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Method for preparing multifunctional nickel-doped molybdenum disulfide in situ electrode by CVD (Chemical Vapor Deposition) method

A technology of molybdenum disulfide and in-situ electrodes, applied in electrodes, electrolytic processes, electrolytic components, etc., can solve the problems of increasing process complexity and cost

Active Publication Date: 2018-09-11
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, this preparation of doped MoS 2 Wet chemical methods are mostly used, such as hydrothermal, solvothermal, chemical bath, etc., and the prepared samples are mostly powders, which still need to be made into slurry or ink and then coated to form a film, which increases the complexity and cost of the process

Method used

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  • Method for preparing multifunctional nickel-doped molybdenum disulfide in situ electrode by CVD (Chemical Vapor Deposition) method
  • Method for preparing multifunctional nickel-doped molybdenum disulfide in situ electrode by CVD (Chemical Vapor Deposition) method
  • Method for preparing multifunctional nickel-doped molybdenum disulfide in situ electrode by CVD (Chemical Vapor Deposition) method

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Effect test

Embodiment 1

[0027] At room temperature, dissolve nickel chloride and molybdenum chloride in ethanol solution, the concentration of nickel chloride is 40mM, the concentration of molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms plus molybdenum atoms is 10%. Soak the carbon paper in the precursor solution, take it out, and dry it on a hot table at 80 °C for 10 min. Place the coated substrate in a tube furnace with N 2 Air vacuuming repeated three times to discharge the residual air in the tube furnace, and then pass N 2 Gas, the flow rate is 2SCCM, 1g of sulfur powder is placed on the upper part of the tube furnace, as the temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, in N 2 React in +S atmosphere at 550°C for 3 hours, take it out after natural cooling. figure 1 (a) HER, (b) OER, (c) ORR linear voltammetry (LSV) diagrams of the Ni-doped molybdenum disulfide in-situ electrode prepared in Example ...

Embodiment 2

[0029] Dissolve nickel chloride and molybdenum chloride in ethanol solution at room temperature, wherein the concentration of molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms plus molybdenum atoms is 10%. Soak the carbon paper in the precursor solution, take it out, and dry it on a hot table at 80 °C for 10 min. Put the coated substrate into the tube furnace, ventilate Ar gas to vacuumize repeatedly three times to discharge the residual air in the tube furnace, then vent Ar gas, the flow rate is 2SCCM, 1g of sulfur powder is placed on the upper part of the tube furnace, along with When the temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, react in Ar+S atmosphere at 800°C for 45min, and take it out after natural cooling. figure 2 OER linear voltammetry (LSV) diagram of the Ni-doped molybdenum disulfide in-situ electrode prepared in Example 2. As can be seen from the figure, the electr...

Embodiment 3

[0031] Dissolve nickel chloride and molybdenum chloride in ethanol solution at room temperature, wherein the concentration of molybdenum chloride is 360mM, and the ratio of nickel atoms to the sum of the number of nickel atoms plus molybdenum atoms is 10%. Soak the carbon paper in the precursor solution, take it out, and dry it on a hot table at 80 °C for 10 min. Put the coated substrate into the tube furnace, and repeatedly discharge the residual air in the tube furnace with Ar gas and vacuumize it three times, and then pass Ar gas at a flow rate of 1 SCCM. As the temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, react at 800°C for 45 minutes in an Ar+S atmosphere, and take it out after natural cooling. image 3 The OER linear voltammetry (LSV) diagram of the Ni-doped molybdenum disulfide in-situ electrode prepared in Example 3. It can be seen from the figure that the electrode prepared in this embodiment has good oxygen evolution perf...

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Abstract

The invention provides a method for preparing a multifunctional nickel-doped molybdenum disulfide in situ electrode by CVD (Chemical Vapor Deposition) method. The method comprises the following steps:dissolving nickel salt and molybdenum chloride in a volatile non-aqueous solvent to obtain Ni-Mo precursor liquid; coating a substrate with the precursor liquid; and drying the substrate, and then, putting the dried substrate in an Ar+S atmosphere or in an N2+S atmosphere so as to be subjected to CVD vulcanization. The product obtained by the method provided by the invention has the advantages oflow equipment requirements, low required raw material cost, easy control on reaction conditions, simple production processes, good formed product uniformity, little environmental pollution and the like, and can be used for multifunctional electro-catalysts for HER (Hydrogen Evolution Reaction), OER (Oxygen Evolution Reaction) and ORR (Oxygen Reduction Reaction).

Description

technical field [0001] The invention relates to an in-situ electrode and its preparation, and belongs to the field of energy storage and conversion materials and devices. Background technique [0002] Molybdenum disulfide MoS 2 As a new type of graphite material, it is widely used in many fields such as hydrodesulfurization, lithium-ion batteries, supercapacitors, hydrogen production by electrolysis of water, and dye-sensitized solar cells. The Mo and S atoms at the edge of the molybdenum disulfide layer have high catalytic activity due to unsaturated coordination, while the saturated S atoms in the layer are basically inert. Studies have shown that molybdenum disulfide doped with transition metal elements such as cobalt and nickel can effectively improve its catalytic performance in hydrodesulfurization and hydrogen production by electrolysis of water. Bao Xinhe’s research group (Energy Environ.Sci., 2015, 8, 1594-1601.) found that the incorporation of nickel greatly impr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/04C25B11/06
CPCC25B1/04C25B11/091Y02E60/36
Inventor 黄妞闫术芳丁玉岳孙小华孙盼盼
Owner CHINA THREE GORGES UNIV
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