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Preparation method for cobalt sulfide and molybdenum disulfide in-situ composite electrode and application of cobalt sulfide and molybdenum disulfide in-situ composite electrode in hydrogen production by water electrolysis

A technology of molybdenum disulfide and in-situ compounding, which is applied in the direction of electrodes, electrolytic processes, electrolytic components, etc., and can solve problems such as complex processes

Active Publication Date: 2018-08-17
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it requires two-step microwave hydrothermal preparation, and the process is still relatively complicated

Method used

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  • Preparation method for cobalt sulfide and molybdenum disulfide in-situ composite electrode and application of cobalt sulfide and molybdenum disulfide in-situ composite electrode in hydrogen production by water electrolysis
  • Preparation method for cobalt sulfide and molybdenum disulfide in-situ composite electrode and application of cobalt sulfide and molybdenum disulfide in-situ composite electrode in hydrogen production by water electrolysis
  • Preparation method for cobalt sulfide and molybdenum disulfide in-situ composite electrode and application of cobalt sulfide and molybdenum disulfide in-situ composite electrode in hydrogen production by water electrolysis

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Dissolve molybdenum chloride in ethanol solution at room temperature, stir to dissolve, and obtain 450 mM molybdenum chloride ethanol solution. will grow with Co 3 o 4 The carbon paper substrate of the array was soaked in molybdenum chloride solution, and dried on a hot stage at 80°C for 10 min after taking it out. 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 2 SCCM. As the temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, react in an Ar+S atmosphere at 600°C for 30 minutes, and take it out after natural cooling. figure 1 for the growth of Co 3 o 4 (a) SEM and (b) XRD patterns of the arrayed carbon paper, Co 3 o 4 The array adopts the method reported by Kuo-Chuan Ho et al. (ACS nano, 2012, 6, 7016.), specifically 10.6667g urea, 5.7108g CoCl 2 ·6H 2 O was dissolved in 160mL water,...

Embodiment 2

[0026] Dissolve molybdenum chloride in ethanol solution at room temperature, stir to dissolve, and obtain 450 mM molybdenum chloride ethanol solution. will grow with Co 3 o 4 The carbon paper substrate of the array was soaked in molybdenum chloride solution, and dried on a hot table at 90°C for 10 min after taking it out. 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, and then ventilate Ar gas with a flow rate of 1 SCCM. The temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, and reacts at 600°C for 1 hour in an Ar+S atmosphere, and takes it out after natural cooling. Figure 4(a) SEM image and (b) linear voltammetry scanning performance in 1M KOH of the in-situ composite electrode of cobalt sulfide and molybdenum disulfide prepared in Example 2. It can be seen from the figure that when the hydrogen-producing electrode passes through...

Embodiment 3

[0028] Dissolve molybdenum chloride in ethanol solution at room temperature, stir to dissolve, and obtain 570 mM molybdenum chloride ethanol solution. will grow with Co 3 o 4 The carbon paper substrate of the array was soaked in molybdenum chloride solution, and dried on a hot stage at 80°C for 10 min after taking it out. 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, and then ventilate Ar gas with a flow rate of 1 SCCM. The temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, and reacts at 600°C for 2 hours in an Ar+S atmosphere, and takes it out after natural cooling. Figure 5 (a) in 0.5M H 2 SO 4 The linear voltammetric scanning performance in (b) the linear voltammetric scanning performance in 1M PBS solution (PH=7.17), Image 6 is its linear voltammetry sweep performance in 1M KOH. It can be seen from the figure that when the...

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Abstract

The invention provides a preparation method for a cobalt sulfide and molybdenum disulfide in-situ composite electrode. The preparation method particularly comprises the following steps that molybdenumchloride is dissolved in ethanol under the condition of stirring at room temperature, and a precursor solution is obtained; and a substrate on which a cobaltosic oxide array grows is coated with theprecursor solution, the substrate coated with the precursor solution is subjected to high-temperature one-step vulcanization in an Ar+S atmosphere or N2+S atmosphere after being dried and is cooled with a furnace and taken out, and the molybdenum disulfide / molybdenum disulfide composite in-situ electrode is obtained. According to the technical scheme of the preparation method, cobaltosic oxide reacts with sulfur at the high temperature to generate nano-sized cobalt sulfide, and molybdenum disulfide generated by the molybdenum chloride and sulfurization gas phase reaction is deposited around the nano-sized cobalt sulfide to form a heterogeneous interface which has a synergistic and high catalytic effect, is in close contact between cobalt sulfide and molybdenum disulfide and has a large contact area between cobalt sulfide and molybdenum disulfide while a nano-sized pore passageway is left.

Description

technical field [0001] The invention relates to an in-situ composite electrode and its one-step preparation, and belongs to the field of new materials and devices for energy storage and conversion. Background technique [0002] Molybdenum disulfide is a new type of two-dimensional layered transition metal sulfide similar to graphite. The three atomic layers of S-Mo-S are connected by covalent bonds in the layer, and the S-Mo-S layers are bonded by van der Waals bonds. . Because of its special photoelectric, physical and chemical properties, molybdenum disulfide can be used in many fields, such as hydrodesulfurization, dye-sensitized solar cell counter electrode, hydrogen production by electrolysis of water, sensors, field effect transistors, lithium ion electronics and supercapacitors, etc. . Studies have shown that molybdenum disulfide is an efficient and stable catalyst, and density functional theory calculations indicate that the layer edge of molybdenum disulfide has e...

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 黄妞丁玉岳黄华闫术芳孙小华孙盼盼
Owner CHINA THREE GORGES UNIV
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