Three-dimensional integrated electrode, preparation method and application thereof

Abstract

This invention discloses a three-dimensional integrated electrode, its preparation method, and its application, comprising the following steps: S1: Dissolving ruthenium salt, cobalt salt, and nickel salt in deionized water to prepare an electrolyte; S2: Placing the electrolyte prepared in step S1 in a magnetic field and immersing a porous substrate in it, then performing electrodeposition at a constant potential, and drying at a constant temperature to obtain a directionally grown ruthenium-cobalt-nickel catalytic electrode; S3: Partially immersing the directionally grown ruthenium-cobalt-nickel catalytic electrode obtained in step S2 in a hydrophobic material solution, constructing a hydrophobic layer on the electrode surface by immersion, and finally obtaining a three-dimensional integrated electrode. The preparation method of this invention is simple and easy to operate; the materials used are inexpensive; the solvents used are deionized water and ethanol, which are green and environmentally friendly, and suitable for subsequent industrial production.

Description

Technical Field

[0001] This invention belongs to the field of three-dimensional integrated electrode technology, and in particular relates to a three-dimensional integrated electrode, its preparation method and application. Background Technology

[0002] Faced with the global energy crisis and increasing ecological and environmental pressures, building a clean, low-carbon, safe, and efficient modern energy system has become an urgent priority. The massive consumption of traditional fossil fuels has led to resource scarcity and triggered a series of severe challenges, including environmental pollution. Against this backdrop, hydrogen energy, with its high energy density and zero carbon emissions, holds immense potential as a future alternative to fossil fuels. Electrochemical water splitting for hydrogen production is one of the core pathways to achieving large-scale, low-carbon production of green hydrogen. Among numerous water electrolysis technologies, anion exchange membrane (AEM) water electrolysis combines the advantages of alkaline and proton exchange membrane water electrolysis, offering high electrolysis efficiency, fast response, and low cost. It has become a current research hotspot in water electrolysis for hydrogen production, with electrode design being crucial. In particular, the oxygen evolution reaction (OER) at the anode involves a complex four-electron process, and its slow kinetics and high overpotential limit the efficiency of water electrolysis. Therefore, developing high-performance, durable anodes is essential for AEM water electrolysis technology.

[0003] Traditional AEM electrolyzer electrodes consist of two parts: a catalyst layer (CL) and a gas diffusion layer (GDL). The CL is composed of particulate catalysts bonded together by a polymer, while the GDL is typically a conductive porous material such as nickel foam or carbon cloth. This structure has the following drawbacks: (1) The dense CL reduces the active surface area of ​​the catalyst and affects the transport of electrolyte and gaseous products, thus reducing catalyst utilization; (2) The electron transfer efficiency between the CL and GDL is poor, increasing contact resistance; (3) The polymer binder has poor conductivity, increasing ohmic resistance; (4) The large number of bubbles generated during catalysis may cause the catalyst to detach from the substrate surface, reducing the stability of the electrolyzer.

[0004] However, current research on water electrolysis technology focuses on developing efficient and stable OER catalysts. Although some progress has been made in the research of self-supporting electrodes based on nickel foam and carbon cloth, existing research mainly focuses on the catalytic materials themselves, neglecting the interface design between CL and GDL. The catalytically active components often completely encapsulate the substrate, requiring additional GDL components in practical applications, which leads to a significant decrease in catalytic performance in real systems. Based on the above discussion, developing novel electrode structures to overcome the shortcomings of traditional electrodes is a crucial issue that urgently needs to be addressed. Summary of the Invention

[0005] In view of this, the present invention proposes a three-dimensional integrated electrode, its preparation method and application, to solve at least one technical problem in the background art.

[0006] To achieve the above objectives, the technical solution of the present invention is implemented as follows:

[0007] A method for fabricating a three-dimensional integral electrode includes the following steps:

[0008] S1: Dissolve ruthenium salt, cobalt salt, and nickel salt in deionized water to obtain the electrolyte;

[0009] S2: The electrolyte obtained in step S1 is placed in a magnetic field and the porous substrate is immersed in it. Then, electrodeposition is performed at a constant potential. The porous substrate is removed and placed in an oven for constant temperature drying to obtain a directionally grown ruthenium cobalt nickel catalytic electrode.

