CN110415995B - Preparation method of porous NiAl-LDH electrode material - Google Patents

Preparation method of porous NiAl-LDH electrode material Download PDF

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CN110415995B
CN110415995B CN201910680234.8A CN201910680234A CN110415995B CN 110415995 B CN110415995 B CN 110415995B CN 201910680234 A CN201910680234 A CN 201910680234A CN 110415995 B CN110415995 B CN 110415995B
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electrode material
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韩生
赵豆豆
常兴
常伟
薛原
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Shanghai Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
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    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention relates to a preparation method of a porous NiAl-LDH electrode material, which comprises the following steps: 1) mixing and stirring to prepare a NiAl solution; 2) carrying out hydrothermal-freeze drying treatment on the mixed solution; 3) and (3) carrying out alkali treatment on the freeze-dried powder, and then stirring, separating and drying to obtain the porous NiAl-LDH electrode material. Compared with the prior art, the preparation method of the porous NiAl-LDH electrode material is simple and environment-friendly, has controllable morphology, and can be used for research on energy storage.

Description

Preparation method of porous NiAl-LDH electrode material
Technical Field
The invention belongs to the field of material chemical energy storage, relates to a composite electrode material with controllable morphology, and particularly relates to a preparation method of a porous NiAl-LDH electrode material.
Background
With the urgent need for sustainable and renewable energy sources, along with technological innovations, a great deal of effort is devoted to producing flexible, lightweight and environmentally friendly energy storage devices. As an efficient energy storage device, the super capacitor has the advantages of high power density, high charging and discharging speed, good cycle stability and the like, and thus has received much attention. These excellent properties make supercapacitors promising for widespread use in both everyday electronics and portable electronics, as well as industrial energy management, high power density and long cycle life being indispensable conditions for widespread use in these areas. So far, the pseudocapacitance transition metal oxide/hydroxide is widely applied to the super capacitor and has the advantages of large capacitance, low cost, environmental friendliness and the like. However, the main obstacles of these materials are poor conductivity and severe agglomeration of the particulate form, resulting in low high rate performance and lower energy output.
To solve these problems, an effective method is to fix an electroactive material on a specific substrate, prepare an ordered array electrode, and increase electrical conductivity by adding a highly conductive polymer or carbon material (such as carbon nanotube, activated carbon, and graphene). For example, MnO2CNT array, Ni (OH)2Graphene nanoplates, V2O5Carbon nanotube and MnO2Conductive polymer andmixed electrodes such as axial nanowires have been explored for methods of improving electrochemical capacitive behavior. Although advances have been made in improving capacitance and durability, challenges remain in the manufacturing environment for practical power supplies due to the high cost of these materials and the complexity of the fabrication process. Therefore, it is of great significance to develop a novel hybrid electrode through a simple approach to obtain a high-performance supercapacitor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a porous NiAl-LDH electrode material. The method is simple to operate and environment-friendly, the obtained porous NiAl-LDH electrode material can overcome the defects of poor conductivity, easy agglomeration and the like of the bimetallic oxide in the prior art, and meanwhile, the composite electrode material has good cycling stability and mechanical flexibility.
The purpose of the invention can be realized by the following technical scheme:
obtaining NiAl-LDH powder through hydrothermal freeze-drying, and then obtaining the porous NiAl-LDH electrode material through alkaline precipitation treatment, wherein the method comprises the following specific steps:
(1) preparation of NiAl Mixed solution
Mixing soluble nickel salt such as nickel nitrate with deionized water, and stirring to obtain nickel nitrate water solution with certain concentration; mixing and stirring soluble aluminum salt, such as aluminum nitrate, and deionized water to obtain an aluminum nitrate solution with a certain concentration; mixing and stirring nickel nitrate and aluminum nitrate solution in different proportions; adding urea according to different proportions to control the appearance;
(2) carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution
Carrying out hydrothermal reaction on the prepared NiAl mixed solution, and carrying out centrifugal washing after the temperature is reduced to room temperature; then carrying out freeze-drying treatment on the sample;
(3) alkali precipitation-drying treatment
Dissolving the freeze-dried sample in deionized water, and stirring; adding NaOH solutions with different concentrations to perform alkali precipitation and stirring treatment; and then carrying out centrifugal separation and vacuum drying to obtain the electrode material required by the experiment.
