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Micron molybdenum disulfide hydrogen evolution electro-catalytic material, preparation method and application of micron molybdenum disulfide hydrogen evolution electro-catalytic material

An electrocatalytic material, molybdenum disulfide technology, applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of difficult to obtain micron or nanoscale materials, high hydrogen evolution overpotential, difficult to efficiently controllable combination, etc., to achieve good industrialization Basic production, good repeatability, and low-cost effects

Inactive Publication Date: 2016-10-26
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At this stage, various MoS 2 The synthesis of and their use as hydrogen evolution electrode materials have been reported in the literature, but they have certain limitations
Chinese patent (CN 102849798A) provides a kind of MoS 2 Preparation of micron sheet film and its use as hydrogen evolution electrode material, MoS prepared by this method 2 Microsheets grow vertically and orderly on the substrate to form MoS 2 Thin film, the film Tafel slope is small (52mV / dec), has high electrochemical stability, its disadvantage is that the preparation is relatively cumbersome and has a high hydrogen evolution overpotential (-30mv)
This method usually forms aggregates of larger particles, and it is difficult to obtain micron or nanoscale materials, and the preparation process of conductive substrates such as graphene or carbon nanotubes is often costly, and the environmental pollution is large, which is difficult to be efficient and controllable Synthesis of micron-sized MoS with low hydrogen evolution overpotential 2 Material

Method used

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  • Micron molybdenum disulfide hydrogen evolution electro-catalytic material, preparation method and application of micron molybdenum disulfide hydrogen evolution electro-catalytic material
  • Micron molybdenum disulfide hydrogen evolution electro-catalytic material, preparation method and application of micron molybdenum disulfide hydrogen evolution electro-catalytic material
  • Micron molybdenum disulfide hydrogen evolution electro-catalytic material, preparation method and application of micron molybdenum disulfide hydrogen evolution electro-catalytic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 0.31g (0.00025mol) ammonium heptamolybdate tetrahydrate into 10.0mL N,N'-dimethylformamide to prepare a 0.025mol / L solution, then add 0.57g (0.0075mol) thiourea, use Stir with a magnetic stirrer (500r / min) for 30min, transfer the stirred solution to a hydrothermal reaction kettle with a volume of 30mL, conduct a hydrothermal reaction at 220°C for 24h, then cool naturally, centrifuge, and deionize in turn After washing with water and ethanol and drying, 0.42 g of molybdenum disulfide microsheet hydrogen evolution electrocatalyst was obtained. From figure 2 It can be seen that the product is a microsheet structure.

[0032] The test was performed on an electrochemical workstation (Gamry Reference 600 Instruments, USA) using a three-electrode system. Disperse 5.0 mg of molybdenum disulfide prepared in this example as a catalyst and 20.0 μL Nafion (5wt%) solution in an ethanol-water mixed solution (volume ratio of ethanol: water is 1:1), and ultrasonically treat...

Embodiment 2

[0034] Dissolve 0.31g (0.00025mol) ammonium heptamolybdate tetrahydrate into 10mL N,N'-dimethylformamide / deionized water (volume ratio = 1:1) mixed solution to prepare a 0.025mol / L solution , then add 0.57g (0.0075mol) thiourea, stir with a magnetic stirrer for 30min (stirring speed 1000r / min), transfer the stirred solution to a hydrothermal reaction kettle with a volume of 30mL, and carry out hydrothermal reaction at 220°C. Thermal reaction for 24h, then natural cooling, drying after centrifugation, deionized water and ethanol washing to obtain 0.37g molybdenum disulfide micro-sheets, from image 3 As can be seen, the product is a microsheet structure, but agglomeration is beginning to occur.

[0035] The test was performed on an electrochemical workstation (Gamry Reference 600 Instruments, USA) using a three-electrode system. Disperse 5.0 mg of molybdenum disulfide prepared in this example as a catalyst and 20.0 μL Nafion (5wt%) solution in an ethanol-water mixed solution (...

Embodiment 3

[0037] Dissolve 0.62g (0.0005mol) ammonium heptamolybdate tetrahydrate into 10mL N,N'-dimethylformamide / deionized water (volume ratio = 1:1) mixed solution to prepare a 0.05mol / L solution , add 1.14g (0.015mol) thiourea again, utilize magnetic stirrer to stir 30min (stirring speed 1000r / min), the solution after stirring is transferred to the hydrothermal reaction kettle that volume is 30mL, carry out water under the condition of 220 ℃ Thermal reaction for 24h, then natural cooling, drying after centrifugation, deionized water and ethanol washing to obtain 0.68g molybdenum disulfide micro-sheets, from Figure 4 It can be seen that the product agglomeration phenomenon is serious.

[0038] The test was performed on an electrochemical workstation (Gamry Reference 600 Instruments, USA) using a three-electrode system. Disperse 5.0 mg of molybdenum disulfide prepared in this example as a catalyst and 20.0 μL of Nafion (5wt%) solution in an ethanol-water mixed solution (volume ratio ...

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Abstract

The invention discloses a micron molybdenum disulfide hydrogen evolution electro-catalytic material, a preparation method and an application of the micron molybdenum disulfide hydrogen evolution electro-catalytic material in hydrogen evolution electro-catalysis, and belongs to the technical field of catalytic materials. The preparation method comprises the following steps of dissolving ammonium molybdate tetrahydrate (H24Mo7N6O24 4H2O) in a solvent so as to prepare a 0.025-0.05 mol / L of solution; adding thiocarbamide (CH4N2S), wherein the molar ratio of the ammonium molybdate tetrahydrate to the thiocarbamide 1:30 to 1:40; stirring to mix the solution evenly; performing hydrothermal reaction; reducing the temperature to room temperature after the hydrothermal reaction is completed; centrifuging, washing and drying to obtain the micron-grade molybdenum disulfide hydrogen evolution electro-catalytic material. The preparation method disclosed by the invention is low in cost, simple and easily controlled in production process, high in yield, and suitable for industrial production; and the prepared micron sheets are uniform in shape.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials, in particular to a micron molybdenum disulfide (MoS 2 ) Hydrogen evolution electrocatalysis material, preparation method and application in hydrogen evolution electrocatalysis. Background technique [0002] As a transition metal disulfide, molybdenum disulfide semiconductor material with layered structure has good optical, electrical, lubricating, catalytic and other properties. The atomic bonding valences of the inner and edge of the layered molybdenum disulfide microsheets are different. The inner atoms are saturated, while the edge atoms are unsaturated, forming dangling bonds, that is, the edge active site Mo-S facets. The more Mo-S facets, the catalytic performance will have the advantages of large specific surface area, strong adsorption capacity, and high reactivity (Wei Ronghui, preparation of nano-molybdenum disulfide and research on its physical and chemical properties [D]....

Claims

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Application Information

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IPC IPC(8): B01J27/051C25B1/02C25B11/06
CPCC25B1/02C25B11/04B01J27/051
Inventor 戴昉纳林欢范卫东袁雪肖振宇董斌张亮亮
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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