CN114182292A - Iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide, preparation method and application thereof - Google Patents
Iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide, preparation method and application thereof Download PDFInfo
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- CN114182292A CN114182292A CN202111595373.4A CN202111595373A CN114182292A CN 114182292 A CN114182292 A CN 114182292A CN 202111595373 A CN202111595373 A CN 202111595373A CN 114182292 A CN114182292 A CN 114182292A
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Abstract
The invention discloses an iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel-iron hydroxide, a preparation method and application thereof, and belongs to the field of nano material preparation. The preparation method is simple, the component proportion is controllable, the cost is low, the material grows in situ, the combination is tight, the material is not easy to fall off, a binder is not needed, the conductivity of the catalyst is improved, and the stability of the material is also improved to a great extent. The selenide is used as a nuclear layer, so that the conductivity of the electrode can be greatly improved, the electrochemical in-situ conversion of the surface of the electrode can be realized, the stability of the electrode in an oxygen evolution reaction under an alkaline condition can be greatly improved while the stability of the nuclear layer is protected, and in addition, the amorphous hydroxide of the shell layer has a large number of defects and active sites, so that the catalytic activity of the material is greatly improved.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to an iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide, a preparation method and application thereof.
Background
With the growth of the population and the need for global development, the worldwide energy demand continues to increase rapidly. In particular, the dependence on fossil fuels leads to rapid exhaustion of the fossil fuels, and is accompanied by environmental destruction caused by toxic and harmful substances, global warming caused by greenhouse effect, and the like. Therefore, there is a need to develop renewable resources and clean energy as a substitute for traditional fossil fuels in the world to solve the problems of current energy demand increase and environmental pollution, and achieve green chemistry and sustainable development. Hydrogen is a convenient and high-energy source, and is of great interest, especially as the most promising green energy source. Hydrogen has many potential uses and is a potential energy carrier that can integrate different infrastructure systems to increase economic efficiency, reliability, flexibility and enable environmental protection. Any of these uses will help to reduce carbon emissions in both electricity and traffic. The electrolysis or electrochemical decomposition of water to produce hydrogen and oxygen is considered a clean, efficient and sustainable alternative to fossil fuels.
However, in the process of hydrogen production by water electrolysis, the oxygen evolution reaction of the anode is a four-electron reaction, and more energy is needed compared with the hydrogen evolution reaction of two electrons, so that the hydrogen production process is greatly limited. Therefore, an efficient and stable oxygen evolution catalyst is urgently needed to be found to meet the requirement of hydrogen production. At present, the oxygen evolution reaction catalyst for hydrogen production by water electrolysis in industry is noble metal such as ruthenium, iridium and the like and oxides thereof, but due to the scarcity and low stability of the noble metal, a cheap, efficient and stable catalyst is urgently needed to replace the noble metal catalyst.
At present, in various novel catalysts, metal selenides are concerned due to high metallicity and high intrinsic activity, and compared with single metal selenides, the multi-metal doped selenides greatly improve the conductivity of the selenides due to unique electronic structures, and meanwhile, the coordinated regulation and control of the multi-metal is more beneficial to the catalytic activity of the selenides on electrochemical catalysis, but after the selenides are insufficient, the selenides are easy to lose electrons in the oxygen evolution reaction process to generate oxidation reaction.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the preparation method of the iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide comprises the following steps:
(1) selenizing a ferronickel-vanadium trimetal hydrotalcite material by using selenium vapor formed by sublimation of selenium powder under the protection of inert gas based on a chemical vapor deposition method to obtain a ferrovanadium co-doped nickel diselenide material;
(2) and (3) carrying out in-situ anodic oxidation on the surface of the iron vanadium codoped nickel diselenide material by an electrochemical method to obtain the iron vanadium codoped nickel diselenide core-shell nano material coated with the nickel iron hydroxide.
Further, the specific operation of the step (1) is as follows:
and (2) mixing the components in a mass ratio of 5: and (3) mixing the selenium powder 1 with the ferronickel-vanadium trimetallic hydrotalcite material, placing the mixture in a tube furnace, heating to 400-500 ℃, keeping the temperature for 1-5 hours, and cooling to room temperature to obtain the iron-vanadium co-doped nickel diselenide material.
3. The preparation method of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide according to claim 2, wherein the heating rate and the cooling rate are both 1-10 ℃/min.
Further, the specific operation of the step (2) is as follows:
loading the iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide on carbon paper;
adopting a standard three-electrode system, taking the carbon paper as a working electrode, a platinum sheet electrode as a counter electrode, a mercury oxide electrode as a reference electrode and an electrolyte as an alkaline electrolyte;
scanning in cyclic voltammetry mode at a scanning potential range of 0.2-0.8V and a scanning speed of 1-10 mV s relative to the mercury oxide electrode-1And carrying out 2-10 times of circulation to obtain the ferronickel hydroxide-coated iron-vanadium co-doped nickel diselenide core-shell nano material.
