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Preparation method of Fe5Ni4S8 hydrogen evolution electro-catalytic material

An electrocatalytic material and hydrogen evolution technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex experimental operation, slow temperature rise, and no exposed active sites, etc., to achieve the experimental process Simplify, save economic cost, save time and cost

Pending Publication Date: 2020-07-14
JILIN UNIV
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Problems solved by technology

[0007] The preparation method in the above article is a high-temperature solid-phase method optimized after many experiments, but there are still some shortcomings: the experimental operation is relatively complicated, and the electrocatalytic hydrogen evolution performance of the sample needs to be improved
The reasons are: fusion vacuum sealing operation is required, calcination requires slow temperature rise, and the prepared sample is a block structure with a large particle size, which does not expose more active sites, which limits its electrocatalytic hydrogen evolution performance

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  • Preparation method of Fe5Ni4S8 hydrogen evolution electro-catalytic material
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  • Preparation method of Fe5Ni4S8 hydrogen evolution electro-catalytic material

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preparation example Construction

[0031] The present invention provides the following technical solutions: a Fe 5 Ni 4 S 8 A method for preparing a hydrogen evolution electrocatalytic material, comprising the steps of:

[0032] (1) Weigh each 1.66g, 1.75g, and 1.70g of nano-iron powder, nano-nickel powder, and sulfur powder, add absolute ethanol and grind to make it evenly mixed;

[0033] (2) The mixture is evenly placed in the ceramic ark mortar, then transferred to the tube furnace, after the pipeline is closed, nitrogen gas is introduced, the gas flow rate of nitrogen gas is 150 sccm, and the quartz tube is cleaned for 20 minutes;

[0034] (3) Heating to 700°C at a heating rate of 5°C / min, holding for 3 hours, then heating to 1100°C at the same heating rate, and holding for 10 hours;

[0035] (4) After the obtained sample is ground evenly, after adding ethanol, use a planetary ball mill to mill for 10 hours, and finally obtain the target sample Fe 5 Ni 4 S 8 .

[0036] Further elaboration is given be...

Embodiment 1

[0054] Through the present invention a kind of Fe 5 Ni 4 S 8 Granular Fe prepared by the preparation method of hydrogen evolution electrocatalytic material 5 Ni 4 S 8 The pentlandite material is denoted as S1.

[0055] In order to characterize the composition of the S1 sample and the structure or morphology of atoms or molecules, thereby determining the crystal structure, an X-ray diffraction test (XRD) was performed on the S1 sample. image 3 It is the XRD pattern of the hydrogen evolution electrocatalyst obtained in Example 1. It can be seen from the figure that the S1 samples are at 15.19°, 17.56°, 24.93°, 29.32°, 30.66°, 35.55°, 38.86°, 43.91°, 46.73°, 51.15°, 60.06°, 60.83°, 71.78°, 75.26° The diffraction peaks at ° correspond to (111), (200), (220), (311), (222), (400), (311), (511), (400) in the PDF#86-2470 standard card, respectively ), (533), (622), (731), (800) planes, indicating that Fe 5 Ni 4 S 8 For the pentlandite material, the intensity of each diffrac...

Embodiment 2

[0061] Through the present invention a kind of Fe 5 Ni 4 S 8 Part of the experimental scheme of the preparation method of the hydrogen evolution electrocatalytic material (that is, before the planetary ball mill ball milling operation) to prepare bulk Fe 5 Ni 4 S 8 The pentlandite material is denoted as S2. Compared with the experimental scheme in Example 1, in the experimental scheme of Example 2, no ball milling operation was performed. In order to compare whether the experimental optimization of the ball milling operation has an impact on the performance of the sample.

[0062] Figure 8 is the XRD pattern of the S2 sample. Compared image 3 and Figure 8 It can be observed that the peak positions of the two are consistent, and the peak shape is basically unchanged, indicating that whether the sample is ball-milled or not only affects the size of the sample and does not affect the microstructure of the sample. At the same time, the sample can still maintain good c...

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Abstract

The invention discloses a preparation method of a Fe5Ni4S8 hydrogen evolution electro-catalytic material. The method comprises the following specific steps: weighing nano iron powder, nano nickel powder and sulfur powder; adding absolute ethyl alcohol and grinding; uniformly putting the mixture into a mortar and transferring the mortar into a tubular furnace; sealing the pipeline, introducing nitrogen, cleaning the quartz tube for 20 minutes, performing heating to 700 DEG C at a heating rate of 5 DEG C / min, keeping the temperature for 3 hours, performing heating to 1100 DEG C at the same heating rate, keeping the temperature for 10 hours, performing annealing to room temperature, taking out the mixture, uniformly grinding the obtained sample, adding ethanol, and carrying out ball milling for 10 hours by using a planetary ball mill. According to the method, vacuum cladding operation is replaced by nitrogen atmosphere calcination; a quartz ampoule tube and a vacuum sealing machine whichare required by vacuum cladding are not required; and meanwhile, the experiment risk possibly caused by high sulfur pressure is also avoided due to the circulating gas atmosphere, the microcosmic sizeof the sample reaches the nanometer level due to the added ball milling operation after calcination, the active sites on the surface of the sample are increased, and the electro-catalytic hydrogen evolution performance is improved.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a Fe 5 Ni 4 S 8 Preparation method of hydrogen evolution electrocatalytic material. Background technique [0002] With the rapid development of industrialization and urbanization, the problems of environmental pollution and energy shortage are becoming more and more serious. The search for new clean and sustainable energy sources is imminent. As a clean energy with zero carbon emissions and high energy density, hydrogen energy is considered to be an ideal renewable energy source to replace traditional fossil fuels in the future. At present, industrial hydrogen production is mainly produced by steam reforming of fossil fuels, which inevitably leads to the consumption of fossil fuels and the emission of carbon dioxide. Using existing resources such as solar energy and wind energy, combined with electrochemical hydrolysis technology, provides a feasible method for hydrogen pr...

Claims

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Application Information

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IPC IPC(8): B01J27/043B01J37/20C01G53/00C25B1/04C25B11/06
CPCB01J27/043B01J37/20B01J37/0036C01G53/006C25B1/04C25B11/095B01J35/33Y02E60/36
Inventor 田宏伟张琛旭郑伟涛
Owner JILIN UNIV
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