High-entropy alloy electrode, preparation method and acidic OER application of high-entropy alloy electrode

Abstract

The invention belongs to the technical field of electrocatalyst materials, and provides a high-entropy alloy electrode, a high-entropy alloy comprises at least five of Fe, Co, Ni, Mo, W, Mn and Ir, and a preparation method of the high-entropy alloy electrode comprises the following steps: S1, preparing an electrodeposition solution; s2, adjusting the pH value of the solution in the step S1, and aging at room temperature; s3, the original titanium felt is taken to be subjected to five-step pretreatment procedures of acid pickling, water washing, alcohol washing, water washing and vacuum drying; s4, putting the electrode substrate in the step S3 into the prepared electro-deposition solution, regulating electro-deposition parameters, and then carrying out electro-deposition to obtain a high-entropy alloy electrode material; and S5, pre-oxidizing and annealing the electrode material obtained in the step S4 to obtain the final high-entropy alloy electrode material. According to the method, the deposition rate of the metal elements in the electro-deposition process is regulated and controlled by controlling the concentration of the metal salt in the electro-deposition solution and electro-deposition parameters, and therefore the problem that common and relatively uniform deposition cannot be achieved due to the fact that the potential differences of standard electrodes of different metal elements are large is solved.

Description

Technical Field

[0001] This invention belongs to the field of electrocatalyst materials technology, and particularly relates to a method for preparing a high-entropy alloy electrode and its application. Background Technology

[0002] The increasingly pressing energy crisis and environmental problems strongly demand the development of renewable energy storage and conversion technologies. Hydrogen ( It has the highest energy density Hydrogen, with its clean and renewable properties, is a promising alternative to traditional fossil fuels. Currently, global hydrogen energy primarily consists of "grey hydrogen" produced from fossil fuels, which contradicts the goal of zero emissions. Coupled renewable electricity with water electrolysis to produce decarbonized "green hydrogen" can build a truly clean energy system and is considered the future direction of the hydrogen energy industry. Hydrogen production through water electrolysis mainly involves two half-reactions: the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER), with the OER being the key step limiting the overall reaction rate. To date, alkaline water electrolysis technology for hydrogen production has been well-developed and even commercially viable for industrial applications. While production has progressed, the development of mature proton exchange membrane electrolysis (PEMWE) is still limited by the demanding anodic oxidation environment (low local pH, high anodic potential, and oxygen environment) required for operation in an acidic environment. Currently, iridium ( ) and ruthenium (Ru)-based oxides (such as , Ir black (and Ir black) are the mainstream catalysts for acidic OERs in PEMWE due to their excellent activity and stability. However, Its extremely low abundance in the Earth's crust (approximately 0.001 ppm) results in a high price, making it difficult to reduce the cost of large-scale PEMWE. Furthermore, due to the slow kinetics of acidic OER, high catalyst loadings are typically required to achieve satisfactory electrolysis efficiency. Therefore, highly efficient electrocatalysts with high activity and long-term stability are needed to improve the reaction kinetics of water electrolysis.

[0003] In recent years, although electrocatalytic water electrolysis technology has shown great potential in hydrogen production, its efficiency is limited by the catalytic performance and durability of traditional electrode materials. Against this backdrop, high-entropy alloys (… The unique composition and structure determine its excellent catalytic performance, especially in heterogeneous catalysts. The high mixing configuration entropy of different metal elements at near equimolar concentrations significantly reduces the Gibbs free energy, ensuring the stability of the solid solution phase. This unique microstructure enables high-entropy alloys to exhibit superior overall performance compared to other metallic and non-metallic materials. Due to the unique properties of combining multiple metallic elements, such as the thermodynamic high-entropy effect, the kinetic retarded diffusion effect, the structural lattice distortion effect, and the performance cocktail effect, high-entropy alloy electrodes exhibit excellent electrocatalytic activity and long-term stability in water electrolysis, making them a promising candidate for noble metal catalysts. However, the widespread application of high-entropy alloy electrodes is limited by existing preparation techniques, particularly the shortcomings of electrodeposition technology in controlling the co-deposition of multiple elements, which often leads to inconsistencies in alloy composition and performance. Summary of the Invention

