CN115369435A - Preparation method of foam nickel oxygen evolution electrode material with multilevel array structure, product and application thereof - Google Patents

Abstract

The invention discloses a preparation method of a foamed nickel oxygen evolution electrode material with a multi-level array structure: (1) pickling and activating the foamed nickel; (2) preparing a manganese etching solution with manganese salt and hydrochloric acid, and preparing it with ferric salt Iron etching solution; (3) soaking the foamed nickel after activation in the manganese etching solution; (4) transferring the foamed nickel soaked in step (3) to the iron etching solution for soaking to obtain the modified nickel foam; ( 5) The modified nickel foam is electrochemically activated in situ to obtain a multi-level array structure nickel foam oxygen evolution electrode material. The invention also discloses the foamed nickel oxygen evolution electrode material with multi-level array structure obtained by the above preparation method and its application in oxygen evolution reaction. The preparation method is simple and effective, and does not require high-temperature reaction conditions; the electrode material has excellent oxygen evolution reaction performance and can work efficiently and stably at a large current density.

Description

A kind of preparation method and product of multilevel array structure nickel foam oxygen evolution electrode material and application

technical field

The invention belongs to the technical field of electrochemistry, and in particular relates to a preparation method of a foamed nickel oxygen evolution electrode material with a multi-level array structure and its product and application.

Background technique

Oxygen evolution reaction (OER), as a half-reaction of important technologies such as electrolysis of water, electrochemical synthesis of ammonia, and electrochemical carbon dioxide reduction, involves complex multi-electron-proton coupling steps and has a very slow kinetic process, which requires more energy consumption . The current catalysts with high activity are mostly noble metal-based nanomaterials (such as Ru, Ir, etc.) that are expensive and have a scarce crust content, which significantly increases the cost of these technical applications and restricts the large-scale application of these electrocatalytic technologies. Therefore, seeking and developing low-cost and high-activity catalytic materials for oxygen evolution reaction has become a research hotspot.

In recent years, studies have shown that multi-metal doped nickel foams have excellent catalytic activity for oxygen evolution reaction under alkaline conditions, which can effectively reduce the overpotential. At present, some foamed nickel-based electrode materials exhibit better catalytic performance than noble metal materials at low current densities (eg, 10 mAcm ² ). However, electrode materials for oxygen evolution reaction that can work efficiently at high current densities (>1000mA cm ² ) are seldom reported. In general, polymer binders such as nafion must be used to combine the powder electrocatalyst with the substrate. However, the polymer binder will not only increase the series resistance, block the active sites, inhibit the diffusion of the electrolyte, and lead to weakened catalytic activity, but also the coating process is cumbersome, which is not conducive to large-scale preparation. If the nanocatalysts are directly grown in situ on the conductive substrate to form self-supporting electrodes, there is no need to use polymer binders to avoid the aforementioned disadvantages.

However, the foamed nickel-based self-supporting electrode material obtained by the hydrothermal method or electrodeposition method commonly used at present has a single surface active component and has better performance at low current densities, but at high current densities, a large number of bubbles When detached from the surface of the active component, the mass transfer is seriously affected, making the mass transfer the rate-controlling step under high current, and the tensile stress caused at the interface between the bubble and the active component will seriously damage the active component, resulting in structural damage and Performance decays rapidly. For example, the Chinese patent with publication number CN113802162A discloses a nickel/molybdenum selenide bifunctional composite catalyst and its preparation method and application, belonging to the technical field of new energy materials and electrochemical energy storage. The present invention washes foamed nickel with dilute hydrochloric acid, deionized water and absolute ethanol, then dissolves selenium dioxide, sodium molybdate and nickel acetate in deionized water, and uses graphite rods as counter electrodes in a standard three-electrode system , with nickel foam as the working electrode and silver/silver chloride as the reference electrode, the precursor sample was prepared by a simple electrodeposition method; after the electrodeposition was completed, the prepared precursor sample was rinsed and dried with deionized water The nickel/molybdenum selenide bifunctional composite catalyst is obtained. For example, the Chinese patent with publication number CN111437819A discloses a method and application of synthesizing cobalt-doped nickel-iron mesh nanosheet array with high efficiency and bifunctional electrocatalyst. Through a simple two-pot hydrothermal method, first pretreat the foamed nickel, then immerse the pretreated foamed nickel in the nickel-iron salt solution, take it out after a period of hydrothermal reaction, and then immerse it in the cobalt salt solution for hydrothermal reaction, then take it out Drying yields cobalt-doped nickel-iron mesh nanosheet arrays with high efficiency and bifunctional electrocatalysts.

