CN108823597B - Method for preparing nitrogen-doped nickel sulfide hydrogen evolution catalyst by annealing method and application thereof - Google Patents
Method for preparing nitrogen-doped nickel sulfide hydrogen evolution catalyst by annealing method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of electrocatalysis hydrogen evolution, and relates to a method for preparing a nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method. The prepared catalyst is used as a working electrode to electrolyze water under an alkaline condition to generate hydrogen. The invention takes foam nickel as a substrate, thiourea as a sulfur source and a nitrogen source, and the nitrogen-doped nickel sulfide electrocatalyst synthesized by a one-step annealing method obviously changes Ni3S2The morphology and electronic structure of the material expose more surface active sites, increase the conductivity and enhance the hydrogen evolution reaction activity. The invention solves the defects of low conductivity, few surface active sites and the like of various sulfides of nickel, improves the electrocatalytic hydrogen evolution performance, has excellent stability in alkalinity, and is expected to be industrialized.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis hydrogen evolution, relates to preparation of a hydrogen evolution catalyst, and particularly relates to a method for preparing a nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method and application thereof.
Background
The development of today's society relies heavily on fossil fuels, and the excessive consumption of fossil fuels exacerbates environmental pollution and energy crisis. Therefore, the development of clean, renewable and environmentally friendly alternative energy sources has been imminent. In contrast to various alternative energy sources, hydrogen is considered to be the most promising energy carrier to replace traditional fossil fuels due to its high combustion value and the combustion product being only water. The electrolysis of water to produce hydrogen is considered a green and sustainable method of hydrogen production. Noble metals such as platinum-based catalysts have excellent Hydrogen Evolution Reaction (HER) activity, but their use is greatly limited due to high cost and low reserves, and there is an urgent need to find more inexpensive and readily available hydrogen evolution reaction catalysts.
In recent years, various nickel-based catalysts have been widely used in the field of hydrogen evolution by electrocatalysis, and typical examples thereof include various sulfides, selenides, oxides, hydroxides and various nickel alloys of nickel. Nickel sulfides are considered to be a promising Hydrogen Evolution (HER) catalyst due to their good electrical conductivity and high stability in alkaline media. However, the catalytic activity of various sulfides reported so far with respect to nickel is still low. Studies have shown that the activity of nickel sulfide is highly correlated with the coordination number of the S atoms at the surface and the charge depletion of the adjacent Ni atoms. Therefore, the hydrogen adsorption free energy can be increased by doping nitrogen (N) to further increase the hydrogen evolution reactivity of nickel sulfide.
No nitrogen-doped nickel sulfide (N-Ni) exists at present3S2/NF) the research report of the electrocatalytic hydrogen evolution performance of the nano material in the alkaline.
Disclosure of Invention
The invention aims to disclose a method for preparing nitrogen-doped nickel sulfide (N-Ni) by annealing3S2/NF) hydrogen evolution catalyst.
The technical scheme is as follows:
the method for preparing the nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method comprises the following specific steps:
weighing thiourea into a porcelain boat according to the proportion of 0.5-2 g thiourea to one piece of pretreated foamed nickel, transferring the porcelain boat to the upstream of a programmed heating tube furnace, then placing the pretreated foamed nickel into another porcelain boat, transferring the porcelain boat to the downstream of the programmed heating tube furnace, heating to 300-500 ℃ under the protection of inert gas, calcining, preserving heat for 30-100 min, and taking out after naturally cooling to room temperature.
In a preferred embodiment of the invention, the pretreated foamed nickel is prepared by cutting the foamed nickel into a certain size, sequentially carrying out ultrasonic cleaning for 15-30 min by using hydrochloric acid and acetone to remove oxides on the surface of the foamed nickel, carrying out ultrasonic cleaning for 2-3 times by using absolute ethyl alcohol and deionized water respectively, each time for 5-10 min, and finally carrying out vacuum drying.
In a preferred embodiment of the present invention, the inert gas is nitrogen.
In a preferred embodiment of the present invention, the temperature increase rate is 5 ℃/min.
