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Preparation and electrocatalytic water decomposition application of nickel-doped Fe3O4 nano-powder

A technology of nano-powder and preparation steps, which is applied in the preparation and application of inorganic nano-powder, and the field of electrocatalytic water splitting, can solve the problems of bottleneck, poor conductivity, and poor active sites in the improvement of catalytic activity.

Inactive Publication Date: 2019-11-26
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fe 3 o 4 As a kind of transition metal oxide, its shortcomings such as poor active sites and poor conductivity make it a major challenge for electrocatalytic oxygen generation catalysts.
A large amount of research has been devoted to the regulation of Fe 3 o 4 Electronic structure to achieve the improvement of its catalytic activity, but limited by its own scarce active sites, the improvement of catalytic activity encounters a bottleneck

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Take a 50 mL hydrothermal reaction kettle, which has a stainless steel shell and a polytetrafluoroethylene liner. Take 40 mL of ethylene glycol and add it to a 50 mL beaker, add ferric nitrate nonahydrate (0.3232 g, 0.8 mmol) and nickel acetate (0.0707 g, 0.4 mmol) in turn under magnetic stirring, and stir for 10 min. In a polytetrafluoroethylene liner. After sealing the hydrothermal reactor, it was kept in an oven at 150 °C for 18 h. After natural cooling, wash with absolute ethanol for several times, and vacuum dry to obtain light blue nickel-iron precursor nanopowder.

[0022] The second step: placing the nickel-iron precursor nanopowder in a tube furnace, and performing annealing treatment under a nitrogen atmosphere. Annealing temperature is 100 o C. The time is 4 h; the nitrogen flow rate is 10 mL / min, and the heating rate is 1 o C / min, black nickel-doped Fe was obtained after cooling to room temperature 3 o 4 Nano powder.

[0023] Step 3: Ni-doped ...

Embodiment 2

[0030] The first step: take a 50 mL hydrothermal reactor, the hydrothermal reactor has a stainless steel shell and a PTFE inner tank. Take 5 mL of glycerol and 35 mL of isopropanol into a 50 mL beaker, and add ferric chloride hexahydrate (0.6487 g, 2.4 mmol) and nickel chloride hexahydrate (0.0951 g, 0.4 mmol) in turn under magnetic stirring, After stirring for 10 min, the magnetron was sucked out and transferred to a polytetrafluoroethylene liner. After sealing the hydrothermal reactor, it was placed in an oven at 190 °C for 12 h. After natural cooling, washing with anhydrous ethanol for several times, and vacuum drying to obtain a light blue nickel-iron precursor nano-powder.

[0031] The second step: placing the nickel-iron precursor nano-powder in a tube furnace and annealing in a nitrogen atmosphere. Annealing temperature is 300 o C. The time is 2 h; the nitrogen flow rate is 20 mL / min, and the heating rate is 1 o C / min, after cooling to room temperature, black nickel...

Embodiment 3

[0039] The first step: take a 50 mL hydrothermal reactor, the hydrothermal reactor has a stainless steel shell and a PTFE inner tank. Add 5 mL of glycerol and 35 mL of isopropanol into a 50 mL beaker, and add ferrous acetate (0.5566 g, 3.2 mmol) and nickel acetylacetonate (0.1028 g, 0.4 mmol) in turn under magnetic stirring, and stir for 10 min. The magneton was sucked out and transferred to a Teflon liner. After sealing the hydrothermal reactor, it was placed in an oven at 190 °C for 12 h. After natural cooling, washing with anhydrous ethanol for several times, and vacuum drying to obtain a light blue nickel-iron precursor nano-powder.

[0040] The second step: placing the nickel-iron precursor nano-powder in a tube furnace and annealing in a nitrogen atmosphere. Annealing temperature is 200 o C. The time is 3 h; the nitrogen flow rate is 20 mL / min, and the heating rate is 1 o C / min, after cooling to room temperature, black nickel-doped Fe was obtained 3 O 4 Nano powder...

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Abstract

The invention provides a preparation method and an electrocatalytic application of a nickel-doped Fe3O4 nano-powder. The preparation method comprises the following steps: adding certain proportions ofa nickel source and an iron source into a specially-made reaction solution to prepare a ferronickel pre-reaction solution, heating the pre-reaction solution for a certain time, and collecting to obtain a ferronickel precursor nano-powder; and placing the ferronickel precursor nano-powder in a tubular furnace, and carrying out annealing treatment under the protection of nitrogen to obtain the nickel-doped Fe3O4 nano-powder. The introduction of active atom nickel makes the nickel-doped Fe3O4 nano-powder have an excellent catalytic activity in the oxygen evolution reaction (OER) of water decomposition and have an overpotential of 0.293 V (relative to a standard hydrogen electrode), a Tafel slope of 43 mV / dec and a charge transfer resistance of 34 ohms.

Description

technical field [0001] The invention relates to the field of preparation and application of inorganic nanopowders, in particular to a method for preparing nickel-doped Fe based on solvothermal method. 3 o 4 The method of nanopowder and its application in the field of electrocatalytic water splitting. Background technique [0002] Fossil energy is currently the main energy source. With its rapid consumption and the accompanying environmental pollution problems, the search for clean and efficient new alternative energy sources has become the focus of research all over the world. Among them, hydrogen energy with extremely high energy density has attracted the attention of a large number of researchers. Among many hydrogen production methods, electrocatalytic water splitting for hydrogen production has the advantages of safe and controllable reaction, recyclable products, environmental protection and no pollution, making it promising to become an important process for producin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08C25B11/06C25B1/04B01J23/755B82Y30/00
CPCC01G49/08B01J23/755C25B1/04B82Y30/00C25B11/091B01J35/23B01J35/33Y02E60/36
Inventor 孙旭郭成英高令峰马晓晶赵明珠赵磊匡轩魏琴
Owner UNIV OF JINAN
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