[0004] This invention provides a high-entropy alloy electrode, its preparation method, and its applications, aiming to solve the problems of low efficiency and insufficient durability of traditional electrode materials in electrocatalytic water electrolysis, and to reduce the cost of using precious metals. The high-entropy alloy electrode catalyst of this invention ensures synergistic regulation of stability and catalytic activity. This high-entropy alloy electrode effectively improves the catalytic efficiency of the OER reaction and reduces overall energy consumption by adjusting the electronic structure and adsorption performance through the electronegativity differences between different metal elements; and enhances the electrode's service life and stability through the design and integration of corrosion-resistant elements. Furthermore, the high-entropy alloy electrode preparation method of this invention is specifically designed to overcome the limitations of traditional electrodeposition techniques, ensuring the uniformity and excellent performance of the electrode material, thereby achieving higher gas yields in industrial water electrolysis processes.

[0005] This invention provides a high-entropy alloy electrode, comprising an electrode substrate and a high-entropy alloy attached to the surface of the electrode substrate. The high-entropy alloy contains at least five of the following: Fe, Co, Ni, Mo, W, Mn, and Ir. Fe accounts for 25% to 35% of the atomic percentage of the high-entropy alloy, Co accounts for 25% to 35% of the atomic percentage of the high-entropy alloy, Ni accounts for 10% to 23% of the atomic percentage of the high-entropy alloy, Mo accounts for 10% to 20% of the atomic percentage of the high-entropy alloy, W accounts for 9% to 14% of the atomic percentage of the high-entropy alloy, Mn accounts for 8% to 12% of the atomic percentage of the high-entropy alloy, and Ir accounts for 0.9% to 1.5% of the atomic percentage of the high-entropy alloy.

[0006] This invention also provides a method for preparing a high-entropy alloy electrode, comprising the following steps: S1. Prepare an electrodeposition solution for high-entropy alloy coating using a deionized water solvent; S2. After adjusting the pH of the solution from step S1, age it at room temperature; S3. Take the original titanium felt and perform five pretreatment steps in sequence: acid washing, water washing, alcohol washing, water washing, and vacuum drying to obtain the electrode substrate; S4. Place the electrode substrate obtained in step S3 into the electrodeposition solution obtained in step S2, and perform electrodeposition after adjusting the electrodeposition parameters. S5. The electrode material deposited in step S4 is subjected to pre-oxidation annealing treatment to finally obtain a high-entropy alloy electrode material.

[0007] Preferably, the electrodeposition solution prepared in step S1 comprises at least five soluble metal salts selected from soluble Fe salt, soluble Co salt, soluble Ni salt, soluble Mo salt, soluble W salt, soluble Mn salt, and soluble Ir salt, as well as a soluble ammonium salt, a complexing agent, and a buffer, wherein the concentration of any one of the soluble metal salts is 0.005~0.08 mol / L.

[0008] Preferably, the molar ratio of soluble Fe salt, soluble Co salt, soluble Ni salt, soluble ammonium salt, complexing agent, and buffer in the electrodeposition solution prepared in step S1 is (1-2):(1-2):(2-4):(10-20):(20-40):(2-4).

[0009] Preferably, the soluble ammonium salt includes or The complexing agent comprises any one or at least two of the following, wherein the buffer comprises any one or at least two of the following: boric acid, silicic acid, or acetic acid.

[0010] Preferably, in step S2, the pH of the electrodeposition solution is adjusted to 5.0 to 6.0.

[0011] Preferably, in step S3, the electrode substrate material is microporous titanium felt or ordinary titanium felt, and the pickling solution is... The oxalic acid was washed with anhydrous ethanol and deionized water. The acid washing temperature was 60-80℃, the alcohol washing and water washing temperatures were both 25-40℃, and the vacuum drying temperature was 60-80℃.

[0012] Preferably, the deposition current density in step S4 is The deposition time is 5 to 25 minutes, the electrodeposition temperature is 25 to 60 °C, and the stirring speed is 60 to 120 r / min.

[0013] Preferably, the pre-oxidation annealing temperature in step S5 is 300~800 ℃, the annealing time is 1~4 h, and the heating rate is 5~10 ℃ / min.

[0014] The present invention also provides an application of a high-entropy alloy electrode, which is used as an OER catalyst in acidic water electrolysis via proton exchange membrane.

