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Sulphur vacancy richened Ni3S2 nanorod oxygen evolution electro-catalysis material and preparing method and application thereof

An electrocatalytic material and nanorod technology, which is applied in the fields of nanotechnology, anodization, and nanotechnology for materials and surface science to achieve the effects of wide sources, high electrode oxygen evolution catalytic performance and strong stability

Inactive Publication Date: 2018-10-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the regulation of sulfur vacancies is mainly applied in two-dimensional materials (such as MoS 2 、WS 2 etc.) on the regulation of sulfur vacancies, while for Ni 3 S 2 Sulfur-vacancy regulation of

Method used

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  • Sulphur vacancy richened Ni3S2 nanorod oxygen evolution electro-catalysis material and preparing method and application thereof
  • Sulphur vacancy richened Ni3S2 nanorod oxygen evolution electro-catalysis material and preparing method and application thereof
  • Sulphur vacancy richened Ni3S2 nanorod oxygen evolution electro-catalysis material and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A Ni rich in sulfur vacancies 3 S2 The preparation method of nanorod oxygen evolution electrocatalytic material comprises the following steps:

[0039] (1) Pretreatment of the substrate: Cut the pure nickel sheet into a rectangle of 3.5cm*0.5cm, the 1cm of the upper half is used as the clamping part, and the 2.5cm of the lower half is used as the actual use part, immersed in the electrolyte for anodic oxidation deal with. Put the trimmed matrix into acetone for 30 minutes of ultrasonic vibration, then put it into absolute ethanol for 30 minutes, and then soak it in absolute ethanol.

[0040] (2) Anodic oxidation of the substrate: Prepare an anodic oxidation electrolyte with deionized water as a solvent. The composition of the electrolyte is 1wt% ammonium fluoride, 80wt% phosphoric acid, and the rest is deionized water. The actual use part of the substrate pretreated in step (1) is immersed in the electrolyte, and the clamping part is connected with the anode electrode...

Embodiment 2

[0047] A Ni rich in sulfur vacancies 3 S 2 The preparation method of nanorod oxygen evolution electrocatalytic material comprises the following steps:

[0048] (1) The pretreatment of the substrate is the same as step (1) of Example 1.

[0049] (2) The anodic oxidation of the substrate is the same as step (2) of Example 1.

[0050] (3) After the anodic oxidation is completed, remove the sample, rinse it with deionized water, and then soak it in methanol for 3-8 hours for later use.

[0051] (4) Place the anodized sample in a porcelain boat, then place the porcelain boat in the middle of the quartz tube of the tube furnace, anneal at 350°C for 2 hours in an atmosphere with a ratio of oxygen to nitrogen of 4:1, and heat up The rate is 10°C / min, and the sample is taken out after cooling to room temperature.

[0052] (5) Sulfurize the sample after annealing by hydrothermal treatment. The solution composition is 0.05mol / L sodium sulfide, 0.1mol / L ammonium fluoride, and the rest...

Embodiment 3

[0056] A Ni rich in sulfur vacancies 3 S 2 The preparation method of nanorod oxygen evolution electrocatalytic material comprises the following steps:

[0057] (1) The pretreatment of the substrate is the same as step (1) of Example 1.

[0058] (2) The anodic oxidation of the substrate is the same as step (2) of Example 1.

[0059] (3) After the anodic oxidation is completed, remove the sample, rinse it with deionized water, and then soak it in methanol for 3-8 hours for later use.

[0060] (4) Place the sample after anodic oxidation in a porcelain boat, then place the porcelain boat in the middle of the quartz tube of the tube furnace, and then anneal for 2 hours at 350°C in an atmosphere with a ratio of oxygen to nitrogen of 3:2 , the heating rate was 10°C / min, and the samples were taken out after cooling to room temperature.

[0061] (5) Sulfurize the sample after annealing by hydrothermal treatment. The solution composition is 0.05mol / L sodium sulfide, 0.1mol / L ammoniu...

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Abstract

The invention discloses a sulphur vacancy richened Ni3S2 nanorod oxygen evolution electro-catalysis material and a preparing method and application thereof, and belongs to the field of electrolytic water catalysis. The preparing method comprises three steps that firstly, a precursor film layer is prepared through anodic oxidation treatment of a nickel sheet; secondly, the precursor film layer is subjected to annealing treatment to obtain oxygen vacancy richened NiO film layer; and finally, the film layer obtained after annealing is subjected to hydrothermal sulfidizing to obtain the sulphur vacancy richened Ni3S2 nanorod oxygen evolution electro-catalysis material. As the existence of the sulphur vacancy, energy barriers needing to be overcome by a midbody on adsorption or desorption on the catalyst surface are reduced, and the oxygen evolution catalytic performance is greatly improved. Sulphur vacancy richened Ni3S2 nanorods grow on a nickel substrate in situ, the resistance between acatalyst and the substrate is reduced, and meanwhile, the oxygen evolution catalyzing stability is improved. The method is simple in operation, the requirement for preparing equipment is low, the material is environment-friendly, the preparing method has generalizability, and the development and application of the transition metal sulfide catalyst are further promoted.

Description

technical field [0001] The present invention relates to the field of electrocatalysis and electrolysis of water, in particular to a Ni that is rich in sulfur vacancies 3 S 2 Nanorod oxygen evolution electrocatalytic material, preparation method and application thereof. Background technique [0002] The continuous consumption of fossil fuels and the resulting environmental pollution force people to find an alternative new energy source. Due to its wide range of sources, high calorific value, and non-polluting products, hydrogen energy is expected to become a new energy source to replace traditional fossil fuels. In the hydrogen production method, hydrogen production by electrolysis of water is considered to be one of the most promising hydrogen production methods due to its simple process, convenient operation, and high purity of the hydrogen produced. In order to achieve large-scale hydrogen production from water electrolysis, it is particularly important to develop elect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/04C25B11/06C25D11/34B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C25B1/04C25D11/34C25B11/075Y02E60/36
Inventor 张果戈徐小兵李孔哲傅年庆
Owner SOUTH CHINA UNIV OF TECH
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