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Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof

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, easy agglomeration, and difficult to refine the particle size, etc. problems, to achieve excellent hydrogen production activity, high stability, and short reaction cycle

Active Publication Date: 2019-04-09
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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  • Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof
  • Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof
  • Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof

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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

The invention discloses an ultra-small vanadium carbide embedded carbon atom layer material and a preparation method thereof. The preparation method comprises the steps: mixing dicyandiamide, ammoniummetavanadate and cobalt nitrate hexahydrate, and sufficiently grinding the mixture to obtain a reactant raw material; placing the reactant raw material into a porcelain boat, and carrying out one-step calcination in a tubular furnace in a vacuum or protective atmosphere to obtain a black powder; placing the black powder into an H2SO4 solution, then, carrying out vacuum drying, then, carrying outgrinding to obtain vanadium carbide coated with a carbon atom layer, namely the ultra-small vanadium carbide embedded carbon atom layer material having vanadium carbide particle size of smaller than 3nm and the crystallized carbon atom layer of 5-10 layers, uniform morphology and good dispersibility. Due to the adoption of a calcination method, the ultra-small vanadium carbide embedded carbon atom layer material is short in reaction period, uniform in chemical components and uniform in shapes and sizes and is used for a VC@CL hydrogen generation electrocatalyst which has high electrocatalyticactivity and stability in alkali electrolyte in acid. The cobalt nitrate hexahydrate in the reactant raw material not only promotes the crystallization of a carbon layer, but also inhibits the growthof VC crystal grains, so that ultra-small VC particles (not exceed 3 nm) are generated.

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 Applications(China)
IPC IPC(8): C01B32/914C01B32/205C25B1/04B82Y30/00B82Y40/00
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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