[0015] Compared with existing technologies, the beneficial effects of this invention are as follows: by employing constant current electrodeposition technology, the deposition rate of metal elements during the electrodeposition process is controlled by adjusting the concentration of metal salts in the electrodeposition solution and the electrodeposition parameters. This solves the problem of the inability to achieve common and relatively uniform deposition of multiple metal elements during the electrodeposition process due to the large differences in the standard electrode potentials of different metal elements. Compared with other self-supporting methods for preparing electrode materials, coatings prepared by constant current electrodeposition are characterized by safe operation, simple equipment, uniform coating morphology, controllable composition, good stability, and good coating adhesion. Therefore, it can fully utilize the high-entropy effect, delayed diffusion effect, lattice distortion effect, and cocktail effect of high-entropy alloys, enabling them to exhibit good electrocatalytic activity and stability in electrocatalytic water electrolysis. Simultaneously, constant current electrodeposition can also improve the utilization rate of metal ions in the electrodeposition solution, reduce electrodeposition time, and improve electrode preparation efficiency, thereby saving electrode preparation costs and making it valuable for application in the electrocatalytic water electrolysis industry. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a flowchart of the preparation method of the high-entropy alloy electrode of the present invention.

[0018] Figure 2 SEM images of the surface morphology of the high-entropy alloy electrode prepared in Example 1.

[0019] Figure 3 EDS image of the elemental distribution on the surface of the high-entropy alloy electrode prepared in Example 1.

[0020] Figure 4 SEM images of the surface morphology of the high-entropy alloy electrode prepared in Example 2.

[0021] Figure 5 EDS image of the elemental distribution on the surface of the high-entropy alloy electrode prepared in Example 2.

[0022] Figure 6 The graph shows the performance test results of the high-entropy alloy electrode prepared in Example 2 on the oxygen evolution reaction at the anode of acidic water electrolysis. Detailed Implementation

[0023] To make the technical solution of this application clearer and more complete, it will be described in detail below with reference to the accompanying drawings and embodiments. It should be noted that the mentioned embodiments are only a part of the numerous embodiments of this application, and not all of them. Based on these embodiments, other embodiments obtained by those skilled in the art without creative effort are also protected by this application.

[0024] The terms "comprising," "having," and their variations, as used in this application, are intended to express a non-exclusive inclusion relationship. For example, if a process, method, system, product, or device comprises a series of steps, operations, components, or modules, this does not mean that it is limited to what has been listed, but may also include other steps, operations, components, or modules not listed, or other related parts inherent in these objects themselves.

[0025] The term "embodiment" in this document indicates that a particular feature, structure, or characteristic described exists in at least one embodiment of this application. The repeated use of this phrase in the specification does not necessarily refer to the same embodiment, and different embodiments are not mutually exclusive, independent, or alternative. Those skilled in the art will explicitly and implicitly understand that the embodiments described herein can be combined with each other. Example 1

[0026] like Figure 1 As shown, an exemplary embodiment of a method for preparing a high-entropy alloy electrode includes the following steps: S1. Prepare the electrodeposition solution for the high-entropy alloy coating by adding 0.01 mol / L... 0.03 mol / L 0.04 mol / L 0.03 mol / L 0.01 mol / L 0.15 mol / L 0.2 mol / L and 0.02 mol / L Dissolve in about 1 L of deionized water to obtain an electrodeposition solution.

[0027] S2. Adjust the pH of the electrodeposition solution from step S1 to 6.0 and age it at room temperature for 12 h.

[0028] S3. Place a 0.4 mm thick ordinary titanium felt at 80 ℃. After sonicating in oxalic acid solution for 30 min, the electrode substrate was transferred to deionized water at 25 °C and sonicated for 5 min. Then it was transferred to anhydrous ethanol at 25 °C and sonicated for 5 min. Finally, the ordinary titanium felt was transferred to a vacuum drying oven at 60 °C and dried for 2 h to obtain the electrode substrate.

[0029] S4. The electrode substrate obtained in step S3 is removed and transferred to the electrodeposition solution obtained in step S2 for electrodeposition. The deposition current density is... The deposition time was 12 min, the electrodeposition temperature was 25℃, and the stirring speed was 100 r / min.