Therefore, the development of foamed nickel-based electrode materials with simple synthesis methods, environmental friendliness, high efficiency, stability, and rapid bubble detachment under high current has very important strategic significance for the research of oxygen evolution reaction electrodes.

Contents of the invention

The object of the present invention is to provide a kind of preparation method of nickel foam oxygen evolution electrode material of multi-level array structure, and this preparation method is simple and effective, does not need high-temperature reaction condition; It has excellent oxygen evolution reaction performance and can work efficiently and stably at high current density.

In order to solve the above problems, the present invention provides the following technical solutions:

A kind of preparation method of foamed nickel oxygen evolution electrode material of multilevel array structure, described preparation method comprises the following steps:

(1) nickel foam is carried out to pickling and activation treatment;

(2) Manganese etching solution is configured with manganese salt and hydrochloric acid, and iron etching solution is configured with ferric salt;

(3) the activated nickel foam is placed in the manganese etching solution for immersion;

(4) the nickel foam soaked in step (3) is transferred to the iron etching solution for soaking to obtain the modified nickel foam;

(5) The modified nickel foam is electrochemically activated in situ to obtain a multi-level array structure nickel foam oxygen evolution electrode material.

In step (2), the manganese salt is one or more of manganese chloride, manganese nitrate and manganese sulfate; the ferric salt is one or more of ferric chloride, ferric nitrate and ferric sulfate Various. Preferably, the manganese salt is manganese chloride, and the ferric salt is ferric chloride: the oxidation of nitrate is too strong, the corrosion ability to the electrode is too strong, the foamed nickel electrode is prone to over-corrosion, and the structure is damaged. Destruction; the etching ability of sulfate is too weak, and there are fewer nucleation sites for manganese salts; chloride salts can properly activate the foamed nickel substrate, etch the electrode surface, and provide nucleation sites.

In step (2), a manganese etching solution is prepared with a substance concentration of 0.1-5 mol/L manganese salt and 0.1-1M hydrochloric acid, and an iron etchant is prepared with a substance concentration of 0.1-1 mol/L ferric salt. The number of nickel-manganese spheres etched by manganese salt lower than 0.1mol/L is small, the thickness is thin, and it is easy to combine with nickel-iron nanosheets, but there are few active sites; The number of manganese spheres is large, the thickness is thick, and there are many active sites, but it is not easy to combine with nickel-iron nanosheets. The nickel-iron nanosheets etched by iron salts lower than 0.01mol/L have low density, large pore size, and few active sites, but they are closely combined with nickel-manganese spheres; the nanosheets etched by iron salts higher than 1mol/L The sheet density is high, the pore size is small, and there are many active sites, but it will damage the nickel-manganese pellets. Manganese chloride with a concentration of 1-5mol/L and 0.2-0.5M hydrochloric acid is preferred to configure the manganese etching solution, and the iron etching solution is configured at a concentration of 0.5mol/L to make the active sites easier to combine and obtain a more suitable density and pore size , with a better oxygen evolution reaction.

In step (3), the activated nickel foam is soaked in manganese etching solution for 0.1-12 hours at an ambient temperature of 20-80°C. This is because when the immersion time in the manganese etching solution is less than 0.1h, the number of nickel-manganese spheres after etching is small, the thickness is thin, and it is easy to combine with nickel-iron nanosheets, but there are few active sites; The number of nickel-manganese spheres after etching is large, the thickness is thick, and there are many active sites, but they are not easy to combine with nickel-iron nanosheets. When the ambient temperature is lower than 20°C, the hydrolysis of manganese salt is slow, and the number of nickel-manganese spheres produced is small and thin, which is easy to combine with nickel-iron nanosheets, but there are few active sites; when the ambient temperature is higher than 80°C, the hydrolysis of manganese salt is fast The number of nickel-manganese spheres is large, the thickness is thick, and there are many active sites, but it is not easy to combine with nickel-iron nanosheets. The preferred soaking time is 10 minutes, and the ambient temperature is 50°C.

