Eutectic high-entropy alloy-based gas diffusion layer for aemwe electrolyzer cell and preparation method

By combining eutectic high-entropy alloy materials with selective laser melting technology and heat treatment processes, a three-dimensional dual-continuous nanoporous structure gas diffusion layer was prepared, which solved the problems of insufficient catalyst performance and structural design in AEMWE water electrolysis technology, realized the integration of efficient mass transfer and catalytic activity, and improved the efficiency and stability of hydrogen production from water electrolysis.

CN121373468BActive Publication Date: 2026-03-24TIANJIN UNIVERSITY OF TECHNOLOGY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-12-24
Publication Date
2026-03-24

AI Technical Summary

Technical Problem

In existing AEMWE water electrolysis technology, the catalyst performance is insufficient, the cost is high, and the stability is poor. The gas diffusion layer structure design cannot achieve the integration of efficient mass transfer and catalytic activity, and traditional manufacturing methods are difficult to prepare gas diffusion layers with complex structures.

Method used

Using the eutectic high-entropy alloy AlFeCoCrNi2.1, a three-dimensional lattice-like superstructure was designed through machine learning, integrally formed using selective laser melting (SLM) technology, and combined with heat treatment process to prepare a gas diffusion layer with a three-dimensional dual continuous nanoporous structure.

Benefits of technology

A gas diffusion layer with high catalytic activity, excellent mechanical strength and good mass transfer performance was achieved, which significantly improved the efficiency and durability of hydrogen production by water electrolysis, reduced costs and solved the problems of catalyst stability and limited mass transfer.

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Abstract

The application belongs to the technical field of hydrogen production by water electrolysis, and discloses a eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cell and a preparation method. 2.1 The method adopts a gas atomization method to prepare eutectic high-entropy alloy spherical powder with a composition of AlFeCoCrNi 2.1 ; a model with a three-dimensional imitated lattice superstructure is established under optimized parameters through an SLM process; after the eutectic high-entropy alloy spherical powder is integrally formed into a gas diffusion layer component according to the model by using a selective laser melting technology, heat treatment and electrochemical dealloying treatment are performed to form a three-dimensional double-continuous nano-porous structure on the surface. The novel high-entropy alloy, the advanced SLM additive manufacturing technology, the structural design concept and the systematic post-treatment process are combined, a new type of EHEA-based gas diffusion layer with excellent performance, controllable structure and reliable preparation is successfully created, and the development of a high-performance water electrolysis device is promoted, thereby laying a solid foundation for industrial application.
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Description

Technical Field

[0001] This invention belongs to the field of water electrolysis for hydrogen production technology, and particularly relates to a eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolyzers and its preparation method. Background Technology

[0002] Hydrogen energy, due to its advantages such as light weight, high calorific value, and zero pollution, is considered an ideal green energy source to replace fossil fuels. Among these technologies, water electrolysis for hydrogen production is simple, produces pure products, and enables carbon recycling, making it an important pathway for the clean production of ultrapure hydrogen. This technology uses electricity to cause water to undergo an electrochemical reaction on the electrode surface, decomposing it into hydrogen and oxygen, including the cathode hydrogen evolution reaction (HER) and the anodic oxygen evolution reaction (OER). Based on the electrolyte type, water electrolysis for hydrogen production is mainly divided into alkaline water electrolysis (AWE), proton exchange membrane water electrolysis (PEM), solid oxide electrolysis (SOEC), and anion exchange membrane water electrolysis (AEMWE). AEMWE combines the advantages of AWE and PEM, using anion exchange membranes as solid electrolytes, and possesses both low-cost catalyst compatibility and high current density operation capabilities, making it a promising new water electrolysis technology.