In the preferred embodiment of the invention, the proportion of 1 g of thiourea corresponding to one pretreated nickel foam is optimized, and the calcination and heat preservation are carried out for 90min at 400 ℃ under the protection of inert gas.
For comparison, the invention discloses a preparation method of a nickel sulfide hydrogen evolution electrocatalyst synthesized by a hydrothermal method, which comprises the following steps: adding 2-2.5 g of thiourea into 15-25 mL of deionized water to prepare a solution, performing ultrasonic dispersion, transferring the solution to a 50 mL polytetrafluoroethylene lined reaction kettle, obliquely placing a piece of pretreated foamed nickel into the reaction kettle and immersing the nickel in the solution, keeping the temperature of the reaction kettle at 100-150 ℃ for 4-6 hours, cooling to room temperature, taking out a sample, washing with the deionized water and absolute ethyl alcohol for multiple times respectively, and finally performing vacuum drying to obtain nickel sulfide (Ni)3S2/NF), preferably 20 mL of deionized water, 2.2g of thiourea, and incubation at 150 ℃ for 5 h.
The invention also aims to apply the prepared catalyst as a working electrode to electrolyze water under alkaline conditions for hydrogen evolution.
The invention utilizes an X-ray diffractometer (XRD), an X-ray photoelectron spectroscopy (XPS) and a Scanning Electron Microscope (SEM) to carry out an electrocatalytic hydrogen evolution experiment on water decomposed by taking a potassium hydroxide (KOH) solution as a target, and evaluates the electrocatalytic hydrogen evolution activity of the water decomposed by the electrocatalytic hydrogen evolution experiment by analyzing an electrochemical polarization curve (LSV) and a Tafel curve (Tafel plot).
32Electrocatalytic activity experiments of electrocatalysts:
(1) preparing a KOH solution with the concentration of 1 mol/L, sealing the prepared solution and placing the solution in a dark place;
(2) the electrochemical performance of the sample was tested in a three-electrode system using CHI760 electrochemical workstation (Shanghai Chenghua instruments, Inc.). Using carbon rod as counter electrode, Saturated Calomel Electrode (SCE) as reference electrode, N-Ni3S2The material is the working electrode. The electrochemical performance of the electrode material was tested in a 1 mol/L KOH electrolyte using Linear Sweep Voltammetry (LSV).
The invention has the advantages that:
(1) the porous foamed nickel is used as a conductive substrate and a nickel source, thiourea is used as a sulfur source and a nitrogen source, nickel sulfide nanowires are directly grown on the surface of the foamed nickel through a one-step annealing method, and nitrogen is introduced into the nickel sulfide, so that the method is simple;
(2) nickel sulfide is directly grown on the foamed nickel, and nitrogen doping is carried out on the nickel sulfide, so that the transmission of electrons can be accelerated. Meanwhile, the strong interaction force between the nickel sulfide and the foam nickel can improve the stability of the catalyst in an alkaline medium;
(3) ni obtained by the invention3S2Optimized N-Ni material for electrocatalytic hydrogen evolution catalyst3S2Under the alkaline condition, the current density of the NWs material is 10mA/cm2When the voltage is over-potential reaches 105 mV, the Tafel slope is only 108mV dec-1。
Advantageous effects
The porous foam Nickel (NF) has a unique three-dimensional structure, so that the NF can be used as a conductive substrate and a nickel source, not only is the surface area increased, but also the product is simple and easy to obtain. The invention takes foam nickel as a substrate and thiourea as a sulfur source and a nitrogen source, and the synthesis is carried out by a one-step annealing methodFormed nitrogen-doped nickel sulfide (N-Ni)3S2/NF) electrocatalyst with significant modification of Ni3S2The morphology and the electronic structure of the material expose more surface active sites, increase the conductivity and further enhance the hydrogen evolution reaction activity. The nitrogen-doped nickel sulfide (N-Ni) synthesized by the invention3S2the/NF) electrocatalyst solves the defects of low conductivity, few surface active sites and the like of various sulfides of the nickel, improves the electrocatalytic hydrogen evolution performance, and has excellent stability in alkalinity.
