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A kind of highly active molybdenum sulfide thin film electrocatalyst and preparation method thereof

An electrocatalyst and molybdenum sulfide technology, applied in the field of materials, can solve the problems of harsh preparation conditions, long reaction time, complex preparation process, etc., and achieve the effects of wide controllable size range, uniform and regular morphology, and simple reaction conditions.

Inactive Publication Date: 2018-01-19
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Molybdenum sulfide, as one of the materials with abundant reserves on the earth, is low in cost and has certain electrocatalytic activity. It is considered to have great potential to replace platinum-based noble metals for catalytic hydrogen production, but the semiconducting nature and two-dimensional layered structure of molybdenum sulfide limit the The improvement of its catalytic activity
[0003] So far, the synthesis of molybdenum sulfide is mainly based on high-temperature impregnation calcination and hydrothermal synthesis technology, but the obtained product is a two-dimensional material similar to graphene, and the prepared molybdenum sulfide is prone to agglomeration and particle growth. The molybdenum sulfide edge of the catalytic active site is usually covered, which seriously affects the improvement of its catalytic performance
In addition, whether it is high-temperature calcination or hydrothermal synthesis, relatively harsh reaction conditions need to be designed, the reaction time is long, and the preparation steps are complicated.
[0004] Although there are also patent reports on the preparation of molybdenum sulfide by electrochemical reduction, such as the Chinese patent "Method for preparing molybdenum disulfide nanoparticles by electrochemical reduction method", publication number CN 1986893A, the target product is still molybdenum sulfide particles, which are very easy to agglomerate. Cannot be applied to efficient electrocatalytic water splitting reaction
Chinese patent "a preparation method of molybdenum disulfide thin film material", publication number CN 103205724A, its preparation process is also relatively complicated, it is not a thin film material, and it is difficult to carry out large-scale industrial production
Chinese patent "Organic solar cell with MoO3 / MoS2 composite thin film as anode interface layer and its preparation method", application number 201310107834.8, although the thin film molybdenum oxide / molybdenum sulfide composite material was prepared, the preparation conditions were harsh and the steps were complicated
The shortcomings and shortcomings of the above-mentioned preparation methods limit the improvement of the catalytic performance of molybdenum sulfide thin film materials and large-scale industrial production
However, at room temperature, the method of synthesizing molybdenum sulfide thin film materials with similar platinum-based catalyst activity by using electrodeposition technology and liquid crystal template system has not been reported so far.

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  • A kind of highly active molybdenum sulfide thin film electrocatalyst and preparation method thereof
  • A kind of highly active molybdenum sulfide thin film electrocatalyst and preparation method thereof
  • A kind of highly active molybdenum sulfide thin film electrocatalyst and preparation method thereof

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Embodiment 1

[0029] The synthesis method of the molybdenum sulfide thin film material on the electrodeposited conductive glass substrate in the water system is as follows: at room temperature, ammonium molybdate is dissolved in 20ml water to make its concentration 0.02M, and ammonia water is added to adjust its pH to 9-10, while stirring Ammonium thioacetamide was added to make the concentration 0.05M, stirred for 30 minutes, and nitrogen gas was passed through during the process to remove oxygen in the aqueous solution. Electrodeposition was carried out by cyclic voltammetry, the scanning potential ranged from -0.2V to (-1.5V), the scanning speed was 100mV s-1, and the number of deposition cycles was 50. The obtained samples were washed with water and washed with ethanol three times each, and dried in vacuum at 60° C. for 12 hours. The sample was characterized by SEM. As shown in the figure, it can be seen that the obtained film has a smooth planar structure and the sample is pure. The o...

Embodiment 2

[0031] Synthesis of electrodeposited molybdenum sulfide film material on conductive glass substrate in liquid crystal template system: at room temperature, ammonium molybdate was dissolved in 20ml water to make the concentration 0.02M, adding ammonia water to adjust its pH to 9-10, adding sulfur while stirring Substitute acetyl ammonium to make the concentration 0.05M, add the aqueous solution of surfactant Brij56 during the stirring process, and keep stirring until a homogeneous stable solution system is obtained, and nitrogen gas is introduced during the process to remove oxygen in the aqueous solution. Electrodeposition was carried out by cyclic voltammetry, the scanning potential ranged from -0.5V to (-1.8V), the scanning speed was 50mV s-1, and the number of deposition cycles was 20. The obtained samples were washed with water and washed with ethanol three times each, and dried in vacuum at 60° C. for 12 hours. The sample is characterized by SEM, as shown in the figure, i...

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Abstract

The invention relates to a simple, efficient, green and highly catalytically active molybdenum sulfide thin film electrocatalyst based on a conductive substrate and a preparation method thereof. The pH is adjusted by forming an aqueous solution of molybdate or thiomolybdate and ammonium thioacetate at room temperature. value, adding a surfactant under stirring to form a stable liquid crystal template system, depositing a molybdenum sulfide film on a conductive substrate by electrodeposition technology, washing the obtained material with water, ethanol, and vacuum drying to finally obtain a black film material. The concentration adjustment of reactants, pH adjustment, and the change of the range of precipitation potential and the number of deposition cycles can control the size of the product and prepare molybdenum sulfide thin film materials with high purity, which is important for the controllable synthesis of molybdenum sulfide thin film materials and their applications at room temperature. significance.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to a high-activity molybdenum sulfide thin-film electrocatalyst and a preparation method thereof. Background technique [0002] Hydrogen energy is one of the most promising clean energy sources in the future. Large-scale clean hydrogen production technology requires highly active electrocatalysts to reduce overpotential and production costs. At present, the most efficient hydrogen production catalysts are platinum-based noble metal catalysts, which are expensive And limited reserves greatly limit its industrial application. Therefore, the development of low-cost, high-activity alternative catalysts has become a worldwide research hotspot. Molybdenum sulfide, as one of the materials with abundant reserves on the earth, is low in cost and has certain electrocatalytic activity. It is considered to have great potential to replace platinum-based noble metals for catalytic hydrogen produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D9/04B01J27/047C01G39/06
CPCB01J27/047B01J35/0033C01G39/06C25D9/04
Inventor 董斌韩冠群胡文慧刘艳茹柴永明刘晨光
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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