Further, the electrolyte was 1.0M KOH.
Further, the preparation method of the nickel-iron-vanadium trimetallic hydrotalcite material in the step (1) comprises the following steps:
the formulation contained 30mM NiCl2·6H2O、10mM FeCl2·4H2O、5mM VCl3And 225mM urea aqueous solution as a precursor solution, and carrying out hydrothermal reaction for 4-12 hours at 100-180 ℃ to obtain the nickel-iron-vanadium trimetallic hydrotalcite material.
An iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel-iron hydroxide is prepared according to the preparation method disclosed by the invention.
The application of the ferronickel hydroxide-coated iron-vanadium co-doped nickel diselenide core-shell nano material disclosed by the invention is to perform an electrocatalytic oxygen evolution reaction in an alkaline aqueous solution.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the ferronickel hydroxide-coated iron-vanadium co-doped nickel diselenide core-shell nano material is simple, the component proportion is controllable, the cost is low, the material grows in situ, the bonding is tight, the material is not easy to fall off, a binder is not needed, the conductivity of the catalyst is improved, and the stability of the material is also improved to a great extent. The invention utilizes a chemical vapor phase method of selenium vapor and hydroxide to synthesize the nuclear layer selenide, and finally realizes the preparation of the doped nickel diselenide nuclear shell nano material coated with the transition metal hydroxide through electrochemical in-situ anodic oxidation operation.
The iron-vanadium co-doped nickel diselenide core-shell nano material coated with the nickel-iron hydroxide can realize the electrocatalytic oxygen evolution reaction under the alkaline condition. The selenide is used as a nuclear layer, so that the conductivity of the electrode can be greatly improved, the in-situ conversion of the surface of the electrode is realized, the stability of the electrode in an oxygen evolution reaction under an alkaline condition is greatly improved while the stability of the nuclear layer is protected, and in addition, the amorphous hydroxide of the shell layer has a large number of defects and active sites, so that the catalytic activity of the material is greatly improved.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of Fe-V co-doped nickel diselenide grown on carbon paper prepared in example 1;
FIG. 2 is an X-ray photoelectron spectroscopy (XPS) graph of Fe-V co-doped nickel diselenide grown on carbon paper prepared in example 1;
FIG. 3 is an XPS plot of iron vanadium co-doped nickel diselenide core shell nanomaterials coated with nickel iron hydroxide;
FIG. 4 is a Transmission Electron Microscope (TEM) image of the ferronickel hydroxide-coated iron-vanadium co-doped nickel diselenide core-shell nanomaterial prepared in example 1;
fig. 5 is an electrochemical linear voltammetry curve of the ferronickel hydroxide coated iron-vanadium co-doped nickel diselenide core-shell nanomaterial prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
According to the invention, the surface of the selenide material is coated with a layer of stable hydroxide material capable of improving the electrocatalytic performance to form a core-shell structure, so that the stability of the electrode is improved while the oxygen evolution reaction is promoted. Compared with selenide, the material has excellent stability; compared with hydroxide, the conductivity of the material is greatly improved.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
(1) Preparation of nickel iron vanadium trimetal hydrotalcite
The formulation contained 30mM NiCl2·6H2O、5mM FeCl2·4H2O、10mM VCl3And 20mL of aqueous solution of 225mM urea, fully dissolving to prepare precursor solution, and carrying out hydrothermal reaction for 6 hours at 120 ℃ to prepare the nickel-iron-vanadium trimetallic hydrotalcite material.
(2) Preparation of iron-vanadium co-doped nickel diselenide
And (3) placing a mixture of 100mg of selenium powder and 20mg of nickel-iron-vanadium trimetallic hydrotalcite material in a tubular furnace, heating to 450 ℃ at a heating rate of 5 ℃/min, keeping the temperature at 450 ℃ for 3 hours, and then cooling to room temperature at a speed of 5 ℃/min to obtain the iron-vanadium co-doped nickel diselenide material.
(3) Preparation of iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide
The electrochemical instrument used was a CHI760E electrochemical workstation (shanghai chenhua instruments corporation) employing a standard three-electrode system with the working electrode being selenide-loaded carbon paper, the reference electrode being mercury oxide electrode, the counter electrode being platinum sheet electrode, and the electrolyte being 1.0M KOH. Performing electrochemical experiment in cyclic voltammetry mode, with a sweep potential of 0.2-0.8V (relative to mercury oxide electrode) and a sweep rate of 5mV s-1And 3 times of circulation is carried out to obtain the iron-vanadium co-doped nickel diselenide core-shell nano material coated with the nickel-iron hydroxide.