[0003] Despite the promising prospects of water electrolysis technologies such as AEMWE, their large-scale application remains constrained by high cost, low efficiency, and high energy consumption, with insufficient catalyst performance being the core limiting factor. Electrolysis reactions heavily rely on efficient catalysts to reduce overpotential and improve energy conversion efficiency. Currently, while noble metal catalysts exhibit excellent performance, their high cost and resource scarcity have driven the development of high-performance, low-cost non-noble metal catalysts. These catalysts require component optimization and structural design (such as porous, low-dimensional, or heterogeneous structures) to expose more active sites and enhance mass transfer, thereby achieving catalytic activity and stability comparable to noble metals. However, excellent catalyst powders must be loaded onto specific conductive substrates to form effective electrodes. Here, the gas diffusion layer (GDL), as a key component of the electrolyzer, has a significant impact on catalytic efficiency and system performance. A superior GDL must possess high conductivity, suitable pore structure, and good hydrophobicity to achieve efficient transport of reactant gases, timely drainage of liquid water, and electron conduction, while simultaneously providing stable support for the catalyst, thereby improving the efficiency of the three-phase interface reaction and overall durability. Therefore, integrating the material innovation of the catalyst with the structural design of the gas diffusion layer, rather than simply "coating" and "loading", has become a key path to break through existing technological bottlenecks and promote the large-scale application of water electrolysis hydrogen production technology.

[0004] Based on the aforementioned "material-structure integration" design concept, high-entropy alloys (HEAs) exhibit great potential. While transition metals show promise in electrocatalysis, the stability of a single metal is insufficient. Multi-metal alloys can optimize performance through synergistic effects. Among them, high-entropy alloys (HEAs) are composed of five or more elements in near equimolar ratios, possessing four core effects: high entropy, lattice distortion, hysteretic diffusion, and a cocktail effect. These effects effectively suppress phase separation, promote electron transfer, enhance structural stability, and synergistically optimize catalytic activity. In particular, eutectic high-entropy alloys (EHEAs), as an important branch of HEAs, possess a layered or rod-shaped biphase lamellar structure formed by eutectic reactions. While retaining the advantages of HEAs, they further introduce abundant phase interfaces and grain boundaries. This microstructure not only provides a large number of highly active interface sites for electrocatalytic processes, significantly enhancing the reaction kinetics of HER and OER, but also effectively disperses stress, suppresses elemental segregation and phase coarsening, thereby greatly improving the durability and stability of materials in harsh electrolysis environments.

[0005] To combine the superior intrinsic properties of EHEA with the complex macroscopic structures required by GDL, selective laser melting (SLM), an advanced additive manufacturing technology, offers an ideal technical approach. SLM possesses high-precision forming capabilities, directly manufacturing porous, channel, or mesh structures with complex three-dimensional periodic arrangements, meeting the stringent requirements of GDL for precise pore design and gas / liquid transport paths. Although this process can be achieved through extremely high cooling rates (up to 10... 8 SLM (Scanning Laser) suppresses elemental segregation, forming a uniform and fine microstructure, thereby improving the structural integrity and conductivity of the material. However, it also introduces significant residual stress, which needs to be eliminated through subsequent heat treatment. By flexibly adjusting process parameters such as laser power and scanning strategy, SLM can also precisely control the porosity, pore morphology, and surface characteristics of GDL (Gas Dioxide), thereby optimizing the gas phase transport, liquid water drainage, and electron conduction capabilities. In addition, the mold-free and near-net-shape characteristics of SLM make it particularly suitable for the rapid manufacturing of customized and integrated GDLs, providing a powerful technical approach for developing next-generation high-performance, long-life electrolyzer electrodes.

[0006] In summary, the preparation of EHEA-based GDL structures with excellent water electrolysis performance using selective laser melting (SLM) technology requires a systematic consideration of the direct impact of key factors such as thermal stress and microstructure evolution generated during the SLM process on catalytic performance. Process parameters, such as laser power and scanning speed, directly affect the solidification behavior of the molten pool, elemental distribution, and defect formation, thereby regulating the phase composition, interfacial characteristics, and catalytic activity of the alloy. Subsequent heat treatment can effectively alleviate residual stress, promote phase stabilization and microstructure homogenization, further improving the overall stability and electrochemical performance of EHEA-GDL. Furthermore, SLM technology provides GDL structural design with great flexibility, enabling the creation of complex three-dimensional spatial configurations with hierarchical porosity. Such structures not only expand the electrochemical active area but also effectively optimize reaction mass transfer, gas diffusion, and electron transport paths, thus significantly enhancing the efficiency of hydrogen evolution / oxygen evolution reactions. Therefore, by synergistically optimizing the SLM process, post-treatment, and structural design, EHEA-based GDLs with both high catalytic activity and good durability can be prepared, providing an integrated material and structural solution for promoting high-performance water electrolysis hydrogen production technology.

