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Solvothermal preparation method of in-situ molybdenum disulfide electrode

A technology of molybdenum disulfide and in-situ electrodes, applied in the direction of coating, etc., to achieve the effect of preventing oxidation, improving purity and electrocatalytic activity

Inactive Publication Date: 2016-07-06
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis process needs to be further optimized, and the conductivity and electrocatalytic activity of the prepared molybdenum disulfide electrodes need to be further improved.

Method used

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  • Solvothermal preparation method of in-situ molybdenum disulfide electrode
  • Solvothermal preparation method of in-situ molybdenum disulfide electrode
  • Solvothermal preparation method of in-situ molybdenum disulfide electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve 2mM molybdenum chloride and 7mM thiourea in ethylene glycol solution, add a piece of fluorine-doped tin oxide conductive glass with an area of ​​1.5cm*7cm, and then put it into a hydrothermal kettle and heat it in a solvent at 200°C for 6h, in which molybdenum The atomic ratio of atoms and sulfur atoms is 1:3.5. The molybdenum disulfide in-situ electrode can be obtained by taking out the substrate, cleaning it, and drying it.

[0020] figure 1 The molybdenum disulfide in-situ electrode (2mMMoO 4 2- ) light transmittance. It can be seen from the figure that the molybdenum disulfide electrode has high transparency, and about 85% of ultraviolet-visible-near-infrared light can pass through the molybdenum disulfide film.

Embodiment 2

[0022] Dissolve 5mM sodium molybdate and 25mM thiourea in ethylene glycol solution, and add a piece of fluorine-doped tin oxide conductive glass with an area of ​​1.5cm*7cm, and then put it into a hydrothermal kettle and heat it at 200°C for 6 hours, in which molybdenum The atomic ratio of atoms to sulfur atoms is 1:5. Take out the substrate, wash it, dry it and put it in N 2 Annealing at 500°C for 1 h in the atmosphere can obtain molybdenum disulfide in-situ electrodes.

[0023] figure 1 The molybdenum disulfide in-situ electrode (5mMMoO 4 2- ) light transmittance. It can be seen from the figure that the molybdenum disulfide electrode has high transparency, and about 75% of ultraviolet-visible-near-infrared light can pass through the molybdenum disulfide film.

[0024] figure 2 Powder XRD of the sample prepared for this implementation example. The comparison with the standard PDF card shows that the prepared sample is molybdenum disulfide.

[0025] image 3 SEM imag...

Embodiment 3

[0027] Dissolve 5mM sodium molybdate and 35mM thioacetamide in ethylene glycol solution, and add a piece of fluorine-doped tin oxide conductive glass with an area of ​​1.5cm*7cm, then put it into a hydrothermal kettle and heat it in a solvent at 200°C for 12h , where the atomic ratio of molybdenum atoms to sulfur atoms is 1:7. Take out the substrate, wash it, dry it and put it in N 2 Annealing at 500°C for 1 h in the atmosphere can obtain molybdenum disulfide in-situ electrodes.

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Abstract

The invention discloses a solvothermal preparation method of an in-situ molybdenum disulfide electrode. The preparation method comprises the following steps: dissolving molybdenum-containing salts (sodium molybdate, etc.) into an alcohol solution containing a sulfur source (thiourea, etc.), adding a substrate material, then filling the mixture into a hydrothermal kettle, carrying out solvothermal reactions for 6 to 24 hours at a temperature of 180 to 230 DEG C; taking out the substrate, and cleaning and drying the substrate. If people want to improve the crystallization property of molybdenum disulfide, the substrate can be annealed in an atmosphere of N2 for one hour at a temperature of 500 DEG C. The prepared in-situ molybdenum disulfide electrode has the advantages of high transparency and uniformity, and strong adhesion force on substrate. The dye-sensitized solar cell prepared from the provided in-situ molybdenum disulfide electrode has a higher photoelectric conversion efficiency, compared with the cells prepared from a conventional pyrolytic Pt electrode, and the result shows that the prepared molybdenum disulfide electrode has an extremely good electro-catalytic activity.

Description

technical field [0001] The invention relates to an in-situ electrode and a preparation method thereof, and belongs to the field of new conductive and electrocatalytic materials. Background technique [0002] Molybdenum sulfide, because of its unique chemical properties, optical, electrical, magnetic and other physical properties and good stability, is widely used in diagnostic materials, optoelectronic materials, sulfide glass, luminescent materials, industrial catalysts, etc., and can also be used as Electrode materials for dye-sensitized solar cells, quantum dot solar cells, lithium-ion batteries, supercapacitors, fuel cells, etc. [0003] Although there are many synthesis methods of molybdenum sulfide, these methods usually use high-temperature gas-phase synthesis or high-temperature solid-phase and thermal decomposition of organic matter, etc. These methods have high requirements on equipment conditions, require many types of raw materials, and high raw material costs ,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/22
CPCC03C17/22C03C2217/288C03C2218/111
Inventor 黄妞孙小华孙盼盼李文静项长华
Owner CHINA THREE GORGES UNIV
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