In step (3), the hydrochloric acid has activation and etching effects on the surface of the nickel foam, and nickel ions and manganese ions are hydrolyzed and deposited on the surface of the nickel foam.

In the step (4), the nickel foam soaked in the step (3) is transferred to the iron etching solution for soaking for 0.1-2h. The density of nickel-iron nanosheets etched by iron salt less than 0.1h is small, the pore size is large, and the active sites are few, but they are closely combined with nickel-manganese spheres; the density of nanosheets etched by iron salts soaked for more than 2h High, small pore size and many active sites, but it will damage the structure of nickel-manganese pellets and foamed nickel electrodes. Therefore, the above conditions are set in order to obtain nickel-iron nanosheets with more suitable density and pore size. The preferred condition is 5-10min.

In step (4), the ferric iron has an etching effect on the foamed nickel, and nickel ions and iron ions are hydrolyzed and deposited on the surface of the foamed nickel.

In step (5), the electrochemical activation is one or more of linear sweep voltammetry, cyclic voltammetry, constant current method and constant voltage method.

In step (5), the linear sweep voltammetry and cyclic voltammetry put the voltage range between 0-2.5V (vs.RHE), scan or cycle 1-80 times; when the initial voltage exceeds Low, the activation effect on the electrode is small, and the voltage is too high, which will cause the catalytic active components on the electrode surface to fall off. And the number of scans is less, the activation effect is not obvious, and the number of scans is too many, which reduces the stability of the electrode. The preferred condition is 1.2-1.8V, 40 scans.

The current density of the constant current method is 10-1500mA cm ^-2 , and the reaction time is 0.05-3h. When the activation current is too low, the activation effect on the electrode is small, and the current is too high, which will cause the catalytic active components on the electrode surface to fall off. If the activation time is short, the activation effect is not obvious, and if the activation time is too long, the stability of the electrode will be reduced. The preferred condition is 100mA cm ^-2 for 5 minutes.

The voltage of the constant voltage method is 1.5-3.5V (vs. RHE), and the reaction time is 0.05-3h. When the activation voltage is too low, the activation effect on the electrode is small, and the voltage is too high, which will cause the catalytic active components on the electrode surface to fall off; at the same time, the activation time is short, the activation effect is not obvious, and the activation time is too long, reducing the stability of the electrode. The optimal condition is 1.6V, and the time is 5min.

The present invention also provides a foamed nickel oxygen evolution electrode material with a multi-level array structure obtained according to the above preparation method.

The structure of the multi-level array structure foamed nickel oxygen evolution electrode material is: nickel-manganese-based pellet arrays, nickel-iron-based nanosheet arrays and hole structures are distributed on the surface of the foamed nickel; the diameter of the nickel-manganese-based pellets is 0.1 -0.5 μm, uniformly distributed to form an array; the length of the nickel-manganese-based nanosheets is 10-100nm, and the interval between adjacent nanosheets is 10-100nm, uniformly distributed to form an array.

The invention also provides the application of a foamed nickel oxygen evolution electrode material with multilevel array structure in oxygen evolution reaction.

The preparation method of the present invention uses foamed nickel as a base, utilizes the hydrolysis and deposition of nickel ions, manganese ions and iron ions, and the etching of nickel by ferric ions, and then obtains oxygen evolution by in-situ electrochemical activation of foamed nickel with a multi-level array structure electrode material. When using etching solution to etch foamed nickel, the pH rises to promote the hydrolysis of nickel ions, iron ions and manganese ions, and the etching of nickel by ferric ions, and then adjust the concentration of etching solution and soaking time to obtain Appropriate amount of multi-metal doping. Then, in the electrochemical process, in-situ corrosion and electrochemical reconstruction of nickel foam, a multi-metal-doped multi-level array structure nickel foam oxygen evolution electrode is obtained.