[0007] Based on the above analysis, the existing technologies have the following problems and defects: in terms of materials, they cannot simultaneously achieve both non-precious metals and high performance and high stability; in terms of structure, there are interface problems between the catalytic layer and the diffusion layer; in terms of manufacturing, they cannot achieve synergistic control of complex structures and excellent material microstructures; and they lack an overall solution that can integrate low-cost, high-stability catalytic materials with precisely controllable three-dimensional porous transport structures. Summary of the Invention

[0008] To overcome the problems existing in related technologies, the present invention discloses an embodiment of a eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells and its preparation method. The method utilizes machine learning-aided design of material composition and macroscopic superstructure, and employs selective laser melting (SLM) technology to achieve integrated preparation of materials and structures. Finally, heat treatment processes are used to optimize its overall performance. The technical solution is as follows:

[0009] This invention is achieved by providing a method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolyzer, comprising the following steps:

[0010] S1, prepared by gas atomization method, has the composition AlFeCoCrNi. 2.1 Eutectic high-entropy alloy spherical powder;

[0011] S2, using the SLM process, a model with a three-dimensional lattice-like superstructure is established under optimized parameters;

[0012] S3, using selective laser melting technology, under a protective atmosphere, the eutectic high-entropy alloy spherical powder is integrally formed into a gas diffusion layer component according to the model;

[0013] S4, the gas diffusion layer component is heat-treated, and then electrochemically dealloyed in an acidic solution to form a three-dimensional bicontinuous nanoporous structure on the surface.

[0014] In step S1, the preparation of eutectic high-entropy alloy spherical powder includes:

[0015] After weighing the metal raw material with an atomic ratio of Al:Fe:Co:Cr:Ni=1:1:1:1:2.1, it was ultrasonically cleaned with alcohol and dried to remove surface contaminants.

[0016] The pretreated metal raw materials are placed in a vacuum induction melting furnace for vacuum induction melting. The melting temperature is controlled at 150-300℃ above the alloy liquidus line, and the melting is repeated 4-6 times.

[0017] Spherical alloy powders were prepared by high-pressure gas atomization under an argon atmosphere of 2-8 MPa, and eutectic high-entropy alloy spherical powders with a particle size of 15-53 μm were obtained by sieving.

[0018] Furthermore, before vacuum induction melting of the metal raw materials, the oxygen content in the furnace is reduced to 10% through a vacuuming-argon gas circulation process. -2 Below Pa.

[0019] In step S2, the lattice-like superstructure adopts a face-centered cubic, body-centered cubic, or multiphase mosaic composite form, with a rod diameter of 100-500 μm and a porosity of 50-80%.

[0020] In step S3, the eutectic high-entropy alloy spherical powder is integrally formed into a gas diffusion layer component according to the model, including:

[0021] Design a 3D model of a lattice structure using CAD software and convert it into a standard triangulation language file;

[0022] Based on the minimum requirements of Z-axis height, surface roughness, and support structure, the optimal manufacturing direction is adjusted, and the support structure is generated.

[0023] The model file is sliced ​​into layers of equal thickness according to the set thickness, and the sliced ​​data is transmitted to the SLM device;

[0024] The 304 stainless steel substrate is preheated at a temperature of 80-120℃, and then a layer of metal with a thickness of 20-50μm is uniformly deposited on the preheated substrate.

[0025] A high-energy-density laser beam selectively melts metal powder in the xy plane according to path planning data;

[0026] A powder-spreading scraper spreads another layer of metal powder on the processed layer. The laser beam selectively melts the powder based on the slice data of the next layer. The powder spreading is repeated until a gas diffusion layer component is obtained.

