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Ball-flower-like V-doped Ni3S2/NF self-supporting electrode material and preparation method thereof

A self-supporting electrode, flower ball technology, applied in the direction of electrode, electrode shape/type, electrolysis process, etc., can solve the problem of few reports, and achieve the effect of strong repeatability, easy operation and high product yield

Active Publication Date: 2019-01-29
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, current studies on curdled Ni 3 S 2 few reports

Method used

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  • Ball-flower-like V-doped Ni3S2/NF self-supporting electrode material and preparation method thereof
  • Ball-flower-like V-doped Ni3S2/NF self-supporting electrode material and preparation method thereof
  • Ball-flower-like V-doped Ni3S2/NF self-supporting electrode material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Sonicate nickel foam by immersing it in acetone solution for 10 minutes, then transfer it to 2mol / L hydrochloric acid for ultrasonic cleaning for 10 minutes, and finally wash it alternately with ethanol and ultrapure water for 3 times, and then vacuum-dry it at 35°C for 10 hours;

[0017] (2) Configure a precursor solution, which contains nickel chloride hexahydrate at a concentration of 0.05mol / L, vanadium chloride at a concentration of 0.0125mol / L, ammonium fluoride at a concentration of 0.05mol / L and 0.125) mol / L aqueous solution of urea, magnetically stirred at room temperature for 20 minutes to obtain a clear solution A. Transfer the clarified solution A and the conductive substrate treated in step (1) into a high-temperature and high-pressure hydrothermal kettle, and then react at 100°C for 18 hours, and the reaction filling ratio should be controlled at 40%. After the hydrothermal reaction was completed, the reactor was naturally cooled to room temperature, a...

Embodiment 2

[0020] (1) Soak nickel foam of 1cm x 5cm in acetone solution for 10 minutes, then transfer it to 2mol / L hydrochloric acid for 10 minutes, and finally rinse it with ethanol and ultrapure water for 3 times, and then clean it at 35°C. Vacuum drying for 10h;

[0021] (2) Configure a precursor solution, which contains nickel chloride hexahydrate at a concentration of 0.1mol / L, vanadium chloride at a concentration of 0.04mol / L, ammonium fluoride at a concentration of 0.05mol / L and Aqueous solution of 0.2mol / L urea, magnetically stirred at room temperature for 20min to obtain clear solution A. Transfer the clarified solution A and the conductive substrate treated in step (1) into a high-temperature and high-pressure hydrothermal kettle, and then react at 120°C for 14 hours, and the reaction filling ratio should be controlled at 40%. After the hydrothermal reaction was completed, the reactor was naturally cooled to room temperature, and then the conductive substrate cooled after the ...

Embodiment 3

[0024] (1) Sonicate 1cm x 5cm nickel foam in acetone solution for 5 minutes, then immerse foam nickel in 2mol / L hydrochloric acid for 5 minutes, and finally rinse with ethanol and ultrapure water for 3 times respectively. After vacuum drying for 10°C, the treated foamed nickel was obtained;

[0025] (2) Configure a precursor solution, which contains nickel chloride hexahydrate at a concentration of 0.1mol / L, vanadium chloride at a concentration of 0.05mol / L, ammonium fluoride at a concentration of 0.05mol / L and Aqueous solution of 0.2mol / L urea, magnetically stirred at room temperature for 20min to obtain clear solution A. Transfer the clarified solution A and the nickel foam treated in step (1) into a high-temperature and high-pressure hydrothermal kettle, and then react at 140°C for 10 hours, and the reaction filling ratio should be controlled at 30%. After the hydrothermal reaction was completed, the reactor was naturally cooled to room temperature, and then the conductive...

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Abstract

The invention provides a preparation method of a ball-flower-like V-doped Ni3S2 / NF self-supporting electrode material. The preparation method comprises the steps of soaking cleaned foam nickel into apolymeric precursor solution containing nickel chloride hexahydrate, vanadium chloride, ammonium fluoride and urea to conduct primary hydrothermal reaction; soaking the reactive foam nickel into an aqueous solution containing thioacetamide and polyvinyl pyrrolidone to conduct secondary hydrothermal reaction to obtain the ball-flower-like V-doped Ni3S2 / NF self-supporting electrode material. The invention further discloses the ball-flower-like V-doped Ni3S2 / NF self-supporting electrode material. The preparation method provided by the invention is simple in operation, and the reaction period is short. The prepared V-doped Ni3S2 is uniform in morphology and has the self-assembly structure, and the electro-catalytic property of the material is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of electrocatalysts, in particular to a flower-shaped V-doped Ni 3 S 2 / NF self-supporting electrode material and its preparation method. Background technique [0002] Ni 3 S 2 The regulation of micro-nanomaterials has become the Ni 3 S 2 Materials research hotspots. Ni with different microscopic morphology (nanosheet, nanorod, nanowire structure, etc.) can be synthesized by hydrothermal method, microwave hydrothermal method, solvothermal method, template method, etc. 3 S 2 micro-nano materials. Patent "Zhao Hailei, Zhang Zijia, Zeng Zhipeng, etc. A nano-Ni with sheet structure 3 S 2 Preparation method of materials, CN 104201380 B[P]. 2017." Using solvothermal method, using Ni network with three-dimensional porous structure as carrier, synthesized nano-Ni with lamellar structure 3 S 2 Materials; literature "Zhou W, Wu X J, Cao X, et al. Ni 3 S 2 nanorods / Ni foam composite electrode with low o...

Claims

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Application Information

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IPC IPC(8): C25B11/06C25B11/03C25B1/04
CPCC25B1/04C25B11/031C25B11/051C25B11/075Y02E60/36
Inventor 黄剑锋刘倩倩冯亮亮曹丽云杨丹张晓
Owner SHAANXI UNIV OF SCI & TECH
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