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Preparation method of vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electro-catalytic material

An electrocatalytic material, graphene technology, applied in the field of material chemistry, can solve the problems of limited commercial application, high cost, and scarce content

Active Publication Date: 2020-05-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, their commercial applications in electrolyzed water are severely limited due to their high cost, rare content, and poor stability.

Method used

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  • Preparation method of vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electro-catalytic material
  • Preparation method of vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electro-catalytic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Preparation of nitrogen-sulfur double-doped reduced graphene oxide:

[0022] (a) 100 mg of graphene oxide and 1.0 g of L-cysteine ​​were placed in a mortar and ground for 30 min;

[0023] (b) The mixture obtained in (a) was placed in a tube furnace, heated to 600°C in a nitrogen atmosphere, kept for 2 hours, then cooled to room temperature with the furnace, washed and dried to obtain nitrogen-sulfur double-doped reduced graphene oxide.

[0024] (2) Preparation of NiV-LDH / NSG:

[0025] (a) Disperse 30 mg of nitrogen-sulfur double-doped reduced graphene oxide obtained by ultrasonication for 5 h in 60 mL of deionized water, and add 0.900 mmol of NiCl 2 , 0.100mmol VCl 3 , 10mmol urea and 5mmol NH 4 F Stir to a homogeneously mixed solution;

[0026] (b) Transfer the solution in (a) to the reaction kettle, then react at 120°C for 16h, centrifuge to obtain the precipitate, wash it with absolute ethanol and dry it at 60°C to obtain the precursor material NiV-LDH / NSG;...

Embodiment 2

[0031] (1) Preparation of nitrogen-sulfur double-doped reduced graphene oxide:

[0032] (a) 100 mg of graphene oxide and 0.5 g of L-cysteine ​​were placed in a mortar and ground for 30 min;

[0033] (b) The mixture obtained in (a) was placed in a tube furnace, heated to 700° C. in a nitrogen atmosphere, kept for 1 h, then cooled to room temperature with the furnace, and then washed and dried to obtain nitrogen-sulfur double-doped reduced graphene oxide.

[0034] (2) Preparation of NiV-LDH / NSG:

[0035] (a) Disperse 30 mg of nitrogen-sulfur double-doped reduced graphene oxide in 40 mL of deionized water by ultrasonication for 5 h, and add 0.833 mmol of NiCl 2 , 0.166mmol VCl 3 , 10mmol urea and 5mmol NH 4 F Stir to a homogeneously mixed solution;

[0036] (b) Transfer the solution in (a) to the reaction kettle, then react at 120°C for 16h, centrifuge to obtain the precipitate, wash it with absolute ethanol and dry it at 60°C to obtain the precursor material NiV-LDH / NSG; ...

Embodiment 3

[0041](1) Preparation of nitrogen-sulfur double-doped reduced graphene oxide:

[0042] (a) 100 mg of graphene oxide and 1.5 g of L-cysteine ​​were placed in a mortar and ground for 30 min;

[0043] (b) The mixture obtained in (a) was placed in a tube furnace, heated to 800°C in a nitrogen atmosphere, kept for 4 hours, then cooled to room temperature with the furnace, washed and dried to obtain nitrogen-sulfur double-doped reduced graphene oxide.

[0044] (2) Preparation of NiV-LDH / NSG:

[0045] (a) Disperse 30 mg of nitrogen-sulfur double-doped reduced graphene oxide obtained by ultrasonication for 5 h in 30 mL of deionized water, and add 0.750 mmol of NiCl 2 , 0.250mmol VCl 3 , 10mmol urea and 5mmol NH 4 F Stir to a homogeneously mixed solution;

[0046] (b) Transfer the solution in (a) to the reaction kettle, then react at 120°C for 16h, centrifuge to obtain the precipitate, wash it with absolute ethanol and dry it at 60°C to obtain the precursor material NiV-LDH / NSG; ...

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Abstract

The invention discloses a preparation method of a vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electro-catalytic material. The preparation method comprises the following steps: 1) grinding graphene oxide and L-cysteine; 2) putting a mixture ground in step 1) into a tubular furnace to prepare nitrogen-sulfur double-doped reduced graphene oxide; 3) preparing a nitrogen-sulfur double-doped reduced graphene oxide solution with the concentration of 0.5-1.0 mg / mL; 4) adding urea, NH4F, vanadium chloride and a nickel salt into the nitrogen-sulfur double-doped reduced graphene oxide solution, and stirring until a uniform solution is formed; 5) transferring the solution in step 4) into a reaction kettle to prepare a precursor NiV-LDH / NSG; and (6) putting the precursor NiV-LDH / NSG material and sodium hypophosphite into a tubular furnace together, heating to 300-400 DEG C, and keeping the temperature to obtain the vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material NiVP / NSG. The preparation method is low in cost and simple, and the obtained electro-catalytic material has good OER.

Description

technical field [0001] The invention belongs to the field of material chemistry, in particular to a method for preparing a vanadium-doped nickel phosphide composite nitrogen-sulfur double-doped reduced graphene oxide electrocatalytic material. Background technique [0002] With the aggravation of the global energy crisis and environmental pollution, the development of clean and renewable energy has become a problem that has attracted much attention and needs to be solved urgently. As a clean energy, hydrogen has the characteristics of high energy density, high conversion efficiency and no pollution. It provides convenience for meeting the huge energy demand in the future, and has been extensively studied. Electrocatalytic water splitting is an effective method for hydrogen production, and the whole reaction process consists of two half-reactions: oxygen evolution reaction (OER) and hydrogen evolution reaction (HER). Since the oxygen evolution reaction is a four-electron pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/06C25B1/04B01J27/24B01J35/00B01J37/28
CPCC25B1/04B01J27/24B01J37/28C25B11/091B01J35/33Y02E60/36
Inventor 刘毅赵蓉杨梦雅王欢
Owner ZHEJIANG UNIV
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