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
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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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