In the invention, in the step (1), the mixing ratio of the nickel nitrate and the deionized water is 0.5mg:1ml-40mg:1 ml; the stirring time of the nickel nitrate and the deionized water is 15-30 min.
In the invention, in the step (1), the mixing ratio of the nickel nitrate and the deionized water is 0.5mg:1ml-40mg:1 ml; stirring the nickel nitrate and the deionized water for 15-30 min;
in the invention, in the step (1), the mixing ratio of the aluminum nitrate and the deionized water is 0.7mg:1ml-30mg:1 ml; stirring the aluminum nitrate and the deionized water for 15-30 min;
in the invention, in the step (1), the molar mass ratio of the nickel nitrate to the aluminum nitrate is 9:1-1:1, and the mixing and stirring time of the nickel nitrate and the aluminum nitrate is 15-30 min.
In the invention, in the step (1), the mass ratio of the nickel nitrate to the urea is 3:1-1: 5; the stirring time of the nickel nitrate and the urea is 15-30 min.
In the invention, in the step (2), the hydrothermal temperature of the mixed solution of nickel nitrate and aluminum nitrate is 90-120 ℃; the hydrothermal time of the mixed solution of nickel nitrate and aluminum nitrate is 12-24 h;
in the invention, in the step (2), the freeze-drying time of the mixed solution of the nickel nitrate and the aluminum nitrate is 12-48 h.
In the invention, in the step (3), 25-100ml of deionized water is added into the sample obtained after freeze-drying; the stirring time of the sample and the deionized water is 15-30 min.
In the invention, in the step (3), the concentration of NaOH solution required for alkali precipitation treatment is 0.5-6 mol/L; the volume of NaOH solution required for the alkaline precipitation treatment was 100-200 ml.
In the invention, in the step (3), when alkali treatment is carried out, the stirring temperature of the sample and NaOH solution is 0-30 ℃; the stirring time is 4-12 h.
Through condition screening, the molar mass of nickel nitrate and aluminum nitrate is selected to be 4:1, urea with controllable morphology is added (the ratio of nickel nitrate to urea is 1:1), and the specific gravity of different urea can influence the morphology of the prepared electrode material, so that different electrochemical properties are caused. Meanwhile, through experimental investigation, the reaction is carried out for 20 hours at 120 ℃, the freeze-drying treatment is carried out for 24 hours, and the optimal electrode material required by the final experiment is obtained by utilizing 4mol/LNaOH alkali treatment, because of different hydrothermal temperatures and time, the reaction degree, the appearance and the dispersion degree of particles of the material are different, and further the conductivity of the electrode material is influenced.
Compared with the prior art, the electrode material obtained by hydrothermal and alkali treatment solves the problems of poor conductivity, serious agglomeration in particle form, low high-rate performance and low energy output at present. The obtained porous NiAl-LDH electrode material has controllable morphology, excellent charge and discharge performance and ideal cycle stability, and is one of ideal green energy storage materials.
Drawings
FIG. 1 is a scanning electron micrograph of an electrode material prepared in example 1;
FIG. 2 is a scanning electron micrograph of the electrode material prepared in example 2;
FIG. 3 is an x-ray diffraction pattern of the electrode material prepared in example 2;
FIG. 4 is a graph of the cycling stability performance of the electrode material prepared in example 2;
FIG. 5 is a scanning electron micrograph of the electrode material prepared in example 3;
fig. 6 is a transmission scan of the electrode material prepared in example 3.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
A preparation method of a porous NiAl-LDH electrode material comprises the following steps:
(1) preparing a NiAl mixed solution: respectively preparing a soluble nickel salt aqueous solution with the concentration of 0.5-40mg/L and a soluble aluminum salt aqueous solution with the concentration of 0.7-30mg/L, mixing the soluble nickel salt and the soluble aluminum salt according to the molar ratio of 9:1-1:1, and then adding urea for shape control, wherein the mass ratio of the soluble nickel salt to the urea is 3:1-1:5, so as to obtain a NiAl mixed solution;
(2) carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution: carrying out hydrothermal reaction on the prepared NiAl mixed solution at the temperature of 90-120 ℃ for 12-24h, cooling to room temperature, carrying out centrifugal washing, and carrying out freeze-drying treatment for 12-48 h;
(3) alkali precipitation-drying treatment: dissolving the freeze-dried product in deionized water, and stirring; adding NaOH solution with the concentration of 0.5-6 mol/L to perform alkali precipitation and stirring treatment for 4-12h, wherein the temperature is controlled to be 0-30 in the process; and then carrying out centrifugal separation and vacuum drying to obtain the porous NiAl-LDH electrode material.
