Synthetic method of Ni3S2 microrod array

A synthesis method and micro-rod technology, applied in nanotechnology, nanotechnology, electrode shape/type, etc., can solve the problems of harsh reaction conditions, large hydrogen evolution overpotential, complicated operation steps, etc., and achieve low synthesis temperature and uniform chemical composition. , the effect of cheap and easy-to-obtain raw materials

Inactive Publication Date: 2017-11-07
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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. 201510657154.2 discloses a flower-shaped Ni 3 S 2 /The preparation of graphene three-dimensional composite electrode material, first react with hydrothermal method, and then adopt the method

Method used

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  • Synthetic method of Ni3S2 microrod array
  • Synthetic method of Ni3S2 microrod array
  • Synthetic method of Ni3S2 microrod array

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) Soak nickel foam (1×5) cm in acetone solution for 5 minutes, then immerse nickel foam in 2 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;

[0031] (2) Weigh sodium dodecahydrate vanadate and sodium sulfide, take sodium dodecahydrate vanadate as 0.2 mmol, control the molar ratio of vanadium source and sulfur source to 1:1, add it into 20 ml deionized water at the same time, Stir magnetically at room temperature for 3 min to obtain a homogeneous solution A;

[0032] (3) Pour the stirred solution A into a hydrothermal kettle with a polytetrafluoroethylene liner, put the nickel foam treated in step (1) into the polytetrafluoroethylene liner, seal it, and place In a homogeneous reactor, the reaction was carried out at 70°C for a reaction time of 6 h;

[0033] (4) After the reaction, the reactor was cooled at room temperature, and the product ...

Embodiment 2

[0035] (1) Sonicate (1×5) cm nickel foam in acetone solution for 10 minutes, then immerse foam nickel in 3 mol / L hydrochloric acid for 15 minutes, and finally use ethanol and deionized water alternately Rinse 4 times and vacuum dry at 20 °C for 10 h to obtain the treated nickel foam;

[0036] (2) Take sodium vanadate and sodium diethylthiocarbamate, the sodium vanadate is 0.4 mmol, the molar ratio of vanadium source and sulfur source is 1:4, add it to 20 ml ethanol at the same time, and control it under magnetic stirring at room temperature 15 min to obtain a homogeneous solution A;

[0037] (3) Pour the stirred solution A into a hydrothermal kettle with a polytetrafluoroethylene liner, put the nickel foam treated in step (1) into the polytetrafluoroethylene liner, seal it, and place In a homogeneous reactor, the reaction was carried out at 90 °C for a reaction time of 10 h;

[0038](4) After the reaction, the reactor was cooled at room temperature, and the product was alter...

Embodiment 3

[0040] (1) Sonicate (1×5) cm nickel foam in acetone solution for 10 minutes, then immerse foam nickel in 3 mol / L hydrochloric acid for 15 minutes, and finally use ethanol and deionized water alternately Rinse 4 times and vacuum dry at 25 °C for 10 h to obtain the treated nickel foam;

[0041] (2) Take ammonium metavanadate and sulfur element, the ammonium metavanadate is 0.8mmol, control the molar ratio of vanadium source and sulfur source to 1:6, add it to 20 ml of methanol solvent at the same time, stir magnetically at room temperature for 15 min to get a homogeneous solution A;

[0042] (3) Pour the stirred solution A into a hydrothermal kettle with a polytetrafluoroethylene liner, put the nickel foam treated in step (1) into the polytetrafluoroethylene liner, seal it, and place In a homogeneous reactor, the reaction was carried out at 120 °C for a reaction time of 24 h;

[0043] (4) After the reaction, the reactor was cooled at room temperature, and the product was alter...

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Abstract

The invention discloses a synthetic method of Ni3S2 microrod array. The synthetic method comprises following steps: 1, nickel foam to be treated is subjected to full ultrasonic cleaning and drying; 2, a vanadium source and a sulfur are dissolved in an appropriate amount of a solvent at a molar ratio of 1: (1-11), and full stirring is carried out so as to obtain a solution A, wherein the concentration of the vanadium source in the solution A is controlled to be 10 to 40mM; 3, the solution A is delivered into a hydrothermal reactor with a polytetrafluoroethylene lining, the nickel foam obtained via pretreatment in step 1 is immersed in the solution A, the hydrothermal reactor is sealed, and solvothermal reaction is carried out at 70 to 200 DEG C for 6 to 30h; and 4, after reaction, the hydrothermal reactor is cooled at room temperature, and an obtained product is washed fully and dried so as to obtain the Ni3S2 microrod array. Operation of the synthetic method is simple; reaction conditions are mild; reaction period is short; the purity of prepared Ni3S2 is high; the morphology is uniform; and excellent electrocatalytic hydrogen evolution performance is achieved.

Description

technical field [0001] The invention belongs to the technical field of surface treatment of electrode materials, in particular to a Ni 3 S 2 Synthesis of microrod arrays. Background technique [0002] With the massive consumption of non-renewable energy such as coal, oil, and natural gas, people will face a serious energy crisis in the future. The search for a clean, safe and renewable energy has become a current research hotspot. As an ideal energy carrier, hydrogen energy has high hopes for it. Electrocatalytic water splitting technology is one of the effective ways to produce hydrogen. The core issue of this technology is to develop efficient and cheap water splitting catalysts. At present, noble metal-based catalysts (such as Pt, Ru, or Ir, etc.) are the best catalysts for water splitting, but the disadvantages of high price and low reserves greatly limit the wide application of such catalysts. [0003] Transition metal sulfides, with the advantages of abundant cont...

Claims

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Application Information

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IPC IPC(8): C01G53/11C25B1/04C25B11/02C25B11/04B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G53/11C01P2002/72C01P2004/03C01P2004/16C01P2004/20C01P2004/51C01P2004/64C01P2006/40C25B1/04C25B11/02C25B11/04Y02E60/36
Inventor 曹丽云杨丹冯亮亮黄剑锋吴建鹏刘倩倩张宁何元元
Owner SHAANXI UNIV OF SCI & TECH
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