Molybdenum carbide material and molybdenum carbide@molybdenum sulfide composite material, and preparation methods and applications thereof

A composite material, molybdenum carbide technology, applied in the direction of molybdenum sulfide, carbide, tungsten/molybdenum carbide, etc., can solve the problems of easy stacking of two-dimensional layered structure, low catalytic activity, limited active sites, etc., to achieve improvement Structure and performance improvement and application, the effect of high catalytic activity and high conductivity

Active Publication Date: 2018-12-18
SHENZHEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide molybdenum carbide materials, molybdenum carbide@molybdenum sulfide composite materials and their preparation methods and applications, aiming to solve the problems of existing molybdenum-based HER electrocatalysts with

Method used

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  • Molybdenum carbide material and molybdenum carbide@molybdenum sulfide composite material, and preparation methods and applications thereof
  • Molybdenum carbide material and molybdenum carbide@molybdenum sulfide composite material, and preparation methods and applications thereof
  • Molybdenum carbide material and molybdenum carbide@molybdenum sulfide composite material, and preparation methods and applications thereof

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preparation example Construction

[0036] The present invention provides a kind of preparation method of molybdenum carbide material, wherein, comprise:

[0037] Step A: Add carbon source and molybdenum source to the dispersion, stir for 6-12 h (preferably 8 h), then dry at 80-120 °C for 12-24 h, grind for 20-30 min, collect, and form carbonization Molybdenum precursor;

[0038] Step B. Place the above-mentioned molybdenum carbide precursor in a clean magnetic boat, place the magnetic boat in a tube furnace, and raise the temperature of the molybdenum carbide precursor from room temperature to 400-900 °C under an inert atmosphere , calcined at this temperature for 1-3 h, ground and collected to obtain molybdenum carbide material.

[0039] Specifically, in step A, the carbon source is selected from one or more of dicyandiamine, melamine, cyanuric acid, benzomelamine, urea, glucose and sucrose. The above-mentioned carbon source of the present invention is relatively common and easy to obtain, which is conducive...

Embodiment 1

[0053] Example 1 Preparation, characterization and electrocatalytic performance test of molybdenum carbide material

[0054] (1) Weigh 1.26 g of melamine, 1.29 g of cyanuric acid, and 0.618 g of ammonium heptamolybdate into a beaker, add 60 mL of deionized water, stir for 8 h to form a uniform dispersion, and put it in a drum at 80 °C Dry in an air oven, then grind for 30 min and collect to obtain the molybdenum carbide precursor.

[0055] (2) Place the above-mentioned molybdenum carbide precursor in a clean magnetic boat, and place the magnetic boat in a tube furnace. Under a nitrogen atmosphere, the temperature of the tube furnace is programmed from room temperature to 750 °C at a rate of 5 °C / min. ℃, and calcined at 750 ℃ ​​for 2 h, then the tube furnace was naturally cooled to 100 ℃, the samples were taken out, ground and collected to obtain molybdenum carbide materials.

[0056] The molybdenum carbide material was tested by X-ray powder diffraction (XRD for short), and t...

Embodiment 2

[0058] Preparation, characterization and electrocatalytic performance test of embodiment 2 molybdenum carbide material

[0059] (1) Weigh 1.29 g of melamine, 1.29 g of cyanuric acid, and 0.618 g of ammonium heptamolybdate into a beaker, add 60 mL of deionized water, stir for 8 h to form a uniform dispersion, and put it in a drum at 80 °C Dry in an air oven, then grind for 30 min and collect to obtain the molybdenum carbide precursor.

[0060] (2) Place the above molybdenum carbide precursor in a clean magnetic boat, and place the magnetic boat in a tube furnace. Under an argon atmosphere, the tube furnace is programmed to heat up from room temperature to 550 °C, and calcined at 550 °C for 2 h, then the tube furnace was naturally cooled to 100 °C, the samples were taken out, ground and collected to obtain molybdenum carbide materials.

[0061] Carry out X-ray powder diffraction test to this molybdenum carbide material, its XRD pattern is as follows Image 6 Shown; Field emiss...

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Abstract

The invention discloses a molybdenum carbide material and a molybdenum carbide@molybdenum sulfide composite material, and preparation methods and applications thereof. The preparation method of the molybdenum carbide material comprises the following steps: adding a carbon source and a molybdenum source to a dispersion liquid, performing stirring for 6-12 h, drying the obtained mixture at 80-120 DEG C, grinding the dried mixture, and collecting the ground mixture to form a molybdenum carbide precursor; and performing temperature programming on the molybdenum carbide precursor to 400-900 DEG C from room temperature in an inert atmosphere, calcining the precursor at 400-900 DEG C for 1-3 h, grinding the calcined precursor, and collecting the ground calcined precursor to obtain molybdenum carbide. The molybdenum carbide is vulcanized at 160-400 DEG C by using a vulcanizing agent to obtain molybdenum carbide@molybdenum sulfide. The molybdenum carbide and the molybdenum carbide@molybdenum sulfide respectively have the morphology of a porous nanosheet structure, and the microstructure facilitates storage of an electrolyte and reduction of the charge transfer impedance and provides a lot of electrocatalytic activity sites; and the material and the composite material can be used as an HER electrocatalyst, have a high catalytic activity and a good stability, and are expected to replace aPt-based catalyst for electrolysis of water to produce hydrogen.

Description

technical field [0001] The invention relates to the technical field of preparation of molybdenum-based hydrogen evolution reaction electrocatalysts, in particular to molybdenum carbide materials, molybdenum carbide@molybdenum sulfide composite materials, preparation methods and applications. Background technique [0002] The rapid economic development has brought about an increasing demand for energy, and the environmental crisis has prompted people to pursue more sustainable and clean fuels, among which hydrogen largely meets the requirements for future energy. Currently, the production of industrial hydrogen relies heavily on methane reforming and coal gasification, which still rely on limited and non-renewable fossil fuels while generating large amounts of carbon dioxide. In addition, hydrogen production from water splitting using renewable energy sources, such as wind and solar energy, has become a research focus in recent years. The dissociation and desorption of hydro...

Claims

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Application Information

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IPC IPC(8): C01B32/949C01G39/06C25B11/06C25B1/04B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G39/06C01P2002/72C01P2004/03C01P2004/04C01P2004/24C01P2004/80C01P2006/40C25B1/04C01B32/949C25B11/091Y02E60/36
Inventor 范梁栋张卉唐超云
Owner SHENZHEN UNIV
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