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Iron-doped molybdenum diselenide nano material with hollow structure as well as preparation method and electro-catalytic nitrogen reduction application thereof

A technology of molybdenum diselenide and nanomaterials, which is applied in the direction of nanotechnology, nanotechnology, and nanotechnology for materials and surface science, and can solve problems such as low nitrogen reduction activity, excellent electrolytic hydrogen evolution performance, and difficult conversion , to achieve the effect of convenient operation, simple preparation method and strong nitrogen adsorption capacity

Pending Publication Date: 2021-04-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, molybdenum diselenide materials are mostly prepared by vapor phase deposition (such as: ZL2017105378640). This preparation method must be under high temperature conditions. The prepared catalyst has few surface defects, low nitrogen reduction activity and excellent hydrogen electrolysis performance. Conversion of Nitrogen to Ammonia at Atmospheric Pressure

Method used

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  • Iron-doped molybdenum diselenide nano material with hollow structure as well as preparation method and electro-catalytic nitrogen reduction application thereof
  • Iron-doped molybdenum diselenide nano material with hollow structure as well as preparation method and electro-catalytic nitrogen reduction application thereof
  • Iron-doped molybdenum diselenide nano material with hollow structure as well as preparation method and electro-catalytic nitrogen reduction application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Add 0.1mmol of selenium powder to 5mL of hydrazine hydrate and stir for 1h in an oil bath at 80°C. Stir well to form a hydrated selenium precursor; then add 0.054mmol of sodium molybdate dihydrate and 0.006mmol of Iron acetate was dispersed in 15ml of dimethylformamide (DMF) and stirred for 2h, stirred evenly to obtain a metal salt solution; then the cooled hydrated selenium precursor was added dropwise to the above metal salt solution and continued to stir 2h, stirred evenly to obtain a mixed solution; finally, the above mixed solution was transferred to a high-pressure reactor and heated at 180°C for 12h; after the reactor was naturally cooled to room temperature, the obtained product was washed with deionized water until neutral, and then heated at 80°C vacuum drying for 12 hours to obtain the iron-doped molybdenum diselenide nanomaterial with a hollow structure.

[0028] The second step: the iron-doped molybdenum diselenide nanomaterial with hollow structure...

Embodiment 2

[0032] Step 1: Add 0.125mmol of selenium powder to 5mL of hydrazine hydrate and stir for 1h in an oil bath at 80°C, and stir evenly to form a hydrated selenium precursor; then add 0.057mmol of sodium molybdate dihydrate and 0.0063mmol of Iron acetate was dispersed in 15ml of dimethylformamide (DMF) and stirred for 2h to obtain a metal salt solution; then the cooled hydrated selenium precursor was added dropwise to the above metal salt solution and continued to stir for 2h Stir evenly to obtain a mixed solution; finally, transfer the above mixed solution to a high-pressure reactor and heat it at 220°C for 18 hours; after the reactor is naturally cooled to room temperature, wash the obtained product with deionized water until it is neutral, and dry it in vacuum at 70°C 8h, obtaining the iron-doped molybdenum diselenide nanomaterial with a hollow structure.

[0033] The second step: the iron-doped molybdenum diselenide nanomaterial with hollow structure is dispersed in the mixed ...

Embodiment 3

[0037] Step 1: Add 0.15 mmol of selenium powder to 5 mL of hydrazine hydrate and stir for 1 h in an oil bath at 80°C, stirring evenly to form a hydrated selenium precursor; then add 0.063 mmol of sodium molybdate dihydrate and 0.0075 mmol of Iron acetate was dispersed in 15ml of dimethylformamide (DMF) and stirred for 2h, stirred evenly to obtain a metal salt solution; then the cooled hydrated selenium precursor was added dropwise to the above metal salt solution and continued to stir 2h, stirred evenly to obtain a mixed solution; finally, the above solution was transferred to a high-pressure reactor and heated at 200°C for 16h; after the reactor was naturally cooled to room temperature, the obtained product was washed with deionized water to neutrality, and vacuumed at 75°C After drying for 6 hours, the iron-doped molybdenum diselenide nanomaterial with a hollow structure was obtained.

[0038] The second step: the iron-doped molybdenum diselenide nanomaterial with hollow str...

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Abstract

The invention discloses an iron-doped molybdenum diselenide nano material with a hollow structure as well as a preparation method and electrocatalytic nitrogen reduction application thereof. The method comprises the following steps: dissolving selenium powder in hydrazine hydrate; dissolving molybdenum salt and iron salt in DMF to obtain a metal salt solution; and adding the hydrated selenium precursor solution into the metal salt solution, heating to carry out a solvothermal reaction, washing and drying to obtain the material. The iron-doped molybdenum diselenide material is a hollow material with a porous structure. Iron-doped molybdenum diselenide is dispersed in ethanol and then is dispensed on carbon cloth to prepare an electrode.The iron-doped molybdenum diselenide material provided by the invention can be applied to an electro-catalytic nitrogen reduction reaction at normal temperature and normal pressure. The catalyst has the advantages of simple preparation method, large specific surface area, high catalytic activity, excellent stability and the like.

Description

technical field [0001] The invention belongs to the field of electrocatalytic nitrogen reduction catalysts, and specifically relates to an iron-doped molybdenum diselenide nanometer material with a hollow structure, a preparation method thereof and an application of electrocatalytic nitrogen reduction. Background technique [0002] Ammonia is an important chemical raw material and plays an important role in modern industry and agriculture. At the same time, due to its high hydrogen density and easy liquefaction characteristics, it is also considered as a potential hydrogen carrier. The traditional Haber process for ammonia synthesis consumes a lot of energy, which accounts for about 2% of the total global energy consumption. At the same time, the high temperature and high pressure environment also requires high equipment investment. Therefore, it is of great significance to develop a new method for synthesizing ammonia. [0003] Electrocatalytic nitrogen reduction (NRR) is...

Claims

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Application Information

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IPC IPC(8): C25B1/27C25B11/091B82Y30/00B82Y40/00
Inventor 丁良鑫滕浩郭浩罗荻
Owner SOUTH CHINA UNIV OF TECH
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