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CVD preparation method of Co-doped MoS2 array in-situ electrodes

An in-situ electrode and array technology, applied in the field of in-situ electrode and its preparation, can solve the problems of inability to achieve vertical growth of molybdenum disulfide sheets, increase process complexity and cost, etc.

Active Publication Date: 2018-08-10
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this Co-doped MoS 2 It is a powder, and it still needs to be made into a slurry or ink and then coated to form a film, which increases the complexity and cost of the process and cannot achieve the vertical growth of molybdenum disulfide sheets

Method used

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  • CVD preparation method of Co-doped MoS2 array in-situ electrodes
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  • CVD preparation method of Co-doped MoS2 array in-situ electrodes

Examples

Experimental program
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Effect test

Embodiment 1

[0022] At room temperature, dissolve cobalt chloride and molybdenum chloride in ethanol solution, wherein the concentration of cobalt chloride is 10mM, the concentration of molybdenum chloride is 290mM, and the ratio of cobalt atoms to the sum of the number of cobalt atoms plus molybdenum atoms is 5%. , through Ar gas and vacuum repeatedly three times to discharge the residual air in the tube furnace, then through Ar, the flow rate is 5SCCM, 0.2g 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 Sulfur vapors are formed. The precursor liquid was drop-coated on the surface of a flat graphite paper substrate, and dried on a hot table at 90°C for 10 min. Put the coated substrate into a tube furnace, react at 800°C for 30min under an Ar+S atmosphere, and take it out after natural cooling. figure 1 The SEM picture of this embodiment is shown, and it can be seen from the picture that a small ...

Embodiment 2

[0024] At room temperature, dissolve cobalt chloride and molybdenum chloride in ethanol solution, wherein the concentration of molybdenum chloride is 290mM, and the ratio of cobalt atoms to the sum of the number of cobalt atoms plus molybdenum atoms is 10%. The precursor liquid was drop-coated on the surface of a flat graphite paper substrate, and dried on a hot table at 90°C for 10 min. Put the coated substrate into the tube furnace, ventilate Ar gas and vacuumize repeatedly three times to discharge the residual air in the tube furnace, then pass Ar again, the flow rate is 2SCCM, 1g of sulfur powder is placed on the upper part of the tube furnace, along with the The temperature in the type furnace rises, the sulfur powder evaporates to form sulfur vapor, and reacts at 800°C for 30 minutes in an Ar+S atmosphere, and takes it out after natural cooling. figure 2 The SEM image of this embodiment is shown, and it can be seen from the figure that many nanosheets with a width of ~1...

Embodiment 3

[0026] At room temperature, dissolve cobalt chloride and molybdenum chloride in ethanol solution, wherein the concentration of molybdenum chloride is 290mM, and the ratio of cobalt atoms to the sum of the number of cobalt atoms plus molybdenum atoms is 15%. The precursor liquid was drop-coated on the surface of a flat graphite paper substrate, and dried on a hot table at 90°C for 10 min. Put the coated substrate into the middle of the tube furnace, and repeatedly discharge the residual air in the tube furnace with Ar gas and vacuumize it three times, then pass Ar again at a flow rate of 1 SCCM, put 0.5g of sulfur powder on the upper part of the tube furnace, and then As the temperature in the tube furnace rises, the sulfur powder evaporates to form sulfur vapor, react in an Ar+S atmosphere at 800°C for 30 minutes, and take it out after natural cooling. image 3 (a) shows the SEM image of this embodiment, from which it can be seen that many nanosheets with a width of 150-200 nm...

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Abstract

The invention provides a CVD preparation method of Co-doped MoS2 array in-situ electrodes. The preparation method specifically comprises the steps that cobalt salt and molybdenum chloride are dissolved in a volatilized non-aqueous solvent to obtain a Co-Mo precursor solution, a substrate is coated with the precursor solution, and CVD vulcanization is carried out in the atmosphere of Ar and S or inthe atmosphere of N2 and S, specifically, the vulcanization reaction temperature is 600-800 DEG C, and the vulcanization reaction time is from 10 min to 2 h. According to the technical scheme, the CVD preparation method can be applied to electrolytic hydrogen making and dye sensitization solar cells and has a great significance on batch production of the in-situ electrodes.

Description

technical field [0001] The invention relates to an in-situ electrode and a preparation method thereof, and belongs to the field of new materials for energy storage and conversion. 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. MoS 2 The S-Mo-S in the layer is combined by covalent bonds, and the interlayer is combined by molecular bonds, so the conductivity in the layer is thousands of times that of the interlayer. In addition, the Mo and S atoms at the edge of the molybdenum disulfide layer have high catalytic activity due to coordination unsaturation, while the coordination-saturated S atoms in the layer are basically inert. Therefore, the preparation of molybdenum sulfide sheets in which the S-Mo-S layer grows perpendicular to the substrate will g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/06C25B1/04C23C16/30H01G9/20
CPCC23C16/305C25B1/04C25B11/091H01G9/20Y02E10/542Y02E60/36Y02P70/50
Inventor 黄妞彭荣诚黄华孙小华孙盼盼
Owner CHINA THREE GORGES UNIV
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