Referring to fig. 1, fig. 1 is an X-ray of fe-v co-doped nickel diselenide grown on carbon paper prepared in example 1The line diffraction (XRD) pattern shows that the NiSe is obtained after the Fe and V are codoped2With NiSe2The crystal forms of the materials are consistent, no redundant peak appears, and the materials are proved to be NiSe after the transition metal is doped2A host phase, wherein the Fe and V transition metals are doped without changing the crystal form.
Referring to fig. 2, fig. 2 is an X-ray photoelectron spectroscopy (XPS) graph of the iron vanadium co-doped nickel diselenide grown on carbon paper prepared in example 1, from which it can be seen that Ni, Fe, V and Se are present and can be said that Fe, V have been successfully incorporated into the material.
Referring to fig. 3, fig. 3 is an XPS diagram of the iron vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel iron hydroxide. As can be seen from the figure, Ni, Fe and oxygen are present. The peaks of V, Se disappeared, demonstrating that during the in situ conversion process, the surface was oxidized in situ to nickel iron hydroxide.
Referring to fig. 4, fig. 4 is a Transmission Electron Microscope (TEM) image of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide prepared in example 1, and it can be seen that the material is in the form of nanoparticles and has a clear core-shell structure, and the interface of the core-shell can be seen.
Referring to FIG. 5, FIG. 5 is the electrochemical linear voltammetry curve of the ferronickel hydroxide-coated Fe-V co-doped nickel diselenide core-shell nanomaterial prepared in example 1, in a 1.0M KOH solution at a sweep rate of 5 mV. s-1Tests were carried out in which the working area of the working electrode was 1X 1cm2As can be seen from the graph, the current density reached 10mA cm in the course of the oxygen evolution reaction-2Only 248mV overpotential is needed.
Example 2:
(1) preparation of nickel iron vanadium trimetal hydrotalcite
The formulation contained 30mM NiCl2·6H2O、10mM FeCl2·4H2O、5mM VCl3And 20mL of aqueous solution of 225mM urea, fully dissolving to prepare precursor solution, and carrying out hydrothermal reaction for 4 hours at 100 ℃ to prepare the nickel-iron-vanadium trimetallic hydrotalcite material.
(2) Preparation of iron-vanadium co-doped nickel diselenide
100mg of selenium powder and 20mg of nickel-iron-vanadium trimetallic hydrotalcite material are mixed and then placed in a tubular furnace, the temperature is raised to 400 ℃ at the heating rate of 1 ℃/min, the temperature is kept constant for 1 hour at 400 ℃, and then the temperature is lowered to room temperature at the speed of 1 ℃/min, so that the iron-vanadium co-doped nickel diselenide material is obtained.
(3) Preparation of iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide
The electrochemical instrument used was a CHI760E electrochemical workstation (shanghai chenhua instruments corporation) employing a standard three-electrode system with the working electrode being selenide-loaded carbon paper, the reference electrode being mercury oxide electrode, the counter electrode being platinum sheet electrode, and the electrolyte being 1.0M KOH. Performing electrochemical experiment in cyclic voltammetry mode, with a sweep potential of 0.2-0.8V (relative to mercury oxide electrode) and a sweep rate of 1mV · s-1And performing 2 times of circulation to obtain the iron-vanadium co-doped nickel diselenide core-shell nano material coated with the nickel-iron hydroxide.
Example 3
(1) Preparation of nickel iron vanadium trimetal hydrotalcite
The formulation contained 30mM NiCl2·6H2O、7.5mM FeCl2·4H2O、7.5mM VCl3And 20mL of aqueous solution of 225mM urea, fully dissolving to prepare precursor solution, and carrying out hydrothermal reaction for 12 hours at 180 ℃ to prepare the nickel-iron-vanadium trimetallic hydrotalcite material.
(2) Preparation of iron-vanadium co-doped nickel diselenide
100mg of selenium powder and 20mg of nickel-iron-vanadium trimetallic hydrotalcite are mixed and then placed in a tube furnace, the temperature is increased to 500 ℃ at the heating rate of 10 ℃/min, the temperature is kept constant at 500 ℃ for 5 hours, and then the temperature is reduced to room temperature at the speed of 10 ℃/min, so that the iron-vanadium co-doped nickel diselenide material is obtained.
(3) Preparation of iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide
The electrochemical instrument used was a CHI760E electrochemical workstation (shanghai chenhua instruments corporation) employing a standard three-electrode system with the working electrode being selenide-loaded carbon paper, the reference electrode being mercury oxide electrode, the counter electrode being platinum sheet electrode, and the electrolyte being 1.0M KOH. Use ofPerforming electrochemical experiment in cyclic voltammetry mode, wherein the scanning potential range is 0.2-0.8V (relative to a mercury oxide electrode), and the scanning speed is 20mV s-1And performing 10 times of circulation to obtain the iron-vanadium co-doped nickel diselenide core-shell nano material coated with the nickel-iron hydroxide.