Compared with the prior art, the present invention has the advantages of:

The preparation process of the existing oxygen evolution reaction foamed nickel-based multi-metal doped electrode material is cumbersome and under high current density, a large number of bubbles hinder the contact between the electrode and the electrolyte, making mass transfer a problem in the rate-controlling step. Compared with the prior art, the preparation process of this method is simple and effective, and does not require high-temperature reaction conditions, and the material with a special multi-level array structure prepared by the method of the present invention is conducive to the rapid transfer of bubbles when undergoing an oxygen evolution reaction; Doping regulates the electronic structure, so that it has excellent oxygen evolution reaction performance. The best overpotential of the electrode material is only 208mV when the current density is 10mA cm ^-2 ; and at a large current density of 1000mA cm ^-2 , Its overpotential is only 406mV. Moreover, the nickel foam participates in the reaction and is corroded in situ, so that the nanosheets on the surface and the nickel foam substrate have a strong bonding force, and can work efficiently and stably at a large current density. The electrode prepared by this method can maintain the stability for at least 48 hours under the optimal current density of 1000mA cm ^-2 , exhibits low overpotential and high stability, and satisfies market requirements well.

Description of drawings

Figure 1 is a scanning electron microscope image and an elemental mapping image of the Ni foam oxygen evolution electrode material with a multi-level array structure prepared in Example 1.

Fig. 2 is the linear sweep voltammetry performance test graph of multilevel array structure nickel foam oxygen evolution electrode material, iron etching foam nickel, manganese etching foam nickel, iridium dioxide loaded foam nickel and foam nickel prepared in Example 1.

Fig. 3 is a galvanostatic stability test diagram of the nickel foam oxygen evolution electrode material with a multi-level array structure prepared in Example 1 of the present invention.

Detailed ways

In order to make the above objects, features and advantages of the present invention more obvious and comprehensible, the specific implementation manners of the present invention will be described in detail below in conjunction with the embodiments of the specification.

In the following description, a lot of specific details are set forth in order to fully understand the present invention, but the present invention can also be implemented in other ways different from those described here, and those skilled in the art can do without departing from the connotation of the present invention. By analogy, the present invention is therefore not limited to the specific examples disclosed below.

Second, "one embodiment" or "an embodiment" referred to herein refers to a specific feature, structure or characteristic that may be included in at least one implementation of the present invention. "In one embodiment" appearing in different places in this specification does not all refer to the same embodiment, nor is it a separate or selective embodiment that is mutually exclusive with other embodiments.

Example 1

Sonicate the nickel foam in acetone for 30 minutes to remove oil, and clean it with absolute ethanol; then put it in absolute ethanol for 30 minutes, and clean it with ultrapure water; Clean with pure water, stand-by; configure manganese etching solution with the concentration of substance 1mol/L manganese chloride and 0.2M hydrochloric acid, configure iron etching solution with concentration of substance 0.5mol/L ferric chloride; foam nickel after activation Soak in manganese etching solution for 10 minutes at an ambient temperature of 50°C; then transfer the manganese-etched nickel foam to iron etching solution and soak for 5 minutes, take out the foam nickel, wash it, and dry it. Finally, the modified nickel foam was directly used as an electrode, and in-situ electrochemical activation was performed by cyclic voltammetry to obtain a multi-level array structure nickel foam oxygen evolution electrode material (FeMn NF), in which the cycle range was 1.0-1.7V (vs. RHE), the sweep rate is 50mV/s, and the cycle is 40 cycles. Referring to Figure 1, nickel-manganese-based spheres are distributed on the surface of nickel foam, with a diameter of 0.1-0.5 μm, uniformly distributed to form an array; the length of nickel-manganese-based nanosheets is 10-100nm, and the interval between adjacent nanosheets is 10-100nm, uniformly distributed to form an array . The element map shows the uniform distribution of iron and manganese.