The following are more detailed embodiments, and the technical solutions and the technical effects obtained by the present invention will be further described by the following embodiments.
Example 1
A preparation method of a porous NiAl-LDH electrode material comprises the following steps:
(1) preparation of NiAl Mixed solution
Mixing nickel nitrate and deionized water according to a ratio of 10mg to 10ml, and stirring for 15 min; mixing aluminum nitrate and deionized water according to a ratio of 10mg to 10ml, and stirring for 15 min; mixing the prepared solution according to the molar ratio of nickel nitrate to aluminum nitrate of 2:1, and stirring for 15 min; and adding urea into the prepared NiAl mixed solution for morphology control, wherein the ratio of nickel nitrate to urea is 3:1, and then stirring the mixed solution for 15 min.
(2) Carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution
Placing the prepared NiAl mixed solution in a hydrothermal kettle at 100 ℃ for reaction for 16 hours; the temperature is reduced to room temperature, centrifugal washing is carried out, and then freeze-drying is carried out for 14h, so that the next required sample powder is obtained.
(3) Alkali precipitation-drying treatment
Dissolving the freeze-dried sample in 50ml of deionized water for dispersion, and stirring for 15 min; then 100ml of NaOH solution with a concentration of 2mol/L was added and stirred at 10 ℃ for 8 h. And (4) carrying out centrifugal separation treatment, and drying in a vacuum oven at 60 ℃ to obtain the porous NiAl-LDH electrode material.
The powder of the porous NiAl-LDH electrode material obtained above was scanned by a field emission scanning electron microscope (Zeiss ultra 55, Germany), and the scanning electron micrograph is shown in FIG. 1, and it can be seen from FIG. 1 that the electrode material is distributed in hexagonal flakes.
And (3) electrochemical performance testing:
under the condition of 1mol/LKOH electrolyte, a standard electrode is an inert Pt electrode, a reference electrode is an Ag/AgCl electrode, a working electrode is a Pt net loaded with active substances, and the electrochemical performance of the material is tested by using a three-electrode system in an electrochemical workstation and a blue-ray system. The results show that the prepared composite electrode material is 2Ag-1The charging and discharging curves under the constant current condition are symmetrical triangular, and show good pseudo-capacitance behavior. At a current of 2Ag-1In a circulation stability curve under sweeping speed, the specific capacity of the material has little change, and after 4000 times of circulation, the specific capacity can still be kept at about 80 percent, so that the material has good circulation stability.
Example 2
A preparation method of a porous NiAl-LDH electrode material comprises the following steps:
(1) preparation of NiAl Mixed solution
Mixing nickel nitrate and deionized water according to a ratio of 20mg to 10ml, and stirring for 20 min; mixing aluminum nitrate and deionized water according to a ratio of 20mg to 10ml, and stirring for 20 min; mixing the prepared solution according to the molar ratio of nickel nitrate to aluminum nitrate of 4:1, and stirring for 20 min; and adding urea into the prepared NiAl mixed solution for morphology control, wherein the ratio of nickel nitrate to urea is 1:1, and then stirring the mixed solution for 20 min.
(2) Carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution
Placing the prepared NiAl mixed solution in a hydrothermal kettle at 120 ℃ for reaction for 24 hours; and (5) cooling to room temperature, performing centrifugal washing, and freeze-drying for 24h to obtain the next required sample powder.
(3) Alkali precipitation-drying treatment
Dissolving the freeze-dried sample in 40ml of deionized water for dispersion, and stirring for 20 min; then 150ml of NaOH solution with a concentration of 4mol/L was added and stirred at 20 ℃ for 10 hours. And (4) carrying out centrifugal separation treatment, and drying in a vacuum oven at 60 ℃ to obtain the porous NiAl-LDH electrode material.
The powder of the porous NiAl-LDH electrode material obtained above was scanned using a field emission scanning electron microscope (Zeiss ultra 55, Germany) instrument, and the scanning electron micrograph obtained is shown in FIG. 2. It can be seen from figure 2 that the porous NiAl-LDH electrode material aggregated into a flower-like structure and was tested at 2-80 ° using an x-ray diffractometer (XRD), as shown in figure 3, with the NiAl peak corresponding to that of the standard card.
