CN114525546B - Preparation method of binary nickel cobalt selenide nanosheet material - Google Patents
Preparation method of binary nickel cobalt selenide nanosheet material Download PDFInfo
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- CN114525546B CN114525546B CN202210328339.9A CN202210328339A CN114525546B CN 114525546 B CN114525546 B CN 114525546B CN 202210328339 A CN202210328339 A CN 202210328339A CN 114525546 B CN114525546 B CN 114525546B
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a preparation method of a binary nickel cobalt selenide nanosheet material, which comprises the following specific steps: nickel nitrate hexahydrate and cobalt nitrate hexahydrate are used as a nickel source and a cobalt source, deionized water and methanol with proper proportions are used as solvents, a hydrothermal method is adopted to synthesize nickel cobalt oxalate precursor nanosheets, then the nickel cobalt oxalate precursor nanosheets are mixed with selenium powder and calcined in argon in a tubular furnace, and a nickel cobalt selenide nanosheets material is obtained. The binary nickel cobalt selenide nanosheet material prepared by the invention has larger specific surface area and higher conductivity, and greatly improves electrochemical performance when being used as an electrocatalytic material for oxygen evolution reaction.
Description
Technical Field
The invention relates to the technical field of electrochemical catalyst material preparation, in particular to a preparation method of a binary nickel cobalt selenide nanosheet material.
Background
With the rapid development of economy, there is an increasing demand for energy. New green energy sources are urgently needed due to the non-renewable nature of fossil energy sources and environmental pollution. The obtaining of hydrogen and oxygen by electrolysis of water is a solution of great interest, but the key factor limiting this is the slow kinetics of the oxygen evolution reaction. Currently, the most efficient oxygen evolution electrocatalysts on the market are mainly noble metals and their oxides, but they are difficult to use on a large scale in industry due to the high price and scarce reserves. At present, the transition metal oxide is paid more attention to due to the advantages of convenient synthesis, large yield, high storage capacity, low price and the like, wherein the nickel-cobalt compound has two redox pairs of divalent nickel/trivalent nickel and divalent cobalt/trivalent cobalt, thereby being more beneficial to the oxygen evolution reaction. Nickel cobalt selenide materials have attracted increasing researchers' favor due to their higher intrinsic conductivity and carrier transfer rate.
The traditional selenide manufacturing method is to prepare metal oxide in advance and then convert the oxide into selenide by a wet chemical method, and the method is complex in process, low in yield, and capable of leaving a large amount of waste liquid after selenization to pollute the environment. There is a strong need for a simple and efficient method of making nickel cobalt selenide materials with high conductivity and high active site count.
Disclosure of Invention
The invention aims to provide a preparation method of a binary nickel cobalt selenide nanosheet material, which has the advantages of simple and easily obtained raw materials, low production cost, high yield and no pollution, is suitable for large-scale industrial production, and has good commercial prospect.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of a binary nickel cobalt selenide nanosheet material comprises the steps of preparing a binary nickel cobalt precursor solution through a hydrothermal reaction, and then preparing the binary nickel cobalt selenide nanosheet material through a selenizing annealing method, wherein the length of a nickel cobalt selenide nanosheet is 600-700nm, the width of the nickel cobalt selenide nanosheet is 200-300nm, and the entire nanosheet material is formed by stacking multiple layers of nanosheets.
Preferably, the hydrothermal reaction specifically comprises the following steps:
(1) Placing oxalic acid into deionized water for magnetic stirring, and then placing oxalic acid solution into an ultrasonic device for ultrasonic dispersion;
(2) Adding nickel nitrate and cobalt nitrate into methanol, performing ultrasonic treatment and stirring to obtain a nitrate solution;
(3) Pouring the solution prepared in the step (2) into the solution prepared in the step (1), and stirring the mixed solution for 5-10 min to obtain the binary nickel cobalt precursor solution.
Preferably, the specific process of the step (1) is as follows, oxalic acid is placed in deionized water to be magnetically stirred for 5-10 min, the stirring speed is 600-800 r/min, and then oxalic acid solution is placed in an ultrasonic device to be subjected to ultrasonic dispersion for 5-10 min.
Preferably, in the step (2), ultrasonic is performed for 5-10 min, magnetic stirring is performed for 5-10 min, stirring speed is 600-800 r/min, and the molar ratio of nickel and cobalt ions in the obtained nitrate solution is 1:2.
Preferably, the oxalic acid is 3mmol, the deionized water is 20ml, the nickel nitrate is 1mmol, the cobalt nitrate is 2mmol, and the methanol is 40ml.
Preferably, the volume ratio of deionized water in the step (1) to methanol in the step (2) is 1:2.