In order to test the performance of the prepared multi-level array structure nickel foam oxygen evolution electrode material, the electrochemical performance test was carried out, and the results are shown in Figure 2 and Figure 3:

Fig. 2 is embodiment 1 of the present invention foam nickel oxygen evolution electrode material, comparative example iron etching foam nickel, iridium dioxide loaded foam nickel and foam nickel's linear sweep voltammetry performance test figure, as can be seen from the figure The overpotential of nickel foam oxygen evolution electrode material with multi-level array structure is only 208mV when the current density is 10mA cm ^-2 ; the overpotential is 269mV when the current density is 100mA cm ^-2 ; the overpotential is only 406mV when the current density is 1000mA cm ^-2 . To achieve the corresponding current densities, nickel foam etched with iron alone requires 223mV, 293mV, and 460mV, respectively. Pure nickel foam is difficult to work at high current densities, and this transition metal-based electrode outperforms the current benchmark noble metal IrO ₂ (332mV, 100mA cm ^-2 ).

Figure 3 is the galvanostatic stability test diagram of the multi-level array structure nickel foam oxygen evolution electrode material. It can be seen from the figure that the overpotential of the material has no obvious increase after 48 hours of testing at a current density of 1000mA cm ^-2 , so it can be used in Under the condition of current density 1000mA cm ^-2 , it can work stably for at least 48h.

Example 2

Sonicate the nickel foam in acetone for 30 minutes to remove oil, and clean it with absolute ethanol; then put it in absolute ethanol for 30 minutes, and clean it with ultrapure water; Clean with pure water, stand-by; configure manganese etching solution with the concentration of substance 5mol/L manganese chloride and 0.2M hydrochloric acid, configure iron etching solution with concentration of substance 0.5mol/L ferric chloride; foam nickel after activation Soak in manganese etching solution for 10 minutes at an ambient temperature of 50°C; then transfer the manganese-etched nickel foam to iron etching solution and soak for 5 minutes, take out the foam nickel, wash it, and dry it. Finally, the modified nickel foam is directly used as an electrode, and the in-situ electrochemical activation is performed by linear sweep voltammetry to obtain a multi-level array structure nickel foam oxygen evolution electrode material, in which the cycle range is 1.0-1.7V (vs.RHE), The scanning speed is 10mV/s, and the scanning is performed 20 times. When the current density is 10mA cm ^-2 , the overpotential is 251mV; when the current density is 100mA cm ² , the overpotential is 294mV; when the current density is 1000mA cm ^-2 , the overpotential is 420mV. Under the current density of 1000mA cm ^-2 , the overpotential of the material did not increase significantly after testing for 12 hours.

Example 3

Sonicate the nickel foam in acetone for 30 minutes to remove oil, and clean it with absolute ethanol; then put it in absolute ethanol for 30 minutes, and clean it with ultrapure water; Wash with pure water and wait for use; prepare manganese etching solution with a concentration of 1mol/L manganese chloride, 1mol/L manganese nitrate, 1mol/L manganese sulfate and 0.2M hydrochloric acid, and chlorinate with a concentration of 0.1mol/L Prepare iron etching solution for iron; soak the activated nickel foam in manganese etching solution for 10 minutes at an ambient temperature of 20°C; then transfer the manganese-etched nickel foam to iron etching solution for 0.5 hours, take out the foam nickel, wash and dry . Finally, the modified nickel foam was directly used as an electrode, and the multi-level array structure nickel foam oxygen evolution electrode material was obtained by in-situ electrochemical activation by constant current method, in which the current density was 1000mA cm ^-2 and the time was 30min. When the current density is 10mA cm ^-2 , the overpotential is 192mV; when the current density is 100mA cm ² , the overpotential is 287mV; when the current density is 1000mA cm ^-2 , the overpotential is 432mV. Under the current density of 200mA cm ^-2 , the overpotential of the material did not increase significantly after testing for 1h.