[0027] Furthermore, the substrate preheating temperature is 80-120℃, the powder coating thickness is 20-50μm, and the protective atmosphere is argon with an oxygen content of less than 100ppm;

[0028] The process parameters of the selective laser melting technology are as follows: laser power 100-350W, scanning speed 600-1000mm / s, scanning spacing 0.06-0.1mm, and layer thickness 20-60μm.

[0029] The overall dimensions of the gas diffusion layer component are 18mm×5mm×3mm and 20mm×20mm×20mm.

[0030] In step S4, the heat treatment is carried out under vacuum, with the temperature increased to 600-1100°C at a rate of 5°C / min and held for 1-6 hours; after the holding period, the temperature is decreased to below 300°C at a rate of 2°C / min and cooled to room temperature in the furnace.

[0031] The electrochemical dealloying process employs a dual-electrode system, applying a constant voltage of 4V for 60 minutes in a 0.5mol / L sulfuric acid solution.

[0032] Another object of the present invention is to provide a eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolyzers, which is prepared by the aforementioned method for preparing a eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolyzers, and the material of the gas diffusion layer is AlFeCoCrNi. 2.1 It is a eutectic high-entropy alloy with a three-dimensional pseudo-lattice macroscopic porous structure and a three-dimensional bicontinuous nanoporous structure covering the surface of the macroscopic structural framework.

[0033] Furthermore, in a 1.0M KOH electrolyte, at least one of the following performance indicators must be met:

[0034] The hydrogen evolution reaction at 50 mA cm -2 Overpotential at current density ≤150mV;

[0035] The oxygen evolution reaction occurs at 50 mA cm⁻¹ -2 Overpotential at current density ≤300mV;

[0036] The Tafel slopes for the hydrogen evolution reaction and the oxygen evolution reaction are less than 180 mV / dec and 110 mV / dec, respectively.

[0037] At 50mA cm -2After continuous operation at current density for 120 hours, the activity decay rate of both hydrogen evolution reaction and oxygen evolution reaction does not exceed 5%.

[0038] Furthermore, it possesses a hierarchical porous structure, with a compressive yield strength of 800-2000 MPa, a compressive strength of 1000-3200 MPa, and a strain rate of 20-35%.

[0039] Combining all the above technical solutions, the beneficial effects of this invention are as follows:

[0040] First, this invention uses machine learning to design a composition of AlFeCoCrNi. 2.1 This invention utilizes a eutectic high-entropy alloy and integrates a gas diffusion layer with a three-dimensional lattice-like superstructure using selective laser melting (SLM) technology. The invention employs gas atomization to prepare spherical alloy powder; uses SLM technology with optimized parameters to form components with multi-level porosity; and then performs heat treatment to eliminate residual stress and optimize the microstructure.

[0041] This invention specifically relates to a eutectic high-entropy alloy (EHEA) catalytic material composed of Al, Fe, Co, Cr, and Ni elements, with the chemical composition AlFeCoCrNi. 2.1 This invention utilizes machine learning methods to design various superstructures with macroscopic pore structures and employs selective laser melting (SLM) technology to fabricate these superstructures. The invention optimizes the thermal stress and microstructure generated during SLM forming through heat treatment processes. Finally, the optimized new material and structure are applied to the gas diffusion layer of an AEMWE electrolyzer, achieving integrated mechanical support, gas-liquid diffusion, and catalytic activity. This represents an innovative material-structure-function co-design method.

[0042] The eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolyzers prepared by this invention has high catalytic activity, excellent mechanical strength and good mass transfer performance. It realizes the integrated integration of hydrogen / oxygen evolution reaction sites and gas transport channels, which significantly improves the efficiency and durability of AEMWE electrolyzers and provides an effective solution to the problems of high cost, poor stability and limited mass transfer of water electrolysis catalysts.

[0043] Secondly, the innovative fabrication process and improved microstructure and properties of this invention: The gas diffusion layer (GDL) is prepared using selective laser melting (SLM) technology, overcoming defects such as component segregation, coarse microstructure, and cracks that are easily generated by traditional casting methods. By optimizing process parameters such as laser power and scanning speed, a formed part with a density higher than 99.5% is obtained, ensuring structural integrity and conductivity. The rapid melting and solidification process of SLM significantly refines the grains, increasing the number of grain boundaries that serve as efficient catalytic sites, thereby enhancing intrinsic catalytic activity. The subsequent heat treatment process effectively eliminates residual tensile stress generated during forming, greatly enhancing the structural stability and long-term service life of the electrode and preventing stress corrosion failure.