Preferably, the selenization annealing method specifically includes the following steps:
(1) Adding a binary nickel cobalt precursor solution into a liner of a high-pressure reaction kettle, screwing the liner into a shell of the high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 115-125 ℃, and keeping for 20-25 h; after the hydrothermal reaction is finished, separating precipitate by centrifugation, washing the precipitate with deionized water and ethanol for 2-4 times respectively, and then placing the precipitate in a vacuum drying oven for drying;
(2) And (3) mixing the product obtained in the step (1) with selenium powder, placing the mixture in a tube furnace, annealing the mixture in an argon atmosphere, and naturally cooling the mixture to obtain the binary nickel cobalt selenide nanosheet material.
Preferably, in the step (1), after the hydrothermal reaction, the drying condition is as follows, the drying temperature is 55-65 ℃, and the drying time is 10-14 h.
Preferably, in the step (2), the calcination temperature is 300-350 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 0.5-1 h.
Preferably, in the step (2), the heat preservation time is 2 hours, the argon flow is 80-100 sccm, and the selenium powder is sublimated after being cooled along with the furnace, so that the selenization of the nanoparticle sheet is facilitated.
Compared with the prior art, the invention has the beneficial effects that:
1. the binary nickel cobalt selenide nano-sheet material has a multi-layer nano-sheet structure, can effectively improve the electrochemical active area, improve the charge transmission speed and the material diffusion, accelerate the reaction kinetics process and greatly improve the electrochemical performance of the material;
2. the binary nickel cobalt selenide nano sheet material is prepared from NiSe 2 And CoSe 2 Is compounded into NiSe 2 /CoSe 2 The oxidation-reduction pair of the bimetallic center in the binary heterogeneous material can obviously enhance the electrochemical activity of the material, and NiSe 2 And CoSe 2 Can optimize the reaction kinetics;
3. the binary nickel cobalt selenide nano-sheet material is rich in high-proportion high-valence metal ion Ni 3+ With Co 3+ Enhancing OH - The chemical adsorption of (2) promotes electron transfer, and compared with a single metal catalyst, the bimetallic catalyst has better dynamics promoting effect;
4. the binary nickel cobalt selenide nano-sheet material has excellent electrocatalytic oxygen evolution performance, and the current density is 10mA/cm -2 The over-potential of 310mV can be achieved, and the method has commercial application prospect;
5. the selenizing annealing method provided by the invention has the advantages that the stable multilayer structure is prepared, the problems of waste liquid pollution and low yield caused by the traditional wet chemical selenizing method for preparing the selenide are avoided, the preparation method is simple and stable, the yield is high, no pollution is caused, and the method is favorable for large-scale industrial production and can be applied to electrocatalytic oxygen evolution materials.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of the binary nickel cobalt selenide nanosheet material prepared in examples 1-3;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the binary nickel cobalt selenide nanosheet material prepared in example 2 at low magnification;
FIG. 3 is a Co 2p peak-splitting diagram of an X-ray photoelectron spectrum (XPS) of the binary nickel-cobalt selenide nanosheet material prepared in example 2;
FIG. 4 is a Ni 2p peak-splitting diagram of an X-ray photoelectron spectrum (XPS) of the binary nickel-cobalt selenide nanosheet material prepared in example 2;
FIG. 5 is an O1s peak-splitting diagram of an X-ray photoelectron spectrum (XPS) of a binary nickel cobalt selenide nanosheet material prepared in example 2;
FIG. 6 is a Se 3d peak-splitting diagram of an X-ray photoelectron spectrum (XPS) of the binary nickel cobalt selenide nanosheet material prepared in example 2;
FIG. 7 is a linear scanning plot (LSV) of electrolyzed water oxygen evolution for the binary nickel cobalt selenide nanoplatelets materials prepared in examples 1-3.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a binary nickel cobalt selenide nanosheet material comprises the following steps:
(1) Placing 3mmol of oxalic acid in 20ml of deionized water, magnetically stirring for 5min at the stirring speed of 600r/min, and then placing the oxalic acid solution in an ultrasonic device for ultrasonic dispersion for 5min;
(2) Adding 1mmol of nickel nitrate and 2mmol of cobalt nitrate into 40ml of methanol, carrying out ultrasonic treatment for 5min, magnetically stirring for 5min at the stirring speed of 600r/min to obtain pink transparent nitrate solution, wherein the molar ratio of nickel ions to cobalt ions is 1:2;
(3) Pouring the solution prepared in the step (2) into the solution prepared in the step (1), and stirring the mixed solution for 5min to obtain a precursor solution;
(4) Adding the precursor solution obtained in the step (3) into a liner of a high-pressure reaction kettle, screwing the liner into a shell of the high-pressure reaction kettle, putting the high-pressure reaction kettle into a blast drying oven, heating to 120 ℃, and keeping for 24 hours; after the hydrothermal reaction is finished, separating the precipitate by centrifugation, washing the precipitate with deionized water and ethanol for three times respectively, and then drying the precipitate in a vacuum drying oven at 60 ℃ for 12 hours;
(5) And (3) mixing the product obtained in the step (4) with selenium powder, placing the mixture in a porcelain boat, and annealing the mixture in an argon atmosphere, wherein the molar ratio of the precursor to the selenium powder is 0.5:1.2, the heating rate is 10 ℃/min, the annealing temperature is 350 ℃, the heat preservation time is 2 hours, the argon flow is 80sccm, and the mixture is cooled along with a furnace, so that the selenium powder sublimates, the selenization of a nano particle sheet is facilitated, and the binary nickel cobalt selenide nano sheet material is obtained.