Example 4

Sonicate the nickel foam in acetone for 30 minutes to remove oil, and clean it with absolute ethanol; then put it in absolute ethanol for 30 minutes, and clean it with ultrapure water; Wash with pure water and set aside; prepare manganese etching solution with a concentration of 1mol/L manganese chloride and 1M hydrochloric acid, and use a concentration of 0.1mol/L ferric chloride, 0.1mol/L ferric nitrate, and 0.1mol/L Prepare iron etching solution with ferric sulfate; soak the activated nickel foam in manganese etching solution for 1 hour at an ambient temperature of 80°C; then transfer the manganese-etched nickel foam to iron etching solution for 5 minutes, remove the foam nickel, wash and dry . Finally, the modified nickel foam was directly used as an electrode, and the multi-level array structure nickel foam oxygen evolution electrode material was obtained by in-situ electrochemical activation by constant voltage method, wherein the voltage was 2.5V (vs. RHE) and the time was 30min. When the current density is 10mA cm ^-2 , the overpotential is 242mV; when the current density is 100mA cm ² , the overpotential is 300mV; when the current density is 1000mA cm ^-2 , the overpotential is 471mV. Under the current density of 100mA cm ^-2 , the overpotential of the material did not increase significantly after testing for 12h.

Example 5

Sonicate the nickel foam in acetone for 30 minutes to remove oil, and clean it with absolute ethanol; then put it in absolute ethanol for 30 minutes, and clean it with ultrapure water; Wash with pure water and wait for use; prepare manganese etching solution with a concentration of 0.5mol/L manganese chloride, 0.5mol/L manganese nitrate, 0.5mol/L manganese sulfate and 0.2M hydrochloric acid, and prepare a manganese etching solution with a concentration of 0.2mol/L L ferric chloride, 0.2mol/L ferric nitrate, 0.2mol/L ferric sulfate configure iron etchant; place the foamed nickel after activation in manganese etchant and soak for 0.5h, ambient temperature 50 ℃; The nickel foam is transferred to the iron etching solution and soaked for 5 minutes, then the nickel foam is taken out, washed and dried. Finally, the modified nickel foam was directly used as an electrode, and in-situ electrochemical activation was performed by linear sweep voltammetry, cyclic voltammetry, constant current method, and constant voltage method to obtain a multi-level array structure nickel foam oxygen evolution electrode material, in which The linear scan interval is 1.0V-1.7V (vs.RHE), the sweep speed is 10mV/s, scan 10 times, the cycle interval is 1.0V-1.7V (vs.RHE), the sweep speed is 20mV/s, and the cycle is 5 laps , wherein the current density is 500 mAcm ^-2 , the time is 10 min, the voltage is 2.0 V (vs. RHE), and the time is 10 min. When the current density is 10mA cm ^-2 , the overpotential is 253mV; when the current density is 100mA cm ² , the overpotential is 314mV; when the current density is 1000mA cm ^-2 , the overpotential is 493mV. Under the current density of 1000mA cm ^-2 , the overpotential of the material did not increase significantly after testing for 12 hours.

The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person familiar with the technical field can easily think of various equivalents within the technical scope disclosed by the present invention. Modifications or replacements shall all fall within the protection scope of the present invention.

The present invention proposes a new method different from the synthesis of traditional foamed nickel-based electrodes from the multi-level array structure nickel foam oxygen evolution electrode material, adopts multi-metal doping and step-by-step etching, and optimizes the multi-level array structure foam nickel oxygen evolution electrode material The optimal synthesis parameters of ^the electrode material can make it have excellent oxygen evolution reaction performance. When the current density is 10mA cm ^-2 , the overpotential of the electrode material is only 208mV; It is only 406mV, and it can work efficiently and stably at a large current density. The electrode prepared by this method can keep the stability for at least 48h under the current density of 1000mA cm ^-2 . At the same time, it was found that in the process of synthesizing foamed nickel oxygen evolution electrode material by etching method, a multi-level array structure can be skillfully formed, and the bubble transfer rate under high current is optimized, which provides a basis for solving the problem of bubble hindering mass transfer under high current. refer to.

