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Preparation method and electrocatalytic nitrogen reduction application of ultrathin nanosheet vanadium-doped nickel sulfide nanopowder

A nano-powder and nano-flaky technology, which is applied in the preparation of inorganic nano-powder and the application field of electrocatalytic nitrogen reduction, can solve the problems that cannot eliminate the strong competition reaction

Inactive Publication Date: 2019-08-16
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Sun Xuping's research group reported that density functional calculation (DFT) and experimental results have confirmed that molybdenum disulfide can be used as an excellent electrocatalytic nitrogen reduction catalyst for 0.1 M Na 2 SO 4 In the electrolyte, however, the high HER activity of molybdenum disulfide itself inhibits the further improvement of its electrocatalytic nitrogen reduction catalytic activity.
The electrocatalytic nitrogen reduction process has encountered a bottleneck in the further exploration and development of catalysts due to the irreversible strong competitive reaction (HER).

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. Take 40 mL of deionized water and add it to a 50 mL polytetrafluoroethylene liner, add sodium carbonate (0.0050 g, 0.048 mmol) and urea (0.0721 g, 1.2 mmol) in sequence and stir for 30 min to form a colorless transparent solution, then continue stirring Next, sodium pyrovanadate (0.0489 g, 0.16 mmol) and nickel acetylacetonate (0.0822 g, 0.32 mmol) were added in sequence, stirred for 1 h and transferred to a polytetrafluoroethylene liner until fully dissolved. After sealing the hydrothermal autoclave, it was placed in an oven at 130 °C for 32 h. After natural cooling, deionized water and absolute ethanol are used to centrifugally wash and vacuum-dry respectively to obtain vanadium-nickel precursor nanopowder.

[0024] Step 2: Take 40 mL of absolute ethanol in a 50 mL polytetrafluoroethylene liner, add 50...

Embodiment 2

[0036] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. Take 40 mL of deionized water and add it to a 50 mL polytetrafluoroethylene liner, add sodium carbonate (0.0021 g, 0.02 mmol) and urea (0.0721 g, 1.2 mmol) in sequence and stir for 30 min to form a colorless and transparent solution, then continue stirring Next, ammonium metavanadate (0.0187 g, 0.16 mmol) and nickel chloride hexahydrate (0.5705 g, 2.4 mmol) were added in turn, stirred for 1 h until they were fully dissolved, and then transferred to a polytetrafluoroethylene liner. After sealing the hydrothermal autoclave, it was kept in an oven at 140 °C for 26 h. After natural cooling, deionized water and absolute ethanol are used to centrifugally wash and vacuum-dry respectively to obtain vanadium-nickel precursor nanopowder.

[0037] Step 2: Take 40 mL of absolute ethanol in a 50 mL polytetrafluoroeth...

Embodiment 3

[0049] Step 1: Take a 50 mL hydrothermal reaction kettle for laboratory use. The hydrothermal reaction kettle has a stainless steel shell and a polytetrafluoroethylene liner. Take 40 mL of deionized water and add it to a 50 mL polytetrafluoroethylene liner, add sodium carbonate (0.0021 g, 0.02 mmol) and urea (0.0721 g, 1.2 mmol) in sequence and stir for 30 min to form a colorless and transparent solution, then continue stirring Potassium metavanadate (0.0331 g, 0.24 mmol) and nickel nitrate hexahydrate (1.0468 g, 3.6 mmol) were added in turn, stirred for 1 h until they were fully dissolved, and then transferred to a polytetrafluoroethylene liner. After sealing the hydrothermal autoclave, it was kept in an oven at 150 °C for 20 h. After natural cooling, deionized water and absolute ethanol are used to centrifugally wash and vacuum-dry respectively to obtain vanadium-nickel precursor nanopowder.

[0050] Step 2: Take 40 mL of absolute ethanol in a 50 mL polytetrafluoroethylene ...

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Abstract

The invention provides a preparation method and an electrocatalytic nitrogen reduction application of an ultrathin nanosheet vanadium-doped nickel sulfide nanopowder. The preparation method comprisesthe following steps: a vanadium source and a nickel source are added to a reaction solution to prepare a pre-reaction solution, the pre-reaction solution is heated and reacted for a certain period oftime, and then is cooled, and the obtained reaction product is washed, centrifuged, vacuum-dried and collected to obtain a vanadium-nickel precursor nanopowder; the vanadium-nickel precursor nanopowder is subjected to a vulcanization reaction through a solvothermal process to obtain a vanadium-doped nickel sulfide intermediate nanopowder; and the vanadium-doped nickel sulfide intermediate nanopowder is placed in a tubular furnace, and is annealed under the protection of an inert gas to obtain the ultrathin nanosheet vanadium-doped nickel sulfide nanopowder. The ultrathin vanadium-doped nickelsulfide has an excellent catalytic property in the field of electrocatalytic nitrogen reduction (NRR), the ammonia yield at -0.2 V (relative to a standard hydrogen electrode) is as high as 63.2 [mu]gh<-1> mg <-1> cat, and the Faraday's efficiency reaches 8.3%.

Description

technical field [0001] The present invention relates to the preparation of inorganic nanopowders and the application field of electrocatalytic nitrogen reduction, in particular to a method for preparing ultrathin nanosheet vanadium-doped nickel sulfide nanopowder based on a hydrothermal method and its application in the field of electrocatalytic nitrogen reduction application. Background technique [0002] With the rapid growth of the world's population today, the demand for chemical fertilizers is increasing worldwide. In addition, currently available energy is mainly fossil fuels. The limitation of fossil fuels and environmental pollution make the further development of human beings face major problems. Therefore, the development of clean, efficient, and recyclable new energy sources and energy storage materials has attracted much attention. Ammonia, as an efficient and non-polluting energy carrier and the main raw material for the production of chemical fertilizers, its...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043C25B1/00C25B11/06C25B11/12
CPCB01J27/043C25B1/00C25B11/075C25B11/051B01J35/33
Inventor 孙旭郭成英高令峰马晓晶李石晶于笑妍阴世新魏琴
Owner UNIV OF JINAN
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