[0010] S3: Immerse the directionally grown ruthenium cobalt nickel catalytic electrode obtained in step S2 into a hydrophobic material solution. By immersing it on the electrode surface, a hydrophobic layer is constructed, and finally a three-dimensional integrated electrode is obtained.

[0011] Furthermore, the ruthenium salt, cobalt salt, and nickel salt in step S1 are all metal ion source compounds that are soluble in water or solvents;

[0012] Preferably, the ruthenium salt is selected from ruthenium trichloride hydrate, or ruthenium nitrate, ruthenium sulfate, ruthenium acetate, and the above-mentioned ruthenium salt hydrates;

[0013] Preferably, the cobalt salt is selected from cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, or hydrates of the above cobalt salts;

[0014] Preferably, the nickel salt is selected from nickel chloride, nickel nitrate, nickel sulfate, nickel acetate, or hydrates of the above nickel salts.

[0015] Furthermore, in step S1, the ruthenium salt is ruthenium trichloride hydrate, the cobalt salt is cobalt chloride or its hydrate, and the nickel salt is nickel chloride or its hydrate;

[0016] The molar ratio of ruthenium ions, nickel ions, cobalt ions to deionized water in the electrolyte is 1:(9~11):(9~11):(5000~6000), preferably 1:(9~11):(9~11):(5300~5700).

[0017] Furthermore, the magnetic field strength in step S2 is 0.9~0.11 T, and the magnetic field direction is perpendicular to the substrate surface.

[0018] Furthermore, the electrodeposition potential in step S2 is -0.6 to -0.9 V, preferably -0.7 to -0.8 V, and the deposition time is 25 to 35 min.

[0019] Furthermore, the porous substrate in step S2 is one of nickel foam, titanium foam, stainless steel mesh, copper foam, nickel fiber felt, or carbon cloth, preferably nickel foam.

[0020] Furthermore, the hydrophobic material in step S2 is an ethanol solution of trans-cinnamic acid with a concentration of 0.25~0.30 mol / L. -1 Soaking time is 2-3 hours.

[0021] Furthermore, the thickness of the hydrophobic layer formed in step S3 accounts for 0.6 to 0.9 of the thickness of the porous substrate, preferably 0.7 to 0.8.

[0022] The three-dimensional integrated electrode is prepared by the above-mentioned method.

[0023] The aforementioned three-dimensional integrated electrode is used as the anode for electrocatalytic water splitting in the oxygen evolution reaction in alkaline media.

[0024] Preferably, the alkaline medium is 1 mol L. -1 A potassium hydroxide solution.

[0025] In this invention, the electrodeposition solution uses ruthenium trichloride hydrate, nickel chloride or its hydrate, cobalt chloride or its hydrate, and deionized water as the solvent. By controlling parameters such as electrodeposition potential and time, a catalyst film can be deposited on the surface of a porous support. During the electrodeposition process, the introduction of a magnetic field can promote the deposition of metal ions along their easy magnetization axis, exposing lower-energy crystal planes, thereby obtaining electrocatalytic materials with preferred orientation growth. Based on this, the electrode portion is immersed in a trans-cinnamic acid solution. Utilizing the bridging effect of nickel, a hydrophobic layer is introduced onto the surface of the electrocatalytic material. The thickness of the hydrophobic layer relative to the entire electrode can be controlled by the immersion height in the solution, thus obtaining a three-dimensional integrated electrode. When applied to water electrolysis, the portion not covered by the hydrophobic layer can serve as an OER catalyst layer, while the portion with the hydrophobic layer can serve as a gas diffusion layer, promoting bubble transport. The combined effect of both improves the efficiency of the water electrolysis reaction.

[0026] Compared with existing technologies, the three-dimensional integrated electrode, its preparation method, and its application described in this invention have the following advantages:

[0027] (1) The three-dimensional integrated electrode prepared in this invention has a three-dimensional porous substrate with good conductivity, which can ensure the efficient transport of electrons and matter. The magnetic field can induce ruthenium and cobalt tetroxide to expose the (101) and (220) crystal planes with lower energy, which is beneficial to optimize the adsorption energy of intermediate products in OER, reduce the reaction energy barrier, and improve the stability of ruthenium. The three-dimensional integrated electrode structure with the catalyst layer and the gas diffusion layer synergistically coupled can effectively reduce the resistance to electron and matter transport during the electrochemical reaction and improve the reaction kinetics. Therefore, as an OER electrocatalyst and an anode of AEM water electrolysis technology, it can significantly improve the efficiency and durability of water electrolysis.