Drawings
FIG. 1 (a) shows Ni3S2SEM images of/NF NRs at high and low resolution;
(b) is N-Ni3S2SEM images of/NF NWs at high and low resolution.
FIG. 2 (a) shows N-Ni3S2Longitudinal cross-sectional SEM images of/NF NWs at low resolution;
(b) is N-Ni3S2Longitudinal cross-sectional SEM images of/NF NWs at high resolution.
FIG. 3 (a) is an XRD pattern of a blank Nickel Foam (NF);
(b, c, d) are NF and Ni respectively3S2NF NRs and N-Ni3S2EDS map of/NF NWs.
FIG. 4 (a) shows Ni3S2NF NRs and N-Ni3S2XRD pattern of/NF NWs;
(b, c, d) are each N-Ni3S2XPS plots of Ni2p, S2 p, N1S in/NF NWs.
FIG. 5, N-Ni3S2Hydrogen evolution activity test of/NF NWs electrocatalytic materials in alkaline medium (1.0M KOH):
wherein (a) is NF, Ni3S2NF NRs and N-Ni3S2Polarization curves of/NF NWs and Pt/NF in 1.0M KOH;
(b) is NF, Ni3S2NF NRs and N-Ni3S2Tafel slopes of/NF NWs and Pt/NF in 1.0M KOH;
(c) is NF, Ni3S2NF NRs and N-Ni3S2Electrochemical impedance plot of/NF NWs in 1.0M KOH;
(d) is Ni3S2NF NRs and N-Ni3S2The polarization curve after 2000 cycles of/NF NWs in alkaline (1.0M KOH) is plotted as the stability test at a certain current density.
Detailed Description
The present invention will be further described with reference to specific examples to provide those skilled in the art with a better understanding of the present invention, but the present invention is not limited to the following examples.
Comparative test
Synthesizing a nickel sulfide hydrogen evolution electrocatalyst by a hydrothermal method, weighing 2-2.5 g of thiourea in a beaker, adding 15-25 mL of deionized water, transferring to a 50 mL polytetrafluoroethylene-lined reaction kettle after ultrasonic dispersion, then obliquely placing a piece of pretreated nickel foam into the reaction kettle and immersing the nickel foam in a solution, placing the reaction kettle in an oven at 100-150 ℃ for heat preservation for 4-6 h, cooling to room temperature, taking out a sample, washing with deionized water and absolute ethyl alcohol for multiple times respectively, and finally performing vacuum drying to obtain nickel sulfide (Ni) by3S2/NF), preferably 2.2g of thiourea in 20 mL of deionized water, and held in an oven at 150 ℃ for 5 h.
Example 1
Weighing 0.5 g of thiourea, placing the thiourea in a porcelain boat, transferring the thiourea to the upstream of a temperature programmed tube furnace, placing a piece of processed foamed nickel in another porcelain boat, transferring the porcelain boat to the downstream of the temperature programmed tube furnace, heating the temperature programmed tube furnace to 400 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving the temperature for 90min, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped nickel sulfide (N-Ni)3S2/NF）。
Example 2
A method for preparing nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method comprises the steps of weighing 1.0 g of thiourea, placing the thiourea in a porcelain boat, and transferring the thiourea onto a temperature programming tube furnaceAnd then placing a piece of processed foamed nickel in another porcelain boat, transferring the porcelain boat to the downstream of a temperature programming tube furnace, heating the temperature programming tube furnace to 400 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving the heat for 90min, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped nickel sulfide (N-Ni)3S2/NF）。
Example 3
A method for preparing a nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method comprises the steps of weighing 1.5 g of thiourea, placing the thiourea in a porcelain boat, transferring the thiourea to the upstream of a temperature-programmed tube furnace, placing a piece of processed foamed nickel in another porcelain boat, transferring the porcelain boat to the downstream of the temperature-programmed tube furnace, heating the temperature-programmed tube furnace to 400 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, preserving the heat for 90min, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped nickel sulfide (N-Ni)3S2/NF）。
Example 4
Weighing 2.0 g of thiourea, placing the thiourea in a porcelain boat, transferring the thiourea to the upstream of a temperature programmed tube furnace, placing a piece of processed foamed nickel in another porcelain boat, transferring the porcelain boat to the downstream of the temperature programmed tube furnace, heating the temperature programmed tube furnace to 400 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving the temperature for 90min, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped nickel sulfide (N-Ni)3S2/NF）。
Example 5
