CN115287701A - Nickel-iron-hafnium three-metal hydrotalcite material, preparation method and application thereof - Google Patents

Nickel-iron-hafnium three-metal hydrotalcite material, preparation method and application thereof Download PDF

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CN115287701A
CN115287701A CN202211055809.5A CN202211055809A CN115287701A CN 115287701 A CN115287701 A CN 115287701A CN 202211055809 A CN202211055809 A CN 202211055809A CN 115287701 A CN115287701 A CN 115287701A
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hafnium
hydrotalcite material
ferronickel
trimetallic
preparation
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杨阳
冯婉欣
杨骞楠
贾妍
郭鹏飞
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Xi'an Huichen Technology Co ltd
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Shaanxi University of Science and Technology
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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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • 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
    • 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
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
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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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/061—Metal or alloy
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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
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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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Abstract

The invention provides a nickel-iron-hafnium trimetal hydrotalcite material, a preparation method and application, and belongs to the field of application of nano materials. The preparation method disclosed by the invention is simple and efficient, the component proportion can be regulated and controlled, the cost is low, the oxygen evolution reaction rate is greatly improved, and the stability is excellent. The invention synthesizes the ferronickel-hafnium trimetal hydrotalcite material by a simple one-step hydrothermal method. The prepared material greatly improves the defects of scarcity and high cost compared with the noble metal. The electrode obtained by the invention can be directly applied to electrocatalytic oxygen evolution reaction under alkaline conditions, and has high activity and stability.