The electrochemical performance test method is the same as that in example 1, under the condition of 1mol/LKOH electrolyte, the standard electrode is an inert Pt electrode, the reference electrode is an Ag/AgCl electrode, the working electrode is a Pt net loaded with active substances, and the electrochemical performance of the material is tested by using a three-electrode system at an electrochemical workstation and a blue-ray system. The results show that the prepared composite electrode material is 2Ag-1The charge-discharge curve under the constant current condition is in a symmetrical triangle shape, and after 4000 cycles, as shown in figure 4, the specific capacity can still be kept at about 90 percent, and the good cycle stability is outstanding.
Example 3
A preparation method of a porous NiAl-LDH electrode material comprises the following steps:
(1) preparation of NiAl Mixed solution
Mixing nickel nitrate and deionized water according to a ratio of 30mg to 20ml, and stirring for 30 min; mixing aluminum nitrate and deionized water according to a ratio of 30mg to 20ml, and stirring for 30 min; and (3) preparing the solution according to the molar ratio of nickel nitrate to aluminum nitrate of 1:1, mixing and stirring for 30 min; and adding urea into the prepared NiAl mixed solution for morphology control, wherein the ratio of nickel nitrate to urea is 1:2, and then stirring the mixed solution for 30 min.
(2) Carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution
Placing the prepared NiAl mixed solution in a hydrothermal kettle at 120 ℃ for reaction for 20 hours; the temperature is reduced to room temperature, centrifugal washing is carried out, and then freeze-drying is carried out for 32h, so that the next required sample powder is obtained.
(3) Alkali precipitation-drying treatment
Dissolving the freeze-dried sample in 60ml of deionized water for dispersion, and stirring for 30 min; then, 120ml of a 6mol/L NaOH solution was added thereto, and the mixture was stirred at 30 ℃ for 12 hours. And (4) carrying out centrifugal separation treatment, and drying in a vacuum oven at 60 ℃ to obtain the porous NiAl-LDH electrode material.
The powder of the porous NiAl-LDH electrode material obtained above was scanned using a field emission scanning electron microscope (Zeiss ultra 55, Germany) instrument, and the scanning electron micrograph obtained is shown in FIG. 5. It can be seen from fig. 5 that the porous NiAl-LDH electrode material exhibits a flower-like structure in the aggregated state, due to the control of the concentration. And a transmission scanning electron microscope instrument is adopted to perform transmission scanning on the prepared sample, the obtained scanning transmission is shown in figure 6, and the cell material can be clearly seen to be in a porous structure.
And (3) electrochemical performance testing:
under the condition of 1mol/LKOH electrolyte, a standard electrode is an inert Pt electrode, a reference electrode is an Ag/AgCl electrode, a working electrode is a Pt net loaded with active substances, and the electrochemical performance of the material is tested by using a three-electrode system in an electrochemical workstation and a blue-ray system. The prepared composite electrode material is prepared in 2Ag-1The charge and discharge curves under the constant current condition are symmetrical and triangular, the good pseudo-capacitance behavior is shown, after 4000 cycles, the specific capacity can still be kept at about 70%, and the electrochemical performance test is influenced due to the concentration proportion.
Example 4
A preparation method of a porous NiAl-LDH electrode material comprises the following steps:
(1) preparation of NiAl Mixed solution
Mixing nickel sulfate with deionized water, and stirring for 30min to obtain a solution with a concentration of 0.5 mg/L; mixing aluminum sulfate and deionized water, and stirring for 30min to obtain a solution with the concentration of 0.7 mg/L; preparing the solution according to the molar ratio of nickel sulfate to aluminum sulfate of 9:1, mixing and stirring for 30 min; and adding urea into the prepared NiAl mixed solution for shape control, wherein the ratio of nickel sulfate to urea is 3:1, and then stirring the mixed solution for 30 min.
(2) Carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution
Placing the prepared NiAl mixed solution in a hydrothermal kettle at 90 ℃ for reaction for 24 hours; and (5) cooling to room temperature, performing centrifugal washing, and freeze-drying for 48 hours to obtain the next required sample powder.