[0028] (2) The preparation method of the present invention is simple and easy to operate; the materials used are inexpensive; the solvents used are deionized water and ethanol, which are green and environmentally friendly and suitable for subsequent industrial production. Attached Figure Description

[0029] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings:

[0030] Figure 1 The image shows a scanning electron microscope (SEM) image of the Ru-CoNi / NF catalytic electrode obtained in Example 1.

[0031] Figure 2 The Ru-CoNi / NF@HL obtained in Example 1 0.75 SEM image of a three-dimensional integrated electrode;

[0032] Figure 3 The Ru-CoNi / NF@HL obtained in Example 1 0.75 X-ray diffraction (XRD) pattern of Ru-CoNi / NF;

[0033] Figure 4 The Ru-CoNi / NF obtained in Example 1 0.75 OER polarization curves of @HL and Ru-CoNi / NF@HL, Ru-CoNi / NF, Ru-Co / NF, Ru-Ni / NF and IrO2 / NF;

[0034] Figure 5 The Ru-CoNi / NF@HL prepared in Example 1 0.75 The complete water electrochemical voltage-ampere curve as the anode;

[0035] Figure 6 Ru-CoNi / NF@HL prepared in Example 1 0.75 Figure showing the results of the total water electrolysis stability test as the anode;

[0036] Figure 7 The OER polarization curve of the electrode prepared in Comparative Example 1 is shown.

[0037] Figure 8 The OER polarization curves of the electrodes prepared in Comparative Examples 2 and 3 are shown.

[0038] Figure 9 The OER polarization curves of the electrodes prepared in Comparative Examples 4 and 5 are shown. Detailed Implementation

[0039] It should be noted that, unless otherwise specified, the embodiments and features described in the present invention can be combined with each other.

[0040] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0041] Example 1

[0042] The three-dimensional monolithic electrode prepared in this embodiment uses Ru-CoNi / NF@HL. 0.75 The term is a code name, where Ru-CoNi is the catalyst name, NF represents the nickel foam substrate, HL represents the hydrophobic layer, and 0.75 indicates that the thickness of the hydrophobic layer accounts for 0.75% of the total thickness of the substrate.

[0043] 1. Material preparation

[0044] (1) 0.0654 g of ruthenium trichloride trihydrate (RuCl3·3H2O), 0.325 g of cobalt chloride (CoCl2) and 0.594 g of nickel chloride hexahydrate (NiCl2·6H2O) were dissolved in 25 mL of deionized water to prepare an electrolyte; the molar ratio of ruthenium ions, nickel ions, cobalt ions and deionized water was 1:10:10:5556. Then HCl was added to adjust the pH of the solution to 1 to prepare the electrolyte.

[0045] (2) The prepared electrolyte was placed in a magnetic field with a magnetic field strength of 0.1 T, and then the pretreated nickel foam was immersed in the solution and placed perpendicular to the magnetic field line. Next, electrodeposition was performed at a constant potential of -0.75 V. After deposition for 30 min, the NF substrate was taken out and placed in an oven at 60 °C for constant temperature drying to obtain Ru-CoNi / NF catalytic electrode.

[0046] (3) Weigh 1 g of trans-cinnamic acid and dissolve it in 25 mL of solution (molar concentration of 0.27 mol L). -1The Ru-CoNi / NF catalytic electrode was then partially immersed in an ethanol solution of trans-cinnamic acid to prepare a hydrophobic layer. The immersion time was 2 hours, depending on the desired thickness (0.75% in this example), to form the hydrophobic layer. This resulted in a three-dimensional integrated electrode with the hydrophobic layer partially coated with Ru-CoNi / NF, namely Ru-CoNi / NF@HL. 0.75 .

