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Co-doped in-situ MoS2 electrode and a preparation method thereof

A molybdenum disulfide, in-situ electrode technology, applied in chemical instruments and methods, cobalt compounds, inorganic chemistry, etc., can solve the problem of weak conductivity of molybdenum disulfide, affecting electron transport, restricting electrocatalytic chemical reactions and electrode stability, etc. question

Active Publication Date: 2018-05-18
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In addition, the conductivity of MoS2 is weak, and its poor electrical contact with the conductive substrate will also affect the transport of electrons, thereby restricting the electrocatalytic chemical reaction and the stability of the electrode.

Method used

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  • Co-doped in-situ MoS2 electrode and a preparation method thereof
  • Co-doped in-situ MoS2 electrode and a preparation method thereof
  • Co-doped in-situ MoS2 electrode and a preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] At room temperature, dissolve 0.9 mmol of molybdenum chloride in 3 mL of ethanol solution, then add 0.1 mmol of cobalt chloride, stir and dissolve the cobalt chloride, add 3 mmol of thiourea, and stir and dissolve the thiourea. Apply 100 μL of the precursor liquid onto a flat 2.5 cm×2.5 cm graphite paper surface, and dry it on a hot stage at 90° C. for 10 min. The substrate coated with Co-Mo-S was placed in a tube furnace for solid-state reaction at 600 °C for 1 h under the protection of Ar. After the furnace temperature cools naturally, take it out. An electrode uniformly loaded with cobalt-doped molybdenum disulfide on graphite paper can be obtained, and the loading capacity is about 270μg / cm 2 . figure 1 The powder XRD of cobalt-doped molybdenum disulfide prepared in Example 1 is shown. It can be seen from the figure that the phase of cobalt-doped molybdenum disulfide is 2H-type molybdenum disulfide, and there are no other impurity phases. It is initially indicated...

Embodiment 2

[0028] At room temperature, dissolve 1.8 mmol of molybdenum chloride in 3 mL of ethanol solution, then add 0.2 mmol of cobalt chloride, stir and dissolve the cobalt chloride, add 4 mmol of thiourea, and stir and dissolve the thiourea. Apply 100 μL of the precursor liquid onto a flat graphite paper surface of 2.5 cm×2.5 cm, and dry it on a hot stage at 70° C. for 20 min. The substrate coated with Co-Mo-S was placed in a tube furnace for solid-state reaction at 600 °C for 1 h under the protection of Ar. After the furnace temperature cools naturally, take it out. An electrode uniformly loaded with cobalt-doped molybdenum disulfide on graphite paper can be obtained, and the loading capacity is about 540 μg / cm 2 . figure 1 The powder XRD of cobalt-doped molybdenum disulfide prepared in Example 2 is shown. It can be seen from the figure that most of the phases of cobalt-doped molybdenum disulfide are 2H type molybdenum disulfide, but there is a small amount of Co 9 S 8 .

Embodiment 3

[0030] At room temperature, dissolve 0.9 mmol of molybdenum chloride in 3 mL of ethanol solution, then add 0.1 mmol of cobalt chloride, stir and dissolve the cobalt chloride, add 3 mmol of thiourea, and stir and dissolve the thiourea. 100 μL of the precursor solution was dropped onto a flat surface of 2.5 cm×2.5 cm graphite paper, and dried on a hot stage at 80° C. for 15 min. The substrate coated with Co-Mo-S was placed in a tube furnace for solid-state reaction at 800 °C for 30 min under the protection of Ar. After the furnace temperature cools naturally, take it out. An electrode uniformly loaded with cobalt-doped molybdenum disulfide on graphite paper can be obtained, and the loading capacity is about 270μg / cm 2 . Figure 5The powder SEM-EDS of cobalt-doped molybdenum disulfide prepared in Example 3 is shown. It can be seen from the figure that cobalt element is easy to concentrate on the surface of the sample at a high temperature of 800°C.

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Abstract

The invention provides a Co-doped in-situ MoS2electrode. Co-doped MoS2 is formed by uniformly replacing Mo with Co, and the physical phase of Co-doped MoS2 is 2H MoS2. A specific preparation method comprises steps as follows: MoCl5 is dissolved in an ethanol solution at room temperature, Co salt is added, then thiourea is added, the materials are stirred and dissolved, and a Co-Mo-S precursor solution is obtained; the precursor solution is dropwise or rotationally applied to a substrate and rapidly dried at 70-100 DEG C, and a precursor film is obtained; the precursor film obtained in the steptwo is sintered for 0.5-2 h at 500-800 DEG C under argon or nitrogen protection, cooled with the furnace and then taken out, and the Co-doped in-situ MoS2 electrode is obtained. On the basis of mixing uniformity of Co, Mo and S atoms in the Co-Mo-S precursor solution and the easy uniform film-forming property of the Co-Mo-S precursor solution, Co-doped MoS2 is prepared through high-temperature solid phase reaction at the temperature of 500-800 DEG C; compared with pyrolytic Pt electrodes, the Co-doped in-situ electrode grows with higher stability.

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] As a new type of two-dimensional transition metal sulfide, molybdenum disulfide has become a research hotspot in many fields due to its special physical and chemical properties, such as hydrodesulfurization, hydrogen production by electrolysis of water, field effect transistors, solar cells, sensors, etc. , lithium-ion electronics and supercapacitors, etc. Studies have shown that the active sites of molybdenum disulfide are located at the edge of the sheet structure, while the inside of the sheet plane (basal plane) is basically inert. Therefore, a lot of research work has been devoted to defect regulation to increase the edge of Mo or S, or to structural optimization to allow MoS2 to grow vertically to the substrate to expose more edge sites. Recently, Bao Xinhe's r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00
Inventor 黄妞郑方孙小华孙盼盼
Owner CHINA THREE GORGES UNIV
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