Synthesis method of vanadium-modified Ni3S2 electrocatalyst automatically assembled from rodlike shape into ball-flower shape

An electrocatalyst, flower ball-shaped technology, applied in the field of new energy material preparation, can solve the problems of complex operation steps, large material overpotential, harsh reaction conditions, etc., and achieve the effects of wide source of raw materials, increased specific surface area, and low synthesis temperature

Active Publication Date: 2018-07-27
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] China Invention Announcement Patent No. 201610552386.6 discloses a lithium-ion battery negative electrode GO-PANT-Ni 3 S 2 The preparation method of composite materials, but the operation steps are complicated, and the reaction cycle is long, and the technology is difficult
China Invention Announcement Patent No. 201610252105.5 discloses an array-type nickel disulfide-carbon nanotube composite electrode and its preparation method and application. Firstly, a hydrothermal reaction is carried out, followed by heat treatment to obtain an array-type nickel disulfide Nickel-carbon nanotube composite electrode material, long reaction cycle, harsh reaction conditions, and high cost
China Invention Announcement Patent No. 201310320738.1 discloses a composite catalytic electrode for electrolyzing water to produce oxygen and its preparation method. The rod-shaped Ni(OH) electrode is prepared by hydrothermal method. 2 / Ni 3 S 2 Composite electrode, but the overpotential of the material is large, it cannot be used under high current conditions, and the catalytic activity is poor

Method used

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  • Synthesis method of vanadium-modified Ni3S2 electrocatalyst automatically assembled from rodlike shape into ball-flower shape
  • Synthesis method of vanadium-modified Ni3S2 electrocatalyst automatically assembled from rodlike shape into ball-flower shape
  • Synthesis method of vanadium-modified Ni3S2 electrocatalyst automatically assembled from rodlike shape into ball-flower shape

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Soak nickel foam (2×5) cm in acetone and hydrochloric acid for 5 min, and then wash it alternately with ethanol and deionized water for 3 times, respectively. The concentration of hydrochloric acid is 0.5 mol / L. After vacuum drying for 3 h, the treated foamed nickel was obtained;

[0031] (2) Select vanadium pentoxide and thiourea as raw materials, take vanadyl acetylacetonate as 0.075 mmol, control the molar ratio of vanadium source and sulfur source to 1:0.5, and add it to 15 ml of absolute ethanol at the same time, at room temperature Stir magnetically for 3 min to obtain suspension A;

[0032] (3) Place the stirred suspension A and the metal nickel treated in step (1) in a microwave reactor, and conduct a solvothermal reaction at a temperature of 60 °C and a power of 200 W for 30 min.

[0033] (4) After the reaction was completed and cooled, the product was washed alternately with deionized water and ethanol for 3 times, and then vacuum-dried at 10 °C for 3 hou...

Embodiment 2

[0035] (1) Soak nickel foam (2 × 5) cm in acetone and hydrochloric acid for 5 min, then rinse with ethanol and deionized water alternately for 3 times, the concentration of hydrochloric acid is 1 mol / L, and then rinse at 10 °C After vacuum drying for 5 h, the treated foamed nickel was obtained;

[0036] (2) Select vanadium pentoxide and thioacetamide as raw materials, take vanadyl acetylacetonate as 0.15 mmol, control the molar ratio of vanadium source and sulfur source to 1:1, add it to 15 ml of absolute ethanol at the same time, and Magnetic stirring at room temperature for 5 min to obtain suspension A;

[0037] (3) Place the stirred suspension A and the metal nickel treated in step (1) in a microwave reactor, and conduct a solvothermal reaction at a temperature of 80 °C and a power of 200 W for 60 min.

[0038] (4) After the reaction was completed and cooled, the product was washed alternately with deionized water and ethanol three times, and then dried in vacuum at 20 °C ...

Embodiment 3

[0042] (1) Soak nickel foam (2×5) cm in acetone and hydrochloric acid for 10 min, then rinse with ethanol and deionized water alternately for 3 times, the concentration of hydrochloric acid is 2 mol / L, and then rinse at 20 °C After drying under vacuum for 10 h, the nickel foam after treatment was obtained;

[0043] (2) Select sodium metavanadate and sulfur as raw materials, take vanadyl acetylacetonate as 0.3 mmol, control the molar ratio of vanadium source and sulfur source to 1:4, and add it to 15 ml of absolute ethanol at the same time, at room temperature Magnetic stirring was carried out for 10 min to obtain suspension A;

[0044] (3) Place the stirred suspension A and the metal nickel treated in step (1) in a microwave reactor, and conduct a solvothermal reaction at a temperature of 100°C and a power of 300 W for 90 min.

[0045] (4) After the reaction was completed and cooled, the product was washed alternately with deionized water and ethanol for 3 times, and then vac...

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Abstract

The invention discloses a synthesis method of vanadium-modified Ni3S2 electrocatalyst automatically assembled from a rodlike shape into a ball-flower shape. The synthesis method comprises the following steps that clean foamed nickel is dipped into turbid liquid with the vanadium source concentration being 5-30 mM and the mole ratio of a vanadium source to a sulfur source being (1) to (0.5-12), a microwave solvent thermal reaction is conducted, and after the sufficient reaction is completed, the vanadium-modified Ni3S2 electrocatalyst material automatically assembled from the rodlike shape intothe ball-flower shape is obtained. The method is easy to operate, the reaction condition is mild, the consumed time is short, the prepared vanadium modified Ni3S2 product automatically assembled fromthe rodlike shape into the ball-flower shape is high in purity, and uniform in shape and size. In order to achieve the above purpose, the following technical scheme is adopted.

Description

technical field [0001] The invention belongs to the field of preparation of new energy materials, and in particular relates to a vanadium-modified Ni with rod-shaped self-assembly into flower balls 3 S 2 Synthesis of electrocatalysts. Background technique [0002] Electrocatalytic water splitting technology is an emerging technology in the field of energy and environment. Substances such as carbides, phosphides, and sulfides have excellent electrocatalytic properties and have attracted widespread attention. Among them, WS 2 、MoS 2 As a representative substance, it has excellent electrocatalytic hydrogen production activity. But at present, water oxidation, as the rate-controlling step in the water splitting process, still restricts the whole process of water splitting. At present, most oxygen-producing electrocatalysts still have high overpotential and high cost, which limits their large-scale application. Ni 3 S 2 The material has intrinsic metallic properties due to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043C25B11/06C25B1/04
CPCB01J27/043C25B1/04C25B11/04Y02E60/36
Inventor 曹丽云杨丹冯亮亮黄剑锋刘倩倩张宁何丹阳
Owner SHAANXI UNIV OF SCI & TECH
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