[0047] 2.Ru-CoNi / NF@HL 0.75 As a self-supporting anode for water electrolysis

[0048] Electrocatalytic performance testing was conducted using a CHI760E electrochemical workstation with a 1 mol L electrolyte. -1 A potassium hydroxide solution with an effective electrode area of ​​1 cm². 2 The OER test employed a three-electrode system, with Ag / AgCl, a carbon rod, and Ru-CoNi / NF@HL as the reference, counter, and working electrodes, respectively. 0.75 The scan rate of the linear sweep voltammetry is 10 mV / s. -1 The electrode potentials are all converted to the reversible hydrogen electrode potential (RHE) according to the following formula:

[0049] E RHE =E(Ag / AgCl)+0.0591*pH+0.197 V;

[0050] E(Ag / AgCl) is the voltage actually measured relative to the Ag / AgCl electrode as a reference electrode, 0.197 V is the standard potential of the Ag / AgCl reference electrode used, and pH is the acidity or alkalinity of the electrolyte used.

[0051] In the OER test, Ru-CoNi / NF (without hydrophobic layer), Ru-CoNi / NF@HL (substrate completely encapsulated by hydrophobic layer), Ru-Co / NF, Ru-Ni / NF and IrO2 / NF (commercial electrode) were used for comparison.

[0052] The water splitting performance was evaluated using a dual-electrode system, Ru-CoNi / NF@HL. 0.75 Using a commercially available Pt / C electrode as the anode and a commercially available IrO2 and Pt / C electrode as the cathode, and using a system with commercially available IrO2 and Pt / C as both anode and cathode as a control, at 10 mV s -1 The catalyst was tested and its overall water-splitting stability was investigated using the constant current method.

[0053] Figure 1 This is a SEM image of the Ru-CoNi / NF prepared in this embodiment. As can be seen, dense and uniform nanoparticles cover the NF substrate.

[0054] Figure 2 The Ru-CoNi / NF@HL prepared in this embodiment 0.75 The SEM image shows that a transparent thin film, i.e., a hydrophobic layer, covers the nanoparticle layer.

[0055] Figure 3 The image shows the XRD pattern of Ru-CoNi / NF prepared in this embodiment. The figure clearly shows characteristic peaks for Ni and Ru, while the position of the characteristic peak for Co3O4 is shifted, presumably due to its co-deposition with Ni and Ru. This indicates that the prepared material is a composite of Ni, Ru, and Co3O4. Calculations revealed that the Ru crystal growth orientation tends towards the (002) crystal plane (with an orientation index of 1.5), while the Co3O4 growth orientation tends towards the (220) crystal plane (with an orientation index of 2.2). This is because the magnetic field tends to induce exposure of crystal planes with lower energy, and the (002) and (220) crystal planes are the lowest surface energies for Ru and Co3O4 crystals, respectively. Furthermore, the hydrophobic layer coating did not alter the crystal structure of the catalytic material itself.

[0056] Figure 4 The Ru-CoNi / NF@HL prepared in this embodiment 0.75 The OER test results for Ru-CoNi / NF@HL, Ru-CoNi / NF, Ru-Co / NF, Ru-Ni / NF, and commercial IrO2 / NF are also shown. As can be seen from the figure, compared with Ru-CoNi / NF@HL, Ru-CoNi / NF, Ru-Co / NF, Ru-Ni / NF, and commercial IrO2 / NF catalysts, Ru-CoNi / NF@HL... 0.75 At 100 mAcm -2 The overpotential was the smallest (97.4 mV), indicating that Ru-CoNi / NF 0.75 @HL has the best OER performance.

[0057] Figure 5 and Figure 6 The Ru-CoNi / NF@HL prepared in this embodiment 0.75 Performance diagram when used as a total water-splitting anode. (From...) Figure 5 It can be seen that Ru-CoNi / NF@HL 0.75 It can drive water electrolysis to 500 mA cm⁻¹ at 1.68 V. -2 It outperforms the performance of the commercial Pt / CiIrO2 system (1.98 V); by Figure 7 It can be seen that Ru-CoNi / NF@HL 0.75 At 500 mA cm -2It can maintain the stability of water electrolysis for more than 1000 hours under high current density, showing its potential for practical application.