Description

Nickel-iron-hafnium three-metal hydrotalcite material, preparation method and application thereof
Technical Field
The invention belongs to the field of application of nano materials, and particularly relates to a ferronickel-hafnium trimetallic hydrotalcite material, a preparation method and application thereof.
Background
With global environmental pollution, exacerbation of energy crisis and continuous rise of greenhouse gas content, in the coming decades, people are urgently required to explore clean and sustainable environment-friendly energy sources to gradually reduce the use of fossil fuels. Therefore, clean energy is gradually brought into the field of vision of people. Clean energy sources include a wide variety of sources such as wind, solar, tidal and hydrogen. Renewable energy sources such as wind energy, solar energy, tidal energy and the like are intermittent and cannot be effectively utilized, so that a large amount of energy is wasted. Hydrogen energy is receiving attention because of its wide source, many utilization forms and high combustion heat value. Therefore, hydrogen can be considered as one of the cleanest, most promising energy utilization modes. There are three major synthetic routes to hydrogen energy available: steam methane reforming, coal gasification and water electrolysis to produce hydrogen. In steam methane reforming and coal gasification processes, a large amount of fossil fuel is consumed, and environmental pollution and emission of greenhouse gases are caused. The hydrogen production by water electrolysis uses water as the only raw material, realizes the closed hydrogen circulation with zero emission, and is considered as the most green and sustainable hydrogen production method. However, the high cost limits the development of hydrogen production by electrolysis of water, which accounts for only a small portion of the total hydrogen production. Therefore, hydrogen production from electrolyzed water, which is gradually replacing fossil fuel, is a great challenge.
The water electrolysis is divided into two half reactions, namely a cathode hydrogen evolution reaction and an anode oxygen evolution reaction, and the anode oxygen evolution reaction is a reaction with four electrons, so that the slow dynamic reaction is realized, and the process of producing hydrogen by electrolyzing water is limited. Therefore, a high-efficiency and easily-available oxygen evolution catalyst is needed to be found, so that the oxygen evolution reaction rate is accelerated and the required overpotential is reduced to help produce hydrogen by electrolyzing water. Most of the oxygen evolution reaction catalysts which are commercially available at present are noble metal catalysts, but due to the disadvantages of high price and scarcity of noble metals, a low-cost and high-efficiency catalyst needs to be found to replace the noble metal catalysts.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a ferronickel-hafnium trimetallic hydrotalcite material, 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 ferronickel hafnium trimetal hydrotalcite material comprises the following steps:
preparing a nickel-iron-hafnium trimetal hydrotalcite material by a simple one-step hydrothermal method;
the hydrothermal reaction conditions are as follows: reacting for 6-10 h at 120-160 ℃.
Further, the method specifically comprises the following steps:
preparing Ni (NO) 3 ) 2 ·6H 2 O、FeCl 2 ·4H 2 O、HfCl 4 And carrying out hydrothermal reaction on the precursor solution which is an aqueous solution of urea at 120-160 ℃ for 6-10 h to obtain the ferronickel-hafnium trimetallic hydrotalcite material.
Further, ni (NO) in aqueous solution 3 ) 2 ·6H 2 The concentration of O is 15-60 mM.
Further, feCl 2 ·4H 2 The concentration of O is 5-20 mM.
Further, hfCl 4 The concentration of (B) is 2.5 to 10mM.
Furthermore, the concentration of urea is 112.5-450 mM.
The ferronickel-hafnium trimetal hydrotalcite material prepared by the preparation method is provided.
The application of the nickel-iron-hafnium three-metal hydrotalcite material is characterized in that the electrocatalytic oxygen evolution reaction is carried out in an alkaline aqueous solution.
Further, loading a ferronickel-hafnium trimetal hydrotalcite material on the foamed nickel to serve as a working electrode;
and carrying out electrocatalytic oxygen evolution reaction in alkaline electrolyte by taking the counter electrode as a platinum electrode and the reference electrode as a mercury oxide electrode.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the ferronickel-hafnium trimetal hydrotalcite material has the advantages that the component proportion is adjustable, the cost is low, nickel is used as low-valence metal, iron and doped hafnium are used as high-valence metal, and urea is used as a precipitator to form the ferronickel-hafnium trimetal hydrotalcite material, so that the oxygen evolution reaction rate is greatly improved, and the ferronickel-hafnium trimetal hydrotalcite material has excellent stability. The invention synthesizes the ferronickel-hafnium trimetal hydrotalcite material by a simple one-step hydrothermal method, and reduces the cost compared with noble metals.
The ferronickel-hafnium trimetal hydrotalcite material disclosed by the invention has the advantages that the material grows in situ, the combination is tight, the material is not easy to fall off, the doping of the hafnium element promotes the electronic synergistic effect among metal cations and accelerates the electron transfer rate, the intrinsic activity of the oxygen evolution reaction is improved, and compared with a noble metal catalyst, the cost is greatly reduced and the oxygen evolution reaction rate is accelerated. The material characterization shows that the catalyst has good stability.
The application of the nickel-iron-hafnium three-metal hydrotalcite material can realize the electrocatalytic oxygen evolution reaction under the alkaline condition, and has high activity and stability.
Drawings
FIG. 1 is an X-ray diffraction pattern of the NiFe-Hf trimetallic hydrotalcite material of example 1;
FIG. 2 is an X-ray photoelectron spectrum of the Tri-metal hydrotalcite material of example 1;
FIG. 3 is a scanning electron microscope image of the NiFeHf trimetallic hydrotalcite material prepared in example 1;
