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Vanadium-modified Ni3S2 nano-rod array electrode material and preparation method thereof

A nanorod array, electrode material technology, applied in electrodes, chemical instruments and methods, electrolysis process, etc., can solve the problems of harsh reaction conditions, large material overpotential, poor catalytic activity, etc., and achieves short reaction period and simple preparation process. , The effect of stable product quality

Inactive Publication Date: 2019-01-25
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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
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
[0005] Due to its variable valence state, vanadium is widely used in the preparation of sodium ion batteries and catalytic materials, and the combination of vanadium-based materials and Ni 3 S 2 There are few studies on material composites, so a vanadium-modified Ni with low cost, high catalytic activity and simple preparation process is studied. 3 S 2 Electrode materials are of great significance

Method used

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  • Vanadium-modified Ni3S2 nano-rod array electrode material and preparation method thereof
  • Vanadium-modified Ni3S2 nano-rod array electrode material and preparation method thereof
  • Vanadium-modified Ni3S2 nano-rod array electrode material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Soak nickel foam (1×5) 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;

[0033] (2) Weigh vanadyl acetylacetonate and thiourea, take vanadyl acetylacetonate as 0.04 mmol, control the molar ratio of vanadium source and sulfur source to 1:1, add it to 20 ml ethylenediamine at the same time, and magnetically Stir for 3 min to obtain suspension A;

[0034] (3) Add 0.001 g of ammonium fluoride to suspension A and stir for 1 hour to obtain solution B;

[0035] (4) Put the stirred solution B and the metal nickel treated in step (1) into a high-pressure reactor, and then place it in an oven for reaction, and perform a solvothermal reaction at 50°C for a reaction time of 0.5 h ;

[0036] (5) After the reaction was completed, the reactor was cooled at room temperature, and the product was ...

Embodiment 2

[0039] (1) Soak nickel foam (1×5) 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 30 °C for 8 h to obtain the treated nickel foam;

[0040] (2) Weigh sodium metavanadate and thioacetamide, take sodium metavanadate as 0.06 mmol, control the molar ratio of vanadium source and sulfur source to 1:2, add it to 20 ml absolute ethanol at the same time, Under magnetic stirring for 10 min to obtain suspension A;

[0041] (3) Add 0.004 g of ammonium fluoride to suspension A and stir for 1 h to obtain solution B;

[0042] (4) Put the stirred solution B and the metal nickel treated in step (1) into a high-pressure reactor, and then place it in an oven for reaction, and perform a solvothermal reaction at 100°C for a reaction time of 5 h ;

[0043] (5) After the reaction was completed, the reactor was cooled at room temperature, and the product was was...

Embodiment 3

[0046](1) Sonicate a (1×5) cm nickel mesh in acetone for 10 minutes, then immerse the nickel mesh in 3 mol / L hydrochloric acid for 15 minutes, and finally use ethanol and deionized water alternately Rinse 3 times and vacuum dry at 40°C for 10 hours to obtain the treated foamed nickel;

[0047] (2) Weigh sodium vanadate and sodium sulfide, take sodium vanadate as 0.08 mmol, control the molar ratio of vanadium source and sulfur source to 1:3, add it to 20 ml methanol at the same time, stir magnetically at room temperature for 15 min to obtain Suspension A;

[0048] (3) Add 0.006 g of ammonium fluoride to suspension A, stir for 2 h to obtain solution B;

[0049] (4) Put the stirred solution B and the metal nickel treated in step (1) into a high-pressure reactor, and then place it in an oven for reaction, and perform a solvothermal reaction at 120°C for a reaction time of 10 h ;

[0050] (5) After the reaction was completed, the reactor was cooled at room temperature, and the p...

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Abstract

The invention provides a vanadium-modified Ni3S2 nano-rod array electrode material which has a scale-shaped surface appearance formed by self-assembling particles. A preparation method comprises the following steps: immersing metal nickel in a suspension solution containing a vanadium source, a sulfur source and ammonium fluoride, and carrying out solvothermal reaction; then, calcining a product of the solvothermal reaction to obtain the nano-rod-shaped vanadium-modified Ni3S2 electrode material. The vanadium source is vanadiumoxy acetylacetonate, sodium metavanadate, sodium vanadate, sodium vanadate dodecahydrate, ammonium metavanadate or vanadium pentoxide; the sulfur source is thiourea, thioacetamide, sodium sulfide, sodium oiethyl dithiocarbamate or a sulfur elementary substance. A nano-rod structure formed by self-assembling the particles has a secondary-grade unit so that catalytic active sites of the material are effectively increased; compared with a block-shaped catalyst, theresistance of the material is effectively reduced and the material can be used as an excellent electro-catalytic oxygen production electrocatalyst.

Description

technical field [0001] The invention belongs to the field of electrolytic water catalysis, in particular to a vanadium-modified Ni 3 S 2 Nanorod array electrode material and its preparation method. Background technique [0002] Electrocatalytic water splitting for hydrogen production is an emerging technology that satisfies people's current thirst for energy. Solve the current energy crisis and environmental pollution problems. In the process of water electrolysis, water oxidation is the rate-controlling step in the process of water splitting, which restricts the whole process of water splitting. Therefore, finding a high-efficiency water splitting oxygen-producing electrocatalyst is the core of improving the efficiency of water splitting, and has important research significance. [0003] At present, transition metal iron, cobalt, and nickel-based materials, due to their large reserves and high electrical conductivity, exhibit excellent electrocatalytic activity and have...

Claims

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Application Information

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IPC IPC(8): B01J27/043C25B1/04C25B11/06
CPCB01J27/043C25B1/04C25B11/04Y02E60/36
Inventor 曹丽云杨丹冯亮亮黄剑锋刘倩倩王琳琳
Owner SHAANXI UNIV OF SCI & TECH
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