(3) Alkali precipitation-drying treatment
Dissolving the freeze-dried sample in deionized water for dispersion, and stirring for 30 min; then, a NaOH solution having a concentration of 0.5mol/L was added thereto, and the mixture was stirred at 0 ℃ for 4 hours. And (4) carrying out centrifugal separation treatment, and drying in a vacuum oven at 30 ℃ to obtain the porous NiAl-LDH electrode material.
Example 5
A preparation method of a porous NiAl-LDH electrode material comprises the following steps:
(1) preparation of NiAl Mixed solution
Mixing nickel chloride with deionized water, and stirring to obtain a solution with the concentration of 40 mg/L; mixing aluminum trichloride with deionized water, and stirring to obtain a solution with the concentration of 30 mg/L; (ii) a The prepared solution is prepared according to the molar ratio of nickel chloride to aluminum trichloride of 1:1, mixing and stirring for 30 min; and adding urea into the prepared NiAl mixed solution for shape control, wherein the ratio of nickel chloride to urea is 1:5, and then stirring the mixed solution for 60 min.
(2) Carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution
Placing the prepared NiAl mixed solution in a hydrothermal kettle at 100 ℃ for reaction for 18 hours; and (5) cooling to room temperature, performing centrifugal washing, and freeze-drying for 12h to obtain the next required sample powder.
(3) Alkali precipitation-drying treatment
Dissolving the freeze-dried sample in deionized water for dispersion, and stirring for 30 min; then, a NaOH solution having a concentration of 1mol/L was added thereto, and the mixture was stirred at 10 ℃ for 8 hours. And (4) carrying out centrifugal separation treatment, and drying in a vacuum oven at 60 ℃ to obtain the porous NiAl-LDH electrode material.
In conclusion, according to the preparation method of the porous NiAl-LDH electrode material, the charge and discharge performance, XRD (X-ray diffraction) and scanning electron microscope performance diagrams of all the embodiments are comprehensively compared, the electrochemical performance prepared in the embodiment 2 is the best, the porous NiAl-LDH electrode material has a specific capacity of 2243F/g in constant-current charge and discharge of 2A/g, nearly 90% of the specific capacity is still maintained after 4000 cycles, the good cycle stability is highlighted, and the electrode material which has good electrochemical performance and can be applied to a supercapacitor is prepared.
The composite material of the invention fully utilizes the synergistic effect of the double-layer metal and overcomes the problem of insufficient capacitance performance of the original electrode material.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (5)

1. A preparation method of a porous NiAl-LDH electrode material is characterized by comprising the following steps:
preparing a NiAl mixed solution: respectively preparing an aqueous solution of soluble nickel salt and an aqueous solution of soluble aluminum salt, mixing, and adding urea to obtain a NiAl mixed solution;
carrying out hydrothermal-freeze drying treatment on the NiAl mixed solution: carrying out hydrothermal reaction on the prepared NiAl mixed solution, cooling to room temperature, carrying out centrifugal washing and freeze-drying treatment;
alkali precipitation-drying treatment: dissolving the freeze-dried product in deionized water, and stirring; adding 4mol/L NaOH solution to perform alkali precipitation and stirring treatment; then carrying out centrifugal separation and vacuum drying to obtain a porous NiAl-LDH electrode material;
the molar ratio of the soluble nickel salt to the soluble aluminum salt is 9:1-1: 1;
the mass ratio of the soluble nickel salt to the urea is 3:1-1: 5;
the temperature of the hydrothermal reaction is 120 ℃, and the time is 20 h;
the time for the lyophilization process was 24 h.
2. The method for preparing a porous NiAl-LDH electrode material as claimed in claim 1, wherein the soluble nickel salt is nickel nitrate, nickel sulfate or nickel chloride, and the soluble aluminum salt is aluminum nitrate, aluminum trichloride or aluminum sulfate.
3. The method for preparing a porous NiAl-LDH electrode material as claimed in claim 1 or 2, wherein the concentration of the aqueous solution of the soluble nickel salt is 0.5-40mg/L, and the concentration of the aqueous solution of the soluble aluminum salt is 0.7-30 mg/L.
4. The preparation method of the porous NiAl-LDH electrode material as claimed in claim 1, wherein the temperature of the alkali precipitation stirring treatment is 0-30 ℃; the stirring time is 4-12 h.
5. A porous NiAl-LDH electrode material prepared by the method of any one of claims 1 to 4.
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