FIG. 4 is a graph of oxygen evolution reaction performance test of the NiFeHf trimetallic hydrotalcite material of 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 other sequences than those illustrated or described herein. Moreover, 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.
At present, in various novel catalysts, hydrotalcite attracts much attention due to the characteristics of controllable interlayer spacing, large specific surface area, ion exchange and the like, but the conductivity of hydrotalcite is also insufficient. The transition metal is used as an electrocatalyst widely applied to the current industry, the nickel-iron-hafnium tri-metal hydrotalcite material prepared by the invention firstly has greatly reduced cost compared with noble metal, and secondly has greatly improved conductivity and excellent stability compared with a pure bimetallic hydrotalcite material.
The invention is described in further detail below with reference to the accompanying drawings:
example 1:
preparation of nickel-iron-hafnium trimetal hydrotalcite
Preparation of a 15mM Ni (NO) 3 ) 2 ·6H 2 O、5mM FeCl 2 ·4H 2 O、2.5mM HfCl 4 And 40mL of aqueous solution of 112.5mM urea as precursor solution, carrying out hydrothermal reaction for 6 hours at 120 ℃, washing and filtering a reaction product to obtain the ferronickel-hafnium trimetallic hydrotalcite material.
Referring to fig. 1, fig. 1 is an XRD pattern of the NiFe-hf trimetallic hydrotalcite material prepared in example 1, and it can be seen from the figure that the diffraction peaks of NiFe LDH are well matched, which proves that hafnium element is successfully doped into NiFe LDH, and the NiFe-hf trimetallic hydrotalcite material is successfully prepared.
Referring to fig. 2, fig. 2 is an XPS plot of the nife-Hf trimetallic hydrotalcite material prepared in example 1, from which it can be seen that the presence of Ni, fe and Hf led to the successful preparation of the nife-Hf trimetallic hydrotalcite material.
Referring to fig. 3, fig. 3 is a scanning electron microscope image of the nife-hf trimetallic hydrotalcite material prepared in example 1, and it can be seen that the material is in the form of nano-platelets.
Referring to FIG. 4, FIG. 4 is a plot of the electrochemical linear voltammetry of the NiFeHf-NiFei-trimetallic hydrotalcite material prepared in example 1 in a 1.0M KOH solution at a sweep rate of 5 mV. S -1 The test was conducted with a working electrode working area of 0.196cm 2 As can be seen from the graph, the current density reached 10mA cm in the course of the oxygen evolution reaction -2 Only 276mV of overpotential is needed.
Example 2:
preparation of nickel-iron-hafnium trimetal hydrotalcite
Preparation of a composition containing 30mM Ni (NO) 3 ) 2 ·6H 2 O、10mM FeCl 2 ·4H 2 O、5mM HfCl 4 And 40mL of aqueous solution of 225mM urea, fully dissolving to prepare a precursor solution, carrying out hydrothermal reaction for 10 hours at 120 ℃, washing and filtering a reaction product, and obtaining the nickel-iron-hafnium trimetallic hydrotalcite material.
Example 3:
preparation of nickel-iron-hafnium trimetal hydrotalcite
60mM Ni (NO) was prepared 3 ) 2 ·6H 2 O、20mM FeCl 2 ·4H 2 O、10mM HfCl 4 And 40mL of aqueous solution of 450mM urea, fully dissolving to prepare a precursor solution, carrying out hydrothermal reaction for 12 hours at 160 ℃, washing and filtering a reaction product, and obtaining the nickel-iron-hafnium trimetallic hydrotalcite material.
Example 4:
preparation of nickel-iron-hafnium trimetal hydrotalcite
Preparation of a composition containing 30mM Ni (NO) 3 ) 2 ·6H 2 O、10mM FeCl 2 ·4H 2 O、10mM HfCl 4 And 100mL of aqueous solution of 200mM urea, fully dissolving to prepare precursor solution, carrying out hydrothermal reaction for 12 hours at 120 ℃, washing and filtering a reaction product to obtain the nickel-iron-hafnium trimetallic hydrotalcite material.
Example 5:
preparation of nickel-iron-hafnium trimetal hydrotalcite
60mM Ni (NO) was prepared 3 ) 2 ·6H 2 O、5mM FeCl 2 ·4H 2 O、5mM HfCl 4 And 40mL of aqueous solution of 300mM urea, fully dissolving to prepare precursor solution, carrying out hydrothermal reaction for 12 hours at 100 ℃, washing and filtering a reaction product to obtain the nickel-iron-hafnium trimetallic hydrotalcite material.
The products prepared in examples 2-5 are all characterized in that nickel-iron-hafnium trimetallic hydrotalcite is prepared.
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 hafnium trimetal hydrotalcite material is characterized in that Ni (NO) is prepared 3 ) 2 ·6H 2 O、FeCl 2 ·4H 2 O、HfCl 4 And urea aqueous solution as precursor solution, and carrying out hydrothermal reaction for 6-12 h at 100-160 ℃ to obtain the ferronickel-hafnium trimetallic hydrotalcite material.
2. The method of claim 1, wherein Ni (NO) is present in the precursor solution 3 ) 2 ·6H 2 The concentration of O is 15-60 mM.
3. The method of claim 1, wherein a precursor solution of FeCl is FeCl 2 ·4H 2 The concentration of O is 5-20 mM.
4. The method of claim 1, wherein the HfCl in the precursor solution is HfCl 4 The concentration of (B) is 2.5 to 10mM.
5. The method of preparing a ferronickel hafnium trimetallic hydrotalcite material according to claim 1, wherein the concentration of urea in the precursor solution is 112.5-450 mM.
6. A ferronickel hafnium trimetallic hydrotalcite material prepared by the method of any one of claims 1 to 5.
7. Use of the ferronickel hafnium trimetallic hydrotalcite material according to claim 6, characterized in that the electrocatalytic oxygen evolution reaction is carried out in an aqueous alkaline solution.
8. The use of the ferronickel hafnium trimetallic hydrotalcite material as claimed in claim 7, wherein the ferronickel hafnium trimetallic hydrotalcite material is loaded on nickel foam as a working electrode;
and carrying out electrocatalytic oxygen evolution reaction in alkaline electrolyte by taking the counter electrode as a platinum electrode and the reference electrode as a mercury oxide electrode.
CN202211055809.5A 2022-08-31 2022-08-31 Nickel-iron-hafnium three-metal hydrotalcite material, preparation method and application thereof Withdrawn CN115287701A (en)

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