[0058] Example 2:

[0059] The preparation process was the same as in Example 1, except that the amount of deionized water was 23.8 mL, the molar ratio of ruthenium ions, nickel ions, cobalt ions, and deionized water in the electrolyte was 1:10:10:5300, and the electrodeposition potential was -0.7 V. Other steps were the same as in Example 1. The electrochemical performance testing process for the prepared electrocatalytic material was also the same as in Example 1. The results showed that when the prepared electrode was used as the anode in the total water splitting system, it could drive water electrolysis to 500 mAcm at 1.72 V. -2 It outperforms commercial Pt / C‖IrO2 and can maintain water electrolysis stability for more than 1000 h at this current density.

[0060] Example 3:

[0061] The preparation process differs from Example 1 in that the amount of deionized water in the solvent is 25.6 mL, the molar ratio of ruthenium ions, nickel ions, cobalt ions, and deionized water in the electrolyte is 1:10:10:5700, and the electrodeposition potential is -0.8 V. Other steps are the same as in Example 1. The electrochemical performance testing process for the prepared electrocatalytic material is the same as in Example 1. The results show that when the prepared electrode is used as the anode in the total water splitting system, it can drive water electrolysis to 500 mA cm⁻¹ at 1.70 V. -2 Furthermore, it can maintain the stability of electrolyzed water for more than 1000 hours at this current density.

[0062] Comparative Example 1

[0063] The preparation process is the same as in Example 1, except that no magnetic field is applied during the preparation process. Figure 7 As shown, the prepared electrode at 100 mA cm⁻¹ -2 The overpotential of OER under these conditions is 304.1 mV, which is far greater than that of Ru-CoNi / NF@HL. 0.75 The overpotential indicates that its catalytic activity is not as good as the electrocatalytic material prepared in Example 1.

[0064] Comparative Example 2

[0065] The preparation process is the same as in Example 1, except that the deposition potential is -0.5 V during the preparation process. Figure 8 As shown, the prepared electrode is at 100 mA cm⁻¹ -2 The overpotential was 343.2 mV, indicating that its catalytic activity was not as good as the electrocatalytic material prepared in Example 1.

[0066] Comparative Example 3

[0067] The preparation process was the same as in Example 1, except that the deposition potential was -0.95 V during the preparation process. Figure 8 As shown, the prepared electrode is at 100 mA cm⁻¹ -2 The OER overpotential was 349.0 mV, indicating that its catalytic activity was not as good as that of the electrocatalytic material prepared in Example 1.

[0068] Comparative Example 4

[0069] The preparation process is the same as in Example 1, except that the proportion of the hydrophobic layer thickness is 0.5. Figure 9 As shown, the prepared Ru-CoNi / NF@HL 0.5 Electrode at 100 mA cm -2 The OER overpotential was 194.9 mV, indicating that its catalytic activity was not as good as the electrocatalytic material prepared in Example 1.

[0070] Comparative Example 5

[0071] The preparation process is the same as in Example 1, except that the proportion of the hydrophobic layer to the total thickness is 0.95. Figure 9 As shown, the prepared Ru-CoNi / NF@HL 0.95 Electrode at 100 mA cm -2 The OER overpotential was 305.4 mV, indicating that its catalytic activity was not as good as the electrocatalytic material prepared in Example 1.

[0072] Ru-CoNi / NF@HL obtained in Example 1 0.75 The highly conductive three-dimensional porous substrate ensures efficient electron and mass transport; the uniform nanoparticle catalyst guarantees sufficient exposure of active sites and the release and transport of gaseous products; the introduction of a magnetic field induces the exposure of low-energy crystal planes, which is crucial for optimizing the adsorption energy of hydrogen / oxygen intermediates in the electrochemical process; the introduction of a hydrophobic layer gives this integrated electrode hydrophilic-hydrophobic coupling properties, which is beneficial for OER and bubble transport; the integrated design reduces the mass transfer resistance at the catalyst layer and gas diffusion layer interface, promoting the effective release of gaseous products. Therefore, Ru-CoNi / NF@HL 0.75 Self-supported OER electrocatalysts can significantly improve water electrolysis efficiency and stability, which is evident in... Figures 4-6 The electrochemical performance was confirmed as shown. When Ru-CoNi / NF@HL was used as the anode for total water electrolysis, water electrolysis could be driven to 500 mA cm⁻¹ at 1.68 V. -2It outperforms commercially available Pt / C‖IrO2 and can achieve performance at 500 mA cm⁻¹ -2 It maintains the stability of electrolyzed water for more than 1000 hours under high current density.