It can be seen that the present invention uses an etching method to synthesize the foamed nickel oxygen evolution electrode material with a multi-level array structure, which has complex surface morphology, high oxygen evolution reaction performance, and good electrode stability. The preparation condition is mild, the operation is simple, the time consumption is short, the cost can be greatly reduced, and the method is suitable for industrial production.

It should be noted that the above embodiments only illustrate the technical solutions of the present invention without limitation. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention can be modified or Equivalent replacements without departing from the spirit and scope of the technical solution of the present invention shall be covered by the claims of the present invention.

Claims (10)

1. A preparation method of a foam nickel oxygen evolution electrode material with a multilevel array structure is characterized by comprising the following steps:

(1) Carrying out acid washing activation treatment on the foamed nickel;

(2) Preparing a manganese etching solution by using manganese salt and hydrochloric acid, and preparing an iron etching solution by using ferric salt;

(3) Soaking the activated foam nickel in a manganese etching solution;

(4) Transferring the foamed nickel soaked in the step (3) to an iron etching solution for soaking to obtain modified foamed nickel;

(5) And carrying out in-situ electrochemical activation on the modified foamed nickel to obtain the foamed nickel oxygen evolution electrode material with the multilevel array structure.

2. The preparation method of the foam nickel oxygen evolution electrode material with the multilevel array structure according to claim 1, wherein in the step (2), the manganese salt is one or more of manganese chloride, manganese nitrate and manganese sulfate; the ferric salt is one or more of ferric chloride, ferric nitrate and ferric sulfate.

3. The method for preparing a foam nickel oxygen evolution electrode material with a multilevel array structure according to claim 2, wherein in the step (2), a manganese etching solution is prepared by using a manganese salt with a mass concentration of 0.1-5mol/L and 0.1-1M hydrochloric acid, and an iron etching solution is prepared by using a ferric iron salt with a mass concentration of 0.1-1 mol/L.

4. The method for preparing the foam nickel oxygen evolution electrode material with the multilevel array structure according to claim 1, wherein in the step (3), the activated foam nickel is soaked in a manganese etching solution for 0.1-12h at an ambient temperature of 20-80 ℃.

5. The method for preparing the foam nickel oxygen evolution electrode material with the multilevel array structure according to claim 1, wherein in the step (4), the foam nickel soaked in the step (3) is transferred to an iron etching solution to be soaked for 0.1-2h.

6. The method for preparing a multi-stage array structure foam nickel oxygen evolution electrode material according to claim 1, wherein in the step (5), the electrochemical activation is selected from one or more of linear sweep voltammetry, cyclic voltammetry, galvanostatic method and potentiostatic method.

7. The method for preparing the foam nickel oxygen evolution electrode material with the multilevel array structure according to claim 6, wherein in the step (5), the linear sweep voltammetry and cyclic voltammetry put voltages are in a range of 0-2.5V (vs. RHE), and the sweep or cycle is performed for 1-80 times;

the current density of the constant current method is 10-1500mA cm ^-2 The reaction time is 0.05-3h;

the voltage of the constant voltage method is 1.5-3.5V (vs. RHE), and the reaction time is 0.05-3h.

8. A foam nickel oxygen evolution electrode material with a multilevel array structure obtained by the preparation method according to any one of claims 1 to 7.

9. The multi-stage array structure foam nickel oxygen evolution electrode material as claimed in claim 8, wherein the multi-stage array structure foam nickel oxygen evolution electrode material has the structure: the surface of the foamed nickel is distributed with a nickel-manganese-based small ball array, a nickel-iron-based nanosheet array and a hole structure; the diameter of the nickel-manganese-based small balls is 0.1-0.5 mu m, and the nickel-manganese-based small balls are uniformly distributed to form an array; the length of the nickel manganese base nanometer sheet is 10-100nm, the interval between adjacent nanometer sheets is 10-100nm, and the nickel manganese base nanometer sheets are uniformly distributed to form an array.

10. Use of the nickel foam oxygen evolution electrode material with the multilevel array structure of any one of claims 8 to 9 in oxygen evolution reaction.

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