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Synthetic method for 3D self-assembled flower-like vanadium-modified Ni3S2

A synthetic method, a curd-shaped technology, applied in chemical instruments and methods, physical/chemical process catalysts, catalyst activation/preparation, etc., can solve the problems of blank oxygen production performance, harsh reaction conditions, complicated operation steps, etc., and achieve good electrical performance. The effect of catalytic oxygen evolution activity, short reaction period and simple preparation process

Active Publication Date: 2018-09-04
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 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
Efficient Coupling of Hierarchical V 2 o 5 @Ni 3 S 2 Hybrid Nanoarray for Pseudocapacitors and HydrogenProduction and others used a two-step hydrothermal method to prepare V with a hierarchical structure 2 o 5 @Ni 3 S 2 Materials with low hydrogen production overpotential, but there is a gap in oxygen production performance, and the preparation process is complicated
[0005] Currently, combining vanadium-based materials with Ni 3 S 2 There are few reports on the combination, so this patent combines vanadium-based materials with Ni 3 S 2 The combination of materials is of great significance for the mining of efficient, cheap and simple preparation process for oxygen evolution electrocatalysts

Method used

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  • Synthetic method for 3D self-assembled flower-like vanadium-modified Ni3S2
  • Synthetic method for 3D self-assembled flower-like vanadium-modified Ni3S2
  • Synthetic method for 3D self-assembled flower-like vanadium-modified Ni3S2

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Soak nickel foam (2×5) cm in acetone for 5 minutes, then immerse nickel foam in 1 mol / L hydrochloric acid for 5 minutes, and finally use ethanol and deionized water alternately Rinse 3 times and vacuum dry at 20 °C for 5 h to obtain the treated nickel foam;

[0036] (2) Choose sodium dodecahydrate vanadate and thioacetamide as raw materials, take sodium dodecahydrate vanadate as 0.1 mmol, control the molar ratio of vanadium source and sulfur source to 1:1, and add it to 20 ml anhydrous In ethanol, stir magnetically at room temperature for 3 min to obtain suspension A;

[0037] (3) Prepare 1 mol / L hydrochloric acid solution B to adjust the Ph of suspension A;

[0038] (4) Add 1 mol / L hydrochloric acid solution dropwise to suspension A, adjust the Ph to 6, and stir for 10 min to obtain solution C;

[0039] (5) Place the stirred solution C and the nickel foam treated in step (1) in a microwave reactor, and conduct a solvothermal reaction at a temperature of 60°C and ...

Embodiment 2

[0042] (1) Soak nickel foam (2×5) cm in acetone for 5 minutes, then immerse nickel foam in 1 mol / L hydrochloric acid for 5 minutes, and finally use ethanol and deionized water alternately Rinse 3 times and vacuum dry at 20 °C for 5 h to obtain the treated nickel foam;

[0043] (2) Select sodium dodecahydrate vanadate and thiourea as raw materials, take sodium dodecahydrate vanadate as 0.3 mmol, control the molar ratio of vanadium source and sulfur source to 1:2, and add it to 20ml of absolute ethanol at the same time, Stir magnetically at room temperature for 10 min to obtain suspension A;

[0044] (3) Prepare 3 mol / L sulfuric acid solution B to adjust the Ph of suspension A;

[0045] (4) Add 3 mol / L sulfuric acid solution dropwise to suspension A, adjust the Ph to 5, and stir for 10 min to obtain solution C;

[0046] (5) Place the stirred solution C and the nickel foam treated in step (1) in a microwave reactor, and conduct a solvothermal reaction at a temperature of 80°C a...

Embodiment 3

[0049] (1) Sonicate a (2×5) cm nickel mesh in acetone for 10 minutes, then immerse foamed nickel in 3 mol / L hydrochloric acid for 10 minutes, and finally rinse with ethanol and deionized water alternately 3 times, after vacuum drying at 20°C for 5h, the treated foamed nickel was obtained;

[0050] (2) Select sodium dodecahydrate vanadate and sodium sulfide as raw materials, take 0.8 mmol of sodium dodecahydrate vanadate, control the molar ratio of vanadium source and sulfur source to 1:5, and add it to 20 ml of absolute ethanol and dehydrated In the mixed solution of ionic water, magnetically stir at room temperature for 10 min to obtain suspension A;

[0051] (3) Prepare 1 mol / L ammonia solution B to adjust the Ph of suspension A;

[0052] (4) Add 1 mol / L ammonia solution dropwise to suspension A, adjust the Ph to 8, and stir for 10 min to obtain solution C;

[0053] (5) Place the stirred solution C and the nickel foam treated in step (1) in a microwave reactor, and conduct...

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Abstract

The invention provides a synthetic method for 3D self-assembled flower-like vanadium-modified Ni3S2. The method comprises the following steps: immersing clean metal nickel into a suspension having a vanadium source concentration of 5-40 mM, a molar ratio of a vanadium source to a sulfur source of 1: (1-12), and a weakly acidic or weakly alkaline pH, and performing a microwave solvothermal reactionto obtain the 3D self-assembled flower-like vanadium-modified Ni3S2 electrocatalyst material after the reaction is fully performed. The method provided by the invention has simple operation, mild reaction conditions, short time consumption and a uniform morphology and size; and the material has a unique hierarchical structure, so that the catalytic activity of the material is increased, and the material can be used as an excellent electrocatalytic oxygen evolution electrocatalyst.

Description

technical field [0001] The invention belongs to the field of new energy materials and electrochemistry, in particular to a 3D self-assembled spherical vanadium-modified Ni 3 S 2 synthetic method. Background technique [0002] Fossil energy as primary energy, including oil, coal, and natural gas, has limited reserves in the earth's crust, making excessive exploitation and consumption lead to a predictable energy crisis. At the same time, the combustion process has caused environmental pollution and the greenhouse effect. Therefore, it is urgent to exploit alternative new energy sources to alleviate the energy crisis. Among secondary energy sources, hydrogen energy has a high combustion value per unit mass and the cleanest water as a combustion product, making it the most ideal energy carrier to replace fossil energy. Electrocatalytic water splitting technology is one of the effective ways to produce hydrogen, but the development of hydrogen production by electrolysis of wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043B01J35/00B01J35/02B01J37/08B01J37/34
CPCB01J27/043B01J37/08B01J37/346B01J35/00B01J35/30B01J35/33
Inventor 曹丽云杨丹冯亮亮黄剑锋刘倩倩徐瑞
Owner SHAANXI UNIV OF SCI & TECH
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