A method for preparing a nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method comprises the steps of weighing 1.0 g of thiourea, placing the thiourea in a porcelain boat, transferring the thiourea to the upstream of a temperature-programmed tube furnace, placing a piece of processed foamed nickel in another porcelain boat, transferring the porcelain boat to the downstream of the temperature-programmed tube furnace, heating the temperature-programmed tube furnace to 300 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, preserving the heat for 90min, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped nickel sulfide (N-Ni)3S2/NF）。
Example 6
A method for preparing a nitrogen-doped nickel sulfide hydrogen evolution catalyst by an annealing method comprises the steps of weighing 1.0 g of thiourea, placing the thiourea in a porcelain boat, transferring the thiourea to the upstream of a temperature-programmed tube furnace, placing a piece of processed foamed nickel in another porcelain boat, transferring the porcelain boat to the downstream of the temperature-programmed tube furnace, heating the temperature-programmed tube furnace to 500 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, preserving the heat for 90min, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped nickel sulfide (N-Ni)3S2/NF）。
Characterization and experimental analysis of electrocatalytic activity of the prepared electrocatalyst:
as shown in FIG. 1, Ni can be seen from the graph a3S2the/NF morphology was rod-like, about 1 μm in length and about 300nm in diameter, and it can be seen from the graph b that N-Ni3S2The shape of the/NF is linear;
from FIG. 2, it can be seen that N-Ni3S2The NFNWs has a length of about 5.89 μm and a diameter of 30-80 nm;
as shown in FIG. 3, it can be seen from FIG. c that the rod-like Ni was synthesized by the hydrothermal reaction3S2the/NF contains no nitrogen element, and the linear Ni synthesized by annealing reaction can be seen from the d diagram3S2The nitrogen element is introduced into the NF;
as shown in FIG. 4, from the graph (a), diffraction peaks and Ni at 21.8 °, 31.1 °, 37.8 °, 44.3 °, 50.1 °, and 55.3 ° can be seen3S2(JCPDF # 44-1418) which is consistent with the blank foam nickel (JCPDF # 03-1051) at 44.8 °, 52.2 ° and 76.8 °; as can be seen from the graph (b), the peaks of 856.1 eV and 874.2 eV are Ni2p3/2And Ni p1/2The peak at 852.9 eV may be the peak of a foamed nickel substrate; as can be seen from FIG (c), the doublet at 162.7 eV and 163.5 eV may be S2 p3/2And S2 p1/2A peak of (a); the peak at 161.7 eV may be Ni3S2The peak of middle S-Ni; the peak at 398 eV in FIG (d) and the peak at 870.2 eV in FIG (b) are likely to be Ni-N peaks, which indicate that the nitrogen element was successfully introduced into Ni3S2Performing the following steps;
as shown in FIG. 5, N-Ni is clearly seen in the graph (a)3S2the/NFNWs electrocatalytic material has excellent electrocatalytic hydrogen evolution performance in alkalinity, and the current density of the electrocatalytic material is 10mA/cm2And 100mA/cm2Over-potential of (3) is more than NF and Ni3S2A significant reduction in/NF NRs; FIG. (b) shows that N-Ni3S2Tafel slope of/NFNWs electrocatalytic material is higher than NF and Ni3S2The smaller the/NF NRs, the faster the reaction kinetics; (c) N-Ni can be seen in the figure3S2The electrochemical resistance of the/NFNWs electrocatalytic material is better than that of NF and Ni3S2the/NFNRs are small, which indicates that the electron transmission rate is high; (d) as can be seen, N-Ni was present in the alkaline medium after 2000 cycles of CV cycling3S2the/NF NWs electrocatalytic material shows better stability, while Ni3S2The stability of the/NF NRs is relatively poor; from the i-t curve, N-Ni can also be seen3S2The current density of the/NFNWs electrocatalytic material does not decay significantly.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (7)
1. Preparation of nitrogen-doped Ni by annealing3S2The method for the hydrogen evolution catalyst is characterized by comprising the following specific steps: weighing thiourea into a porcelain boat according to the proportion of 0.5-2 g thiourea to one piece of pretreated foamed nickel, transferring the porcelain boat to the upstream of a programmed heating tube furnace, then placing one piece of pretreated foamed nickel into another porcelain boat, transferring the porcelain boat to the downstream of the programmed heating tube furnace, heating to 300-500 ℃ under the protection of inert gas, calcining, preserving heat for 30-100 min, and taking out after naturally cooling to room temperature.