The binary nickel cobalt selenide nano sheet material prepared by the embodiment has obvious nickel selenide and cobalt selenide phases and no impurity phase. The electrocatalytic properties of this example are shown in FIG. 7 at 10mA/cm 2 The overpotential at the current density is 324mV.
Example 2
A preparation method of a binary nickel cobalt selenide nanosheet material comprises the following steps:
(1) Placing 3mmol of oxalic acid in 20ml of deionized water, magnetically stirring for 5min at the stirring speed of 700r/min, and then placing the oxalic acid solution in an ultrasonic device for ultrasonic dispersion for 5min;
(2) Adding 1mmol of nickel nitrate and 2mmol of cobalt nitrate into 40ml of methanol, carrying out ultrasonic treatment for 5min, magnetically stirring for 5min at a stirring speed of 700r/min to obtain pink transparent nitrate solution, wherein the molar ratio of nickel ions to cobalt ions is 1:2;
(3) Pouring the solution prepared in the step (2) into the solution prepared in the step (1), and stirring the mixed solution for 5min to obtain a precursor solution;
(4) Adding the precursor solution obtained in the step (3) into a liner of a high-pressure reaction kettle, screwing the liner into a shell of the high-pressure reaction kettle, putting the high-pressure reaction kettle into a blast drying oven, heating to 120 ℃, and keeping for 24 hours; after the hydrothermal reaction is finished, separating the precipitate by centrifugation, washing the precipitate with deionized water and ethanol for three times respectively, and then drying the precipitate in a vacuum drying oven at 60 ℃ for 12 hours;
(5) And (3) mixing the product obtained in the step (4) with selenium powder and selenium powder, placing the mixture into a porcelain boat, and annealing the mixture under an argon atmosphere, wherein the molar ratio of the precursor to the selenium powder is 0.5:1.3, the heating rate is 10 ℃/min, the annealing temperature is 350 ℃, the heat preservation time is 2 hours, the argon flow is 90sccm, and cooling the mixture along with a furnace, so that the selenium powder sublimates, the selenization of a nano particle sheet is facilitated, and the binary nickel cobalt selenide nano sheet material is obtained.
The binary nickel cobalt selenide nanosheet material prepared by the embodiment has obvious nickel selenide and cobalt selenide phases and no impurity phase. The scanning morphology diagram of fig. 2 shows a clear multi-layer nanoplatelet structure, each layer of nanoplatelets having a length and width of 600-700nm and 200-300nm, respectively. The X-ray photoelectron spectra of FIGS. 3-6 show successful selenization of nickel and cobalt, no impurity incorporation, and high Ni ratio of the material obtained as seen by fitting the area ratio of peaks 3+ With Co 3+ . The electrocatalytic properties of this example are shown in FIG. 7 at 10mA/cm -2 The overpotential at the current density of (2) is 310mV, and the embodiment has lower oxygen evolution overpotential and better oxygen evolution performance.
Example 3
A preparation method of a binary nickel cobalt selenide nanosheet material comprises the following steps:
(1) Placing 3mmol of oxalic acid in 20ml of deionized water for magnetic stirring for 5min at a stirring speed of 800r/min, and then placing the oxalic acid solution in an ultrasonic device for ultrasonic dispersion for 5min;
(2) Adding 1mmol of nickel nitrate and 2mmol of cobalt nitrate into 40ml of methanol, carrying out ultrasonic treatment for 5min, magnetically stirring for 5min at a stirring speed of 800r/min to obtain pink transparent nitrate solution, wherein the molar ratio of nickel ions to cobalt ions is 1:2;
(3) Pouring the solution prepared in the step (2) into the solution prepared in the step (1), and stirring the mixed solution for 5min to obtain a precursor solution;
(4) Adding the precursor solution obtained in the step (3) into a liner of a high-pressure reaction kettle, screwing the liner into a shell of the high-pressure reaction kettle, putting the high-pressure reaction kettle into a blast drying oven, heating to 120 ℃, and keeping for 24 hours; after the hydrothermal reaction is finished, separating the precipitate by centrifugation, washing the precipitate with deionized water and ethanol for three times respectively, and then drying the precipitate in a vacuum drying oven at 60 ℃ for 12 hours;
(5) And (3) mixing the product obtained in the step (4) with selenium powder and selenium powder, placing the mixture into a porcelain boat, and annealing the mixture under an argon atmosphere, wherein the molar ratio of the precursor to the selenium powder is 0.5:1.4, the heating rate is 5 ℃/min, the annealing temperature is 350 ℃, the heat preservation time is 2 hours, the argon flow is 100sccm, and cooling the mixture along with a furnace, so that the selenium powder sublimates, the selenization of a nano particle sheet is facilitated, and the binary nickel cobalt selenide nano sheet material is obtained.
