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Preparation method of micron flower-ball-shaped high-performance full-hydrolytic bifunctional electrocatalyst FeOOH/Ni3S2

An electrocatalyst, high-performance technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc. Catalytic total water splitting performance, simple preparation method and low equipment requirements

Active Publication Date: 2019-05-24
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, FeOOH as a catalyst cannot show excellent performance due to its own semiconductor characteristics.
Currently Ni 3 S 2 The synthesis method is mainly the use of sulfur powder sintering, which requires high temperature and the discharge of toxic gases such as sulfur dioxide during the reaction process, and the synthesized samples are larger particles, the reaction kinetics is higher, and the larger Tafel slope makes it as a full-scale The application of electrocatalysts for water splitting is greatly limited
[0003] FeOOH cannot exhibit excellent electrocatalytic performance due to its low electrical conductivity
In order to increase the conductivity of FeOOH, people generally load it on noble metal materials with good conductivity, such as gold foil and platinum sheet. Although this method can indeed increase the conductivity of FeOOH and improve its catalytic performance, these substrate materials are expensive and have low reserves. , and the noble metal substrate is easily corroded during the electrochemical process, which affects the stability of the catalyst
Ni 3 S 2 (Nickel disulfide) is a nickel-based sulfide material with very good chemical stability and electrical conductivity, but its bulk material has few reactive sites and its reaction kinetics as a catalyst is poor

Method used

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  • Preparation method of micron flower-ball-shaped high-performance full-hydrolytic bifunctional electrocatalyst FeOOH/Ni3S2
  • Preparation method of micron flower-ball-shaped high-performance full-hydrolytic bifunctional electrocatalyst FeOOH/Ni3S2
  • Preparation method of micron flower-ball-shaped high-performance full-hydrolytic bifunctional electrocatalyst FeOOH/Ni3S2

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step 1: Cut the commercially available nickel foam into long strips with a size of 2cm*1cm, wash it in 3M HCl solution for 15 minutes, then use ethanol and acetone to ultrasonically clean it for 20 minutes, and finally use ultrapure water Ultrasound for 10 minutes to clean it, then dry it for later use;

[0039] Step 2: Add 0.8724g (3mmol) of nickel nitrate, 0.2283g (3mmol) of thiourea, and 0.1g (0.3mmol) of hexadecyltrimethylammonium bromide into 25mL of ethanol, and stir until it is completely dissolved. Pour the solution into a 30mL hydrothermal kettle.

[0040] Step 3: Put the cleaned foam nickel (NF) into the solution prepared in step 2 and immerse it in the oven at 150°C for 10 hours. After cooling down to room temperature naturally, take it out and rinse it with deionized water and ethanol, and put it in 80 Dry in an oven at ℃ for 3 hours to obtain Ni grown in situ on nickel foam 3 S 2 Material;

[0041] Step 4: Dissolve weighed 0.606g of ferric nitrate in a ...

Embodiment 2

[0044] Other steps are with embodiment 1, and difference is that the nickel nitrate in step 2 is changed into 0.4362g by 0.8724g.

Embodiment 3

[0046] Other steps are with embodiment 1, and difference is that the nickel nitrate in step 2 is changed into 0.2908g by 0.8724g.

[0047] Test results: Different Ni was prepared by changing the amount of nickel nitrate 3 S 2 Loaded FeOOH / Ni 3 S 2 / NF composite catalyst, and carried out X-ray diffraction, scanning electron microscopy, transmission electron microscopy, linear voltammetry scanning test, electrochemical AC impedance test, stability test, the test results are as follows Figure 1-15 shown.

[0048] figure 1 Be Ni:S=1:2 among the embodiment 5, in Fe(NO 3 ) 3 FeOOH / Ni prepared by deposition in electrolyte for 200s 3 S 2 / NF composite catalyst and FeOOH nanosheets and Ni 3 S 2 In the X-ray diffraction pattern of / NF, FeOOH nanosheets have several strong diffraction peaks at 34.1 degrees, 42.2 degrees, 53.6 degrees, and 63.5 degrees, corresponding to the standard PDF card PDF#77-0247. Ni 3 S 2 / NF samples have several strong diffraction peaks at 21.7 degr...

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Abstract

The present invention relates to a preparation method of micron flower-ball-shaped high-performance full-hydrolytic bifunctional electrocatalyst FeOOH / Ni3S2. According to the method, firstly, thioureaand nickel nitrate are adopted as raw materials, ethanol is adopted as a solution, cetyl trimethyl ammonium bromide is adopted as a surfactant, a solvothermal method is utilized to generate Ni3S2 ona foamed nickel substrate in situ, and then the micron flower-ball-shaped electrocatalyst FeOOH / Ni3S2 is formed on Ni3S2 through one-step electrochemical deposition. The composite catalyst FeOOH / Ni3S2 obtained by means of the method is low in overpotential and high in stability and has a broad application prospect in the aspects of preparation of clean hydrogen energy through electrocatalytic water decomposition and the like.

Description

technical field [0001] The invention belongs to the technical field of new functional materials, more specifically, it is a two-step method of solvothermal and electrochemical deposition to in-situ grow micron flower spherical high-performance fully water-splitting bifunctional electrocatalyst FeOOH / Ni on a nickel foam substrate. 3 S 2 preparation methods and applications. Background technique [0002] The current electrocatalytic materials for oxygen evolution and hydrogen evolution reactions are based on noble metal oxides such as iridium dioxide (IrO 2 ), ruthenium dioxide (RuO 2 ) and platinum (Pt), although they have high catalytic performance, they are expensive, scarce resources, high synthesis cost, and poor stability in the catalytic process, easy to react under acidic or alkaline reaction conditions dissolve. Therefore, the development and application of non-noble metal compounds, especially transition metal compounds, as bifunctional electrocatalytic materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043B01J35/02C25B11/06C25B1/04
CPCY02E60/36
Inventor 张兴华冀雪峰臧泽毫李响李兰兰卢遵铭刘辉
Owner HEBEI UNIV OF TECH
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