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Preparation method for similarly coralloid NiSe@NC and application thereof

A coral-like, trimesic acid technology, applied in electrodes, electrolysis process, electrolysis components, etc., can solve the problem that the advantages of synergistic effect cannot be fully utilized, etc.

Inactive Publication Date: 2018-11-20
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the advantage of the synergistic effect between NiSe nanostructures and highly conductive nitrogen-doped porous carbon cannot be fully exploited.

Method used

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  • Preparation method for similarly coralloid NiSe@NC and application thereof
  • Preparation method for similarly coralloid NiSe@NC and application thereof
  • Preparation method for similarly coralloid NiSe@NC and application thereof

Examples

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Effect test

Embodiment 1

[0038] This embodiment relates to a preparation method similar to coral-like NiSe@NC, such as figure 1 As shown, it specifically includes the following steps:

[0039] Add 1 mmol of trimesic acid, 1 mmol of nickel nitrate hexahydrate, and 1 mmol of 4,4’-bipyridine to 20 mL of DMF in sequence, stir for half an hour, then transfer to a 10 mL vial, heat to 80°C, and react for 3 days. After waiting for the reaction system to drop to room temperature, take out the reaction vessel, wash the obtained green crystals with DMF and absolute ethanol three times, and then vacuum-dry them at 80°C for 24 hours to obtain Ni-MOFs;

[0040] Take 200mg of Ni-MOFs and 200mg of commercial selenium powder, grind and mix them evenly with a mortar and pestle, transfer them to a square porcelain boat, and then in an argon atmosphere from room temperature to 2°C min -1 The heating rate was heated to 500 °C to obtain coral-like NiSe@NC, which was denoted as NiSe@NC-500.

Embodiment 2

[0042] This embodiment relates to a method for preparing coral-like NiSe@NC, which specifically includes the following steps:

[0043]Add 1 mmol of trimesic acid, 1 mmol of nickel nitrate hexahydrate, and 1 mmol of 4,4’-bipyridine to 20 mL of DMF in sequence, stir for half an hour, then transfer to a 30 mL vial, heat to 80°C, and react for 3 days. After waiting for the reaction system to drop to room temperature, take out the reaction vessel, wash the obtained green crystals with DMF and absolute ethanol three times, and then vacuum-dry them at 80°C for 24 hours to obtain Ni-MOFs;

[0044] Take 200mg of Ni-MOFs and 200mg of commercial selenium powder and mix them evenly with a mortar and pestle. -1 The heating rate was heated to 550 °C, and the coral-like NiSe@NC was obtained, which was denoted as NiSe@NC-550.

Embodiment 3

[0046] This embodiment relates to a method for preparing coral-like NiSe@NC, which specifically includes the following steps:

[0047] Add 1 mmol of trimesic acid, 1 mmol of nickel nitrate hexahydrate, and 1 mmol of 4,4’-bipyridyl into 20 mL of DMF in sequence, stir for half an hour, then transfer to a 10 mL vial, heat to 80°C, and react for 3 days. After waiting for the reaction system to drop to room temperature, take out the reaction vessel, wash the obtained green crystals with DMF and absolute ethanol three times, and then vacuum-dry them at 80°C for 24 hours to obtain Ni-MOFs;

[0048] Take 200mg of Ni-MOFs and 200mg of commercial selenium powder and mix them evenly with a mortar and pestle. -1 The heating rate is heated to 600 °C, and the coral-like NiSe@NC is obtained, which is denoted as NiSe@NC-600.

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Abstract

The invention provides a preparation method for similarly coralloid NiSe@NC. The preparation method comprises the following steps that S1, 4,4'-dipyridyl, trimesinic acid and nickel nitrate are dissolved in N,N-dimethylformamide sequentially, after stirring is conducted for 35 minutes at room temperature, the temperature is increased to 120-130 DEG C at the rate of 5-10 DEG C, thermal reaction isconducted for 60-70 h, and Ni-MOFs are obtained; and S2, selenium powder and the Ni-MOFs are heated to 500-800 DEG C at the rate of 1-5 DEG C / min at the argon atmosphere, and after 1-3 h of heat preservation, the similarly coralloid NiSe@NC is obtained. Compared with the prior art, the preparation method has the following beneficial effects that the metal organic frameworks with nickel as the center serve as the precursor, through a one-step in-situ selenylation strategy, the coralloid NiSe@NC is obtained, then the structure can provide abundant catalytic active sites, good electrocatalysis hydrogen production and oxygen production performance is shown, 60 and 320 mV overpotential and 53 and 101 mV dec<-1> Tafel slope are achieved, and the similarly coralloid NiSe@NC can serve as a bifunctional electrocatalyst for electrolysis hydrogen evolution and oxygen evolution.

Description

technical field [0001] The invention relates to a preparation method and application of coral-like NiSe@NC, belonging to the technical field of electrochemical catalysts. Background technique [0002] The ever-increasing energy consumption and related environmental issues around the world have triggered an urgent need for renewable and clean energy. Hydrogen energy is considered to be one of the most ideal clean energy sources due to its high energy density, environmental friendliness, and renewability. Electrolysis is an efficient and reliable way to produce hydrogen. However, the high cathodic overpotential hinders its large-scale industrial application. On the other hand, the oxygen evolution reaction is a critical and challenging step in terms of thermodynamics and kinetics. The current catalysts for electrolyzing water to produce hydrogen are mainly concentrated on noble metals such as platinum, but their high price and limited reserves seriously restrict their indus...

Claims

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Application Information

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IPC IPC(8): C25B11/06C25B1/04
CPCC25B1/04C25B11/091Y02E60/36
Inventor 戴昉纳黄招娣丁硕徐大为张美茜刘建华
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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