[0030] S5. The electrode material deposited in step S4 is placed in a muffle furnace at 800 ℃ for pre-oxidation annealing treatment. The annealing time is 1 h and the programmed heating rate is 10 ℃ / min. Finally, an electrode with a pentagonal high-entropy alloy coating is obtained, wherein Fe accounts for 33.3% of the atomic percentage of the high-entropy alloy, Co accounts for 26.7% of the atomic percentage of the high-entropy alloy, Ni accounts for 11.6% of the atomic percentage of the high-entropy alloy, Mo accounts for 19.2% of the atomic percentage of the high-entropy alloy, and W accounts for 9.2% of the atomic percentage of the high-entropy alloy.

[0031] The surface morphology of the high-entropy alloy electrode prepared in this embodiment is as follows: Figure 2 As shown, the high-entropy alloy coating is densely and uniformly distributed on a 0.4 mm ordinary titanium felt substrate.

[0032] The elemental distribution of the high-entropy alloy electrode prepared in this embodiment is as follows: Figure 3 As shown, the elements are uniformly distributed on the surface of the titanium felt matrix, and different elements appear in the same area with a high degree of overlap, which means that the high-entropy alloy has been successfully prepared. Example 2

[0033] like Figure 1 As shown, an exemplary embodiment of a method for preparing a high-entropy alloy electrode includes the following steps: S1. Prepare the electrodeposition solution for the high-entropy alloy coating; add 0.02 mol / L 0.02 mol / L 0.02 mol / L 0.02 mol / L 0.02 mol / L 0.005 mol / L 0.1 mol / L 0.2 mol / L and 0.015 mol / L Dissolve in about 1 L of deionized water to obtain an electrodeposition solution.

[0034] S2. After adjusting the pH of the electrodeposition solution described in step S1 to 5.0, the electrodeposition solution is aged at room temperature for 12 h.

[0035] S3. Place a 0.4 mm thick microporous titanium felt at 75 °C. The electrode substrate was ultrasonicated in oxalic acid solution for 30 min, then transferred to deionized water at 35°C and ultrasonicated for 5 min, then transferred to anhydrous ethanol at 35°C and ultrasonicated for 5 min, then transferred to deionized water at 35°C and ultrasonicated for 5 min, and finally transferred to a vacuum drying oven at 80°C and dried for 1 h to obtain the electrode substrate.

[0036] S4. The electrode substrate obtained in step S3 is removed and transferred to the electrodeposition solution obtained in step S2 for electrodeposition. The deposition current density is... The deposition time was 12 min, the electrodeposition temperature was 35℃, and the stirring speed was 100 r / min.

[0037] S5. The electrode material deposited in step S4 is placed in a muffle furnace at 600 ℃ for pre-oxidation annealing treatment. The annealing time is 2 h and the programmed heating rate is 5 ℃ / min. Finally, an electrode with a hexa-element high-entropy alloy coating is obtained, wherein Fe accounts for 25.4% of the atomic percentage of the high-entropy alloy, Co accounts for 28.1% of the atomic percentage of the high-entropy alloy, Ni accounts for 21.4% of the atomic percentage of the high-entropy alloy, Mo accounts for 14.6% of the atomic percentage of the high-entropy alloy, W accounts for 9.1% of the atomic percentage of the high-entropy alloy, and Ir accounts for 1.4% of the atomic percentage of the high-entropy alloy.

[0038] The surface morphology of the high-entropy alloy electrode prepared in this embodiment is as follows: Figure 4 As shown, the high-entropy alloy coating is densely and uniformly distributed on the 0.4 mm microporous titanium felt substrate.

[0039] The elemental distribution of the high-entropy alloy electrode prepared in this embodiment is as follows: Figure 5 As shown, the elements are uniformly distributed on the surface of the titanium felt matrix, and different elements appear in the same area with a high degree of overlap, which means that the high-entropy alloy has been successfully prepared.

[0040] This embodiment achieves the co-deposition of catalytically active metal elements in a high-entropy alloy. By adding inactive elements, the electronic structure of the catalytically active metal elements is modulated, achieving a synergistic effect and optimizing the electrocatalytic hydrolysis performance of the high-entropy alloy. Simultaneously, the prepared coating exhibits uniform and intact morphology, homogeneous composition, good stability, and strong adhesion.