[0073] This invention provides a method for preparing a three-dimensional integrated electrode and its application. The method utilizes magnetic field-assisted electrodeposition technology to prepare a preferentially oriented ruthenium-cobalt-nickel catalytic electrode on a porous substrate. Then, the resulting electrode is partially modified with a hydrophobic material to construct a three-dimensional integrated electrode coupling a catalyst layer and a gas diffusion layer. The magnetic field can induce the exposure of lower-energy crystal planes of the metal or metal oxide during electrocatalysis, which is beneficial for optimizing the adsorption energy of intermediate products in the oxygen evolution reaction (OER) and reducing the reaction energy barrier. The catalyst layer catalyzes the OER, while the hydrophobic material-modified portion acts as a gas diffusion layer to promote bubble transport. The integrated design significantly improves reaction kinetics, promotes the effective release of bubbles, and thus improves the catalytic reaction efficiency. Based on these advantages, the electrode material prepared by this invention exhibits good catalytic activity and stability, demonstrating excellent industrialization potential.

[0074] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for fabricating a three-dimensional integrated electrode, characterized in that: Includes the following steps: S1: Dissolve ruthenium salt, cobalt salt, and nickel salt in deionized water to obtain the electrolyte; S2: The electrolyte obtained in step S1 is placed in a magnetic field and the porous substrate is immersed in it. Then, electrodeposition is performed at a constant potential, and the directionally grown ruthenium cobalt nickel catalytic electrode is obtained after constant temperature drying. S3: Immerse the directionally grown ruthenium cobalt nickel catalytic electrode obtained in step S2 into a hydrophobic material solution. By immersing it on the electrode surface, a hydrophobic layer is constructed, and finally a three-dimensional integrated electrode is obtained.

2. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: The ruthenium salt, cobalt salt, and nickel salt in step S1 are all metal ion source compounds that are soluble in water or solvents; Preferably, the ruthenium salt is selected from ruthenium trichloride hydrate, or ruthenium nitrate, ruthenium sulfate, ruthenium acetate, and the above-mentioned ruthenium salt hydrates; Preferably, the cobalt salt is selected from cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, or hydrates of the above cobalt salts; Preferably, the nickel salt is selected from nickel chloride, nickel nitrate, nickel sulfate, nickel acetate, or hydrates of the above nickel salts.

3. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: In step S1, the ruthenium salt is ruthenium trichloride hydrate, the cobalt salt is cobalt chloride or its hydrate, and the nickel salt is nickel chloride or its hydrate. The molar ratio of ruthenium ions, nickel ions, cobalt ions to deionized water in the electrolyte is 1:(9~11):(9~11):(5000~6000), preferably 1:(9~11):(9~11):(5300~5700).

4. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: The magnetic field strength in step S2 is 0.9~0.11 T, and the magnetic field direction is perpendicular to the substrate surface.

5. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: The electrodeposition potential in step S2 is -0.6 to -0.9 V, preferably -0.7 to -0.8 V, and the deposition time is 25 to 35 min.

6. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: The porous substrate in step S2 is one of nickel foam, titanium foam, stainless steel mesh, copper foam, nickel fiber felt or carbon cloth, preferably nickel foam.

7. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: The hydrophobic material solution in step S2 is an ethanol solution of trans-cinnamic acid with a concentration of 0.25~0.30 mol / L. -1 Soaking time is 2-3 hours.

8. The method for fabricating a three-dimensional integrated electrode according to claim 1, characterized in that: The thickness of the hydrophobic layer formed in step S3 accounts for 0.6 to 0.9 of the thickness of the porous substrate, preferably 0.7 to 0.

8.

9. A three-dimensional integrated electrode is obtained by the method for preparing a three-dimensional integrated electrode according to any one of claims 1-8.

10. An application of the three-dimensional integrated electrode as described in claim 9, characterized in that, The three-dimensional integrated electrode is used as the anode for electrocatalytic water splitting in an oxygen evolution reaction in an alkaline medium. Preferably, the alkaline medium is 1 mol L. -1 A potassium hydroxide solution.

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