The binary nickel cobalt selenide nanosheet material prepared by the embodiment has obvious nickel selenide and cobalt selenide phases and no impurity phase. The electrocatalytic properties of this example are shown in FIG. 7 at 10mA/cm 2 The overpotential at the current density of (2) was 335mV.
As shown in FIG. 1, five distinct diffraction peaks are all capable of being compared with NiSe 2 (JCPLDS: 88-1711) and CoSe 2 Diffraction peaks of (JCPCDS: 88-1712) correspond to each other, which shows that the binary nickel cobalt selenide nanosheet materials are successfully prepared in the examples 1-3.
The binary nickel cobalt selenide nanosheet materials prepared in the embodiments 1-3 can be applied to the electrochemical field; the electrode can be selectively applied to the electrode, and the specific usage is as follows: at room temperature, 5mg of binary nickel cobalt selenide nanosheet material sample is dispersed into 990 mu L of ethanol, 10 mu L of 5wt% Nafion (perfluorinated sulfonic acid type polymer solution) solution is added for ultrasonic treatment for 30min to form a uniform solution, then 10 mu L of mixed solution is dripped onto a polished glassy carbon electrode, and the electrode is obtained after natural drying.
The foregoing is merely illustrative and explanatory of the invention, as it is well within the scope of the invention, as it is intended to provide those skilled in the art with various modifications, additions and substitutions to the specific embodiments disclosed and those skilled in the art without departing from the scope of the invention as disclosed in the accompanying claims.
Claims (8)
1. The preparation method of the binary nickel cobalt selenide nanosheet material is characterized by comprising the following steps of:
(1) Placing oxalic acid into deionized water for magnetic stirring, and then placing oxalic acid solution into an ultrasonic device for ultrasonic dispersion;
(2) Adding nickel nitrate and cobalt nitrate into methanol, performing ultrasonic treatment and stirring to obtain a nitrate solution;
(3) Pouring the solution prepared in the step (2) into the solution prepared in the step (1), and stirring the mixed solution for 5-10 min to obtain a binary nickel cobalt precursor solution;
(4) Adding a binary nickel cobalt precursor solution into a liner of a high-pressure reaction kettle, screwing the liner into a shell of the high-pressure reaction kettle, putting the high-pressure reaction kettle into a vacuum drying oven, heating to 115-125 ℃, and keeping for 20-25 h; after the hydrothermal reaction is finished, separating precipitate by centrifugation, washing the precipitate with deionized water and ethanol for 2-4 times respectively, and then placing the precipitate in a vacuum drying oven for drying;
(5) And (3) mixing the product obtained in the step (4) with selenium powder, placing the mixture in a tube furnace, annealing the mixture in an argon atmosphere, and naturally cooling the mixture to obtain the binary nickel cobalt selenide nanosheet material.
2. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: the specific process of the step (1) is as follows, oxalic acid is placed in deionized water to be magnetically stirred for 5-10 min, the stirring speed is 600-800 r/min, and then oxalic acid solution is placed in an ultrasonic device to be subjected to ultrasonic dispersion for 5-10 min.
3. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: in the step (2), ultrasonic treatment is carried out for 5-10 min, magnetic stirring is carried out for 5-10 min, the stirring speed is 600-800 r/min, and the molar ratio of nickel ions to cobalt ions in the obtained nitrate solution is 1:2.
4. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: 3mmol of oxalic acid, 20ml of deionized water, 1mmol of nickel nitrate, 2mmol of cobalt nitrate and 40ml of methanol.
5. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: the volume ratio of the deionized water in the step (1) to the methanol in the step (2) is 1:2.
6. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: in the step (4), after the hydrothermal reaction, the drying condition is as follows, the drying temperature is 55-65 ℃, and the drying time is 10-14 h.
7. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: in the step (5), the calcination temperature is 300-350 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 0.5-2 h.
8. The method for preparing the binary nickel cobalt selenide nanosheet material according to claim 1, wherein the method is characterized by comprising the following steps: in the step (5), the argon flow is 80-100 sccm.
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