[0041] The FeCoNiMoWIr high-entropy alloy electrode prepared in this embodiment was applied to acidic water electrolysis. Figure 6 The results show the oxygen evolution reaction performance of the high-entropy alloy electrode prepared by the above method as the anode in acidic water electrolysis. Figure 6It can be seen that in the oxygen evolution reaction test, the FeCoNiMoWIr high-entropy alloy electrode... At the specified current density, the potential can reach 294 mV, meeting industrial application standards. Using this method, the efficiency of water electrolysis can be significantly improved, thereby reducing the amount of Ir used in commercial precious metal Ir catalysts. Example 3

[0042] like Figure 1 As shown, an exemplary embodiment of a method for preparing a high-entropy alloy electrode includes the following steps: S1. Take 0.01 mol / L 0.02 mol / L 0.04 mol / L 0.03 mol / L 0.08 mol / L 0.005 mol / L 0.08 mol / L 0.25 mol / L and 0.01 mol / L Dissolve it in about 1 L of deionized water to prepare an electrodeposition solution.

[0043] S2. After adjusting the pH of the electrodeposition solution described in step S1 to 5.0, the electrodeposition solution is aged at room temperature for 12 h.

[0044] S3. Place a 0.4 mm thick microporous titanium felt into a container at 60 °C. The electrode substrate was ultrasonicated in oxalic acid solution for 30 min, then transferred to deionized water at 40 °C and ultrasonicated for 5 min, then transferred to anhydrous ethanol at 40 °C and ultrasonicated for 5 min, then transferred to deionized water at 40 °C and ultrasonicated for 5 min, and finally transferred to a vacuum drying oven at 70 °C and dried for 2 h to obtain the electrode substrate.

[0045] S4. The electrode substrate obtained in step S3 is removed and transferred to the electrodeposition solution prepared in step S2 for electrodeposition. The deposition current density is... The deposition time was 15 min, the electrodeposition temperature was 45℃, and the stirring speed was 60 r / min.

[0046] S5. The electrode material deposited in step S4 is placed in a muffle furnace at 300 °C for pre-oxidation annealing treatment. The annealing time is 4 h and the programmed heating rate is 5 °C / min. Finally, an electrode with a high-entropy alloy coating is obtained, wherein Fe accounts for 26.8% of the atomic percentage of the high-entropy alloy, Co accounts for 33.6% of the atomic percentage of the high-entropy alloy, Ni accounts for 16.2% of the atomic percentage of the high-entropy alloy, Mo accounts for 11.6% of the atomic percentage of the high-entropy alloy, W accounts for 10.5% of the atomic percentage of the high-entropy alloy, and Ir accounts for 1.3% of the atomic percentage of the high-entropy alloy. Example 4

[0047] like Figure 1 As shown, an exemplary embodiment of a method for preparing a high-entropy alloy electrode includes the following steps: S1. Adding 0.02 mol / L... 0.02 mol / L 0.04 mol / L 0.4 mol / L 0.1 mol / L 0.05 mol / L 0.3 mol / L and 0.02 mol / L Dissolve in about 1 L of deionized water to prepare an electrodeposition solution.

[0048] S2. After adjusting the pH of the electrodeposition solution prepared in step S1 to 6.0, age it at room temperature for 12 h.

[0049] S3. Place a 0.25 mm thick ordinary titanium felt at 80 ℃. The electrode substrate was ultrasonicated in oxalic acid solution for 30 min, then transferred to deionized water at 25 °C and ultrasonicated for 5 min, then transferred to anhydrous ethanol at 25 °C and ultrasonicated for 5 min, then transferred to deionized water at 25 °C and ultrasonicated for 5 min, and finally transferred to a vacuum drying oven at 60 °C and dried for 2 h to obtain the electrode substrate.

[0050] S4. The electrode substrate obtained in step S3 is removed and transferred to the electrodeposition solution prepared in step S2 for electrodeposition. The deposition current density is... The deposition time was 8 min, the electrodeposition temperature was 60℃, and the stirring speed was 120 r / min.

[0051] S5. The electrode material deposited in step S4 is placed in a muffle furnace at 500 °C for pre-oxidation annealing treatment. The annealing time is 3 h and the programmed heating rate is 5 °C / min. Finally, an electrode with a high-entropy alloy coating is obtained, wherein Fe accounts for 29.3% of the atomic percentage of the high-entropy alloy, Co accounts for 25.6% of the atomic percentage of the high-entropy alloy, Ni accounts for 22.7% of the atomic percentage of the high-entropy alloy, Mn accounts for 9.8% of the atomic percentage of the high-entropy alloy, and W accounts for 12.6% of the atomic percentage of the high-entropy alloy.