Example 4
(1) Preparation of nickel iron hydrotalcite
The formulation contained 30mM NiCl2·6H2O、10mM FeCl2·4H2And fully dissolving the O and 20mL of aqueous solution of 200mM urea to prepare a precursor solution, and carrying out hydrothermal reaction at 140 ℃ for 8 hours to prepare the ferronickel hydrotalcite material.
(2) Preparation of iron-doped nickel diselenide
And (3) placing the mixture of 100mg of selenium powder and 20mg of nickel-iron hydrotalcite in a tube furnace, heating to 450 ℃ at the heating rate of 8 ℃/min, keeping the temperature at 450 ℃ for 2 hours, and then cooling to room temperature at the speed of 8 ℃/min to obtain the iron-doped nickel diselenide material.
(3) Preparation of iron-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide
The electrochemical instrument used was a CHI760E electrochemical workstation (shanghai chenhua instruments corporation) employing a standard three-electrode system with the working electrode being selenide-loaded carbon paper, the reference electrode being mercury oxide electrode, the counter electrode being platinum sheet electrode, and the electrolyte being 1.0M KOH. Performing electrochemical experiment in cyclic voltammetry mode, with a sweep potential of 0.2-0.8V (relative to mercury oxide electrode) and a sweep rate of 8mV · s-1And 8 times of circulation is carried out to obtain the iron-doped nickel diselenide core-shell nano material coated with the nickel iron hydroxide.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. The preparation method of the ferronickel hydroxide-coated iron-vanadium co-doped nickel diselenide core-shell nano material is characterized by comprising the following steps of:
(1) selenizing a ferronickel-vanadium trimetal hydrotalcite material by using selenium vapor formed by sublimation of selenium powder under the protection of inert gas based on a chemical vapor deposition method to obtain a ferrovanadium co-doped nickel diselenide material;
(2) and (3) carrying out in-situ anodic oxidation on the surface of the iron vanadium codoped nickel diselenide material by an electrochemical method to obtain the iron vanadium codoped nickel diselenide core-shell nano material coated with the nickel iron hydroxide.
2. The preparation method of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide according to claim 1, wherein the specific operation of the step (1) is as follows:
and (2) mixing the components in a mass ratio of 5: and (3) mixing the selenium powder 1 with the ferronickel-vanadium trimetallic hydrotalcite material, placing the mixture in a tube furnace, heating to 400-500 ℃, keeping the temperature for 1-5 hours, and cooling to room temperature to obtain the iron-vanadium co-doped nickel diselenide material.
3. The preparation method of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide according to claim 2, wherein the heating rate and the cooling rate are both 1-10 ℃/min.
4. The preparation method of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide according to claim 1, wherein the specific operation of the step (2) is as follows:
loading the iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel iron hydroxide on carbon paper;
adopting a standard three-electrode system, taking the carbon paper as a working electrode, a platinum sheet electrode as a counter electrode, a mercury oxide electrode as a reference electrode and an electrolyte as an alkaline electrolyte;
scanning in cyclic voltammetry mode at a scanning potential range of 0.2-0.8V and a scanning speed of 1-10 mV s relative to the mercury oxide electrode-1And carrying out 2-10 times of circulation to obtain the ferronickel hydroxide-coated iron-vanadium co-doped nickel diselenide core-shell nano material.
5. The preparation method of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide according to claim 4, wherein the electrolyte is 1.0M KOH.
6. The preparation method of the iron vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel iron hydroxide according to claim 1, wherein the preparation method of the nickel iron vanadium trimetallic hydrotalcite material in the step (1) comprises the following steps:
the formulation contained 30mM NiCl2·6H2O、10mM FeCl2·4H2O、5mM VCl3And 225mM urea aqueous solution as a precursor solution, and carrying out hydrothermal reaction for 4-12 hours at 100-180 ℃ to obtain the nickel-iron-vanadium trimetallic hydrotalcite material.
7. An iron-vanadium co-doped nickel diselenide core-shell nano material coated with nickel-iron hydroxide is characterized by being prepared according to the preparation method of any one of claims 1 to 6.
8. The application of the iron-vanadium co-doped nickel diselenide core-shell nanomaterial coated with nickel-iron hydroxide as claimed in claim 7, wherein the electrocatalytic oxygen evolution reaction is performed in an alkaline aqueous solution.
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| CN115959634A (en) * | 2022-12-02 | 2023-04-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon-coated NiSe 2 Composite nano material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115959634A (en) * | 2022-12-02 | 2023-04-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon-coated NiSe 2 Composite nano material and preparation method and application thereof |
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Application publication date: 20220315 |