtain W18O49 with oxygen defect; and placing the W18O49 in a tubular furnace, performing carbonization at 700-900 DEG C under the atmosphere of a carbon source, and cooling the product to a room temperature under the atmosphere of nitrogen protection to obtain WC-CNTs particles. The preparation method is simple and practical to operate, a tungsten oxide with oxygen defect is used as a precursor, atomic diffusion is facilitated, and the carburization process is facilitated; and meanwhile, a carbon nanotube is grown on a tungsten substrate in an in-situ manner to form a complicated three-dimensional network structure taking WC small particles as branch points and a carbon tube as a framework, the WC particles can be effectively diffused, more contact surface between WC and pt is ensured, the conductivity of the composite material is integrally improved, the joint effect of the three parts is developed better, and an electrocatalytic effect is improved.

Description

[0001] (1) Technical field: [0002] The invention relates to a preparation method of a three-dimensional network tungsten carbide-carbon nanotube composite material. [0003] (two) background technology: [0004] Direct Methanol Fuel Cell (DMFC) has a simple structure, high specific energy density, and fuel methanol is abundant and easy to transport and store. This makes direct methanol fuel cells very suitable for vehicle and portable equipment power supply, and has become a current research hotspot. The catalysts used in fuel cells are mainly Pt and Pt-based noble metal catalysts, but Pt-based noble metal resources are scarce and expensive, and CO, an anodic oxidation product of methanol, is easily poisoned. The above-mentioned problems prevent large-scale commercial application and promotion of methanol fuel cells, which seriously restricts the application and development of fuel cells. Therefore, it is of great significance to develop non-precious metal catalysts, improv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/92H01M8/1011
CPCH01M4/9083H01M4/926H01M8/1011Y02E60/50
Inventor 施梅勤黄丽珍陈赵扬江叶坤
Owner ZHEJIANG UNIV OF TECH
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