[0052] The above description is a preferred embodiment of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. A high-entropy alloy electrode, characterized by, The electrode body and high-entropy alloy attached to the surface of the electrode body are included, and the high-entropy alloy contains at least five of Fe, Co, Ni, Mo, W, Mn and Ir, wherein Fe accounts for 25-35% of the atomic percentage of the high-entropy alloy, Co accounts for 25-35% of the atomic percentage of the high-entropy alloy, Ni accounts for 10-23% of the atomic percentage of the high-entropy alloy, Mo accounts for 10-20% of the atomic percentage of the high-entropy alloy, W accounts for 9-14% of the atomic percentage of the high-entropy alloy, Mn accounts for 8-12% of the atomic percentage of the high-entropy alloy, and Ir accounts for 0.9-1.5% of the atomic percentage of the high-entropy alloy.

2. A method of preparing the high-entropy alloy electrode according to claim 1, characterized by, The method comprises the following steps: S1. Using deionized water as a solvent to prepare an electrodeposition solution for high-entropy alloy coating preparation; S2. Adjusting the pH of the solution in step S1 and then aging at room temperature; S3. Taking a raw titanium felt, and sequentially performing five pretreatments of acid washing, water washing, alcohol washing, water washing and vacuum drying to obtain an electrode body; S4. Placing the electrode body obtained in step S3 in the electrodeposition solution obtained in step S2, and then performing electrodeposition after adjusting electrodeposition parameters; S5. Performing pre-oxidation annealing treatment on the electrode material after deposition in step S4 to finally obtain a high-entropy alloy electrode material.

3. The method of claim 2, wherein the high-entropy alloy electrode is prepared by a process comprising: The electrodeposition solution configured in step S1 contains at least five kinds of soluble metal salts of soluble Fe salt, soluble Co salt, soluble Ni salt, soluble Mo salt, soluble W salt, soluble Mn salt and soluble Ir salt, and soluble ammonium salt, complexing agent and buffer, wherein the concentration of any kind of soluble metal salt is 0.005-0.08 mol / L.

4. The method of claim 2, wherein the high-entropy alloy electrode is prepared by a process comprising: The molar ratio of the soluble Fe salt, soluble Co salt, soluble Ni salt, soluble ammonium salt, complexing agent and buffer in the electrodeposition solution configured in step S1 is (1-2):(1-2):(2-4):(10-20):(20-40):(2-4).

5. The method of claim 3, wherein the high-entropy alloy electrode is prepared by a process comprising: The soluble ammonium salt includes any one or a combination of at least two of (NH4)2SO4 or NH4Cl, the complexing agent includes citrate, and the buffer includes any one or a combination of at least two of boric acid, silicic acid or acetic acid.

6. The method of claim 2, wherein the high-entropy alloy electrode is prepared by a process comprising: The pH value of the electrodeposition solution is adjusted to 5.0-6.0 in step S2.

7. The method of claim 2, wherein the high-entropy alloy electrode is prepared by a process comprising: The electrode body material in step S3 is microporous titanium felt or ordinary titanium felt, the acid washing solution is 5-10 wt.% oxalic acid, the alcohol washing solution is anhydrous ethanol, the water washing solution is deionized water, the acid washing temperature is 60-80 ℃, the alcohol washing and water washing temperatures are both 25-40 ℃, and the vacuum drying temperature is 60-80 ℃.

8. The method of claim 2, wherein the high-entropy alloy electrode is prepared by a process comprising: The deposition current density of the step S4 is 60 ~ 160 mA / cm 2 , the deposition time is 5 ~ 25 min, the electrodeposition temperature is 25 ~ 60 ℃, and the stirring speed is 60 ~ 120 r / min.

9. The method of claim 2, wherein the high-entropy alloy is prepared by a process comprising: The pre-oxidation annealing temperature in step S5 is 300-800 ℃, the annealing time is 1-4 h, and the temperature rising rate is 5-10 ℃ / min.

10. Use of a high-entropy alloy electrode, characterized in that, The high-entropy alloy electrode of any one of claims 1-9 is used as an OER catalyst in proton exchange membrane acidic electrolytic water.

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