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An ultra-small vanadium carbide embedded carbon atomic layer material and its preparation method

A technology of carbon atoms and ultra-small carbons, applied in chemical instruments and methods, carbon compounds, nanotechnology for materials and surface science, etc., can solve the problems of difficult to meet the requirements of electrocatalysts, difficult to refine particle size, easy agglomeration, etc. question

Active Publication Date: 2021-04-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Looking at the literature in the past 15 years, we can see that the exploration of vanadium carbide materials in my country is mainly concentrated in the field of cermet material preparation. The synthesis process is diverse, but the same, basically can be attributed to the calcination method, using carbon source, vanadium source, with or without additives Firing in a high-temperature furnace, the material prepared by this method is easy to agglomerate during the sintering process, and the particle size is difficult to refine. At present, the minimum particle size of vanadium carbide prepared in China is 50nm, and most of them are used in the field of cermet materials, which is difficult to meet the requirements of electrocatalysts. Require

Method used

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  • An ultra-small vanadium carbide embedded carbon atomic layer material and its preparation method
  • An ultra-small vanadium carbide embedded carbon atomic layer material and its preparation method
  • An ultra-small vanadium carbide embedded carbon atomic layer material and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0024] Step 1: get 1.625g of dicyandiamide, 0.025g of ammonium metavanadate and 0.225g of cobalt nitrate hexahydrate, mix and fully grind to obtain reactant raw materials;

[0025] Step 2: Put the raw material of the reactant in a porcelain boat, place it in a tube furnace under an argon atmosphere, and raise the temperature from room temperature to 800°C at a heating rate of 5°C / min, and keep it warm for 4 hours to obtain a black powder;

[0026] Step 3: Put the black powder in 0.5mol / L H 2 SO 4 After vacuum drying for 10 h, the ultra-small vanadium carbide intercalated carbon atomic layer material (VC@CL hydrogen-producing electrocatalyst) was obtained.

[0027] Depend on figure 1 It can be seen that the prepared ultra-small vanadium carbide embedded carbon atomic layer material (VC@CL hydrogen production electrocatalyst) corresponds to the VC standard PDF card number 73-0476, and the four diffraction peaks correspond to the crystal planes (111), (200) , (220) and (311), ...

Embodiment 2

[0029] Step 1: get 1.625g of dicyandiamide, 0.025g of ammonium metavanadate and 0.3g of cobalt nitrate hexahydrate, mix and fully grind to obtain reactant raw materials;

[0030] Step 2: Put the raw material of the reactant in a porcelain boat, place it in a tube furnace under an argon atmosphere, raise the temperature from room temperature to 500°C at a rate of 5°C / min, and keep it warm for 2 hours to obtain a black powder;

[0031] Step 3: Put the black powder in 0.5mol / L H 2 SO 4 After 15 hours in the vacuum, the ultra-small vanadium carbide intercalated carbon atomic layer material (VC@CL hydrogen production electrocatalyst) was obtained after vacuum drying.

Embodiment 3

[0033] Step 1: get 2g of dicyandiamide, 0.025g of ammonium metavanadate and 0.25g of cobalt nitrate hexahydrate, mix and fully grind to obtain reactant raw materials;

[0034] Step 2: Put the raw material of the reactant in a porcelain boat, place it in a tube furnace under a nitrogen atmosphere, and raise the temperature from room temperature to 1000°C at a heating rate of 7°C / min, and keep it warm for 1 hour to obtain a black powder;

[0035] Step 3: Put the black powder in 0.5mol / L H 2 SO 4 After vacuum drying for 20 h, the ultra-small vanadium carbide intercalated carbon atomic layer material (VC@CL hydrogen-producing electrocatalyst) was obtained.

[0036] Depend on figure 2 It can be seen that the microstructure of the prepared ultra-small vanadium carbide embedded carbon atomic layer material (VC@CL hydrogen production electrocatalyst) is vanadium carbide coated with carbon atomic layer, and the particle size of vanadium carbide is less than 3nm. The crystal plane i...

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Abstract

An ultra-small vanadium carbide embedded carbon atomic layer material and a preparation method thereof. Dicyandiamide, ammonium metavanadate, and cobalt nitrate hexahydrate are mixed and fully ground to obtain a reactant raw material; the reactant raw material is placed in a porcelain boat, Place the black powder in a tube furnace for one-step calcination under vacuum or protective atmosphere; put the black powder in H 2 SO 4 After the solution is dried in vacuum, it is ground to obtain vanadium carbide coated with a carbon atom layer. The vanadium carbide particle size is less than 3nm, and the crystallized carbon atom layer is 5‑10 layers. The shape is uniform and the dispersion is good. layer material. The VC@CL hydrogen-producing electrocatalyst with short reaction period, uniform material chemical composition, uniform shape and size, high electrocatalytic activity and high stability in acid, medium and alkali electrolytes is adopted. The cobalt nitrate hexahydrate in the raw material of the reactant not only promotes the crystallization of the carbon layer, but also inhibits the growth of VC grains, resulting in the generation of ultra-small VC particles (less than 3nm).

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis and application, in particular to an ultra-small vanadium carbide embedded carbon atom layer material and a preparation method thereof. Background technique [0002] With the intensification of energy problems, the demand for energy in human society is increasing, and hydrogen energy, as a new generation of clean and sustainable energy, has attracted widespread attention, and at the same time promoted the development of hydrogen. Hydrogen production by water splitting is an efficient means of hydrogen production, so the development of efficient hydrogen production catalysts is the key to this technology. Platinum-based catalysts are considered to be the most efficient catalysts for hydrogen production, but their high cost and low content limit their industrial applications. Therefore, it is necessary to find non-noble metal electrocatalysts that can replace platinum-based catalysts, in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/914C01B32/205C25B1/04C25B11/04B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01P2002/72C01P2004/01C01P2004/04C25B1/04C01B32/205C01B32/914Y02E60/36
Inventor 冯亮亮白嘉玺黄倩张宁
Owner SHAANXI UNIV OF SCI & TECH
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