2. The annealing process of claim 1 to produce nitrogen-doped Ni3S2Hydrogen evolution catalystThe method is characterized in that the pretreated foamed nickel is obtained by cutting the foamed nickel into 2 × 3 cm, carrying out ultrasonic cleaning for 15-30 min by using 3 mol/L hydrochloric acid and acetone in sequence, removing oxides on the surface of the foamed nickel, carrying out ultrasonic cleaning for 2-3 times by using absolute ethyl alcohol and deionized water respectively, carrying out 5-10 min each time, and carrying out vacuum drying at 60 ℃ to obtain the pretreated foamed nickel.
3. The annealing process of claim 1 to produce nitrogen-doped Ni3S2A method of evolving a hydrogen catalyst, characterized in that: the inert gas is nitrogen.
4. The annealing process of claim 1 to produce nitrogen-doped Ni3S2A method of evolving a hydrogen catalyst, characterized in that: the heating rate is 5 ℃/min.
5. The annealing process of claim 1 to produce nitrogen-doped Ni3S2A method of evolving a hydrogen catalyst, characterized in that: calcining at 400 ℃ for 90min under the protection of inert gas according to the proportion that 1 g of thiourea corresponds to one pretreated foamed nickel.
6. Nitrogen doped Ni obtainable by the process according to any one of claims 1 to 53S2A hydrogen evolution catalyst.
7. The nitrogen-doped Ni of claim 63S2The application of the hydrogen evolution catalyst is characterized in that: the water is electrolyzed and hydrogen is separated out under the alkaline condition by taking the electrode as a working electrode.
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| CN109759120B (en) * | 2019-03-07 | 2020-05-08 | 燕山大学 | Nitrogen and nickel co-doped cobalt selenide ultrathin nanosheet and preparation method and application thereof |
| CN110201697B (en) * | 2019-05-29 | 2020-08-04 | 浙江大学 | Three-dimensional nitrogen-doped transition metal oxide/nickel sulfide composite catalyst, and preparation method and application thereof |
| CN110180574B (en) * | 2019-06-05 | 2022-03-22 | 北京工业大学 | Preparation and application of nitrogen-doped ternary sulfide electrocatalyst material |
| CN111617780B (en) * | 2020-03-10 | 2023-05-05 | 华中师范大学 | Nitrogen-doped nickel-molybdenum-based composite sulfide for stable hydrogen production by water electrolysis and preparation method thereof |
| CN111977708B (en) * | 2020-06-23 | 2023-05-09 | 江苏大学 | Preparation method of nitrogen-doped transition metal sulfide and application of nitrogen-doped transition metal sulfide in water electrolysis |
| CN113416976A (en) * | 2021-05-31 | 2021-09-21 | 江苏大学 | Cu5FeS4/Ni3S2Preparation method of @ NF composite material and application of @ NF composite material in photoelectric hydrolysis |
| CN113668007B (en) * | 2021-07-23 | 2023-05-05 | 兰州大学 | Hydrogen evolution catalyst and preparation method and application thereof |
| CN115341166A (en) * | 2022-10-19 | 2022-11-15 | 有研工程技术研究院有限公司 | Preparation method of nickel-based vulcanized material |
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