[0044] This invention boasts exceptional mechanical structural stability: the EHEA itself possesses high strength and hardness, providing a robust substrate for the GDL. The integrated structure achieved through SLM technology fundamentally avoids the problems of easy peeling and powdering inherent in traditional catalytic coatings. This structure exhibits extremely high compressive strength, not only withstanding the immense clamping forces during electrolyzer assembly but also resisting fluid erosion during long-term operation, effectively preventing performance degradation due to structural collapse, thereby ensuring the long-term shape stability and service life of the electrode.

[0045] This invention offers high design freedom and improved mass transfer efficiency: Benefiting from the mold-free and freely formable characteristics of SLM technology, this invention successfully fabricates a gas diffusion layer electrode with a three-dimensional porous lattice structure. This design significantly increases the electrode's specific surface area, exposing more catalytic active sites. Simultaneously, the interconnected pore structure significantly optimizes mass transfer efficiency, promotes rapid escape of reaction bubbles and smooth electrolyte replenishment, and effectively prevents active sites from being shielded by bubbles. This results in lower overpotential and Tafel slope at high current densities, significantly improving overall catalytic efficiency.

[0046] This invention optimizes and ensures the reproducibility of the process chain: It provides a complete and systematic process scheme from the preparation of high-quality spherical powder (gas atomization method) → establishment of lattice-like superstructures → SLM forming process window → post-treatment heat treatment regime → performance evaluation. The parameter ranges of each step have been optimized and verified to ensure the repeatability of the preparation process and the consistency of the final product performance, laying a solid foundation for industrial application.

[0047] In summary, this invention combines novel high-entropy alloys, advanced SLM additive manufacturing technology, structural design concepts, and systematic post-processing techniques to successfully create a novel EHEA-based gas diffusion layer with excellent performance, controllable structure, and reliable preparation. This solves several pain points in traditional materials and processes and promotes the development of high-performance water electrolysis devices.

[0048] Third, this invention directly addresses the huge market for green hydrogen energy by employing non-precious metal eutectic high-entropy alloy materials, thus eliminating dependence on precious metal catalysts and significantly reducing raw material and manufacturing costs. The integrated structural design further enhances electrode performance, reduces energy consumption, and extends lifespan, resulting in higher economic efficiency throughout its entire lifecycle. Simultaneously, the introduction of SLM additive manufacturing technology opens up a new path for developing next-generation high-performance, customized electrolyzers, demonstrating enormous potential for technology spillover.

[0049] Unlike the traditional approach of "inert matrix + coated catalyst" that is currently widely used, this invention is the first to directly form a gas diffusion layer with three-dimensional ordered channels from a eutectic high-entropy alloy with intrinsic catalytic activity through selective laser melting technology. This achieves the integrated fusion of mechanical structure, catalytic activity and mass transfer function, filling the technological gap in the field of integrated design and manufacturing from materials to structure.

[0050] Traditional non-precious metal catalysts face problems such as insufficient activity and stability, reliance on binders, and easy detachment. This invention, through synergistic innovation in materials and manufacturing processes, achieves electrodes with high catalytic activity, excellent structural stability, and optimized mass transfer pathways without using precious metals, overcoming a long-standing technical bottleneck in this field. This invention breaks through the perception that "SLM-molded parts are unsuitable for electrocatalysis due to numerous defects," transforming rapid solidification into a structural advantage through machine learning and heat treatment optimization, resulting in a high-density active interface. Furthermore, this invention overcomes the one-sided view that "multi-element high-entropy alloys lead to dilution of active sites or the formation of an inert layer," achieving excellent hydrogen evolution and oxygen evolution performance simultaneously through precise eutectic composition design and process control, utilizing phase interface synergy and an active surface layer. Attached Figure Description

[0051] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this disclosure and, together with the description, serve to explain the principles of this disclosure;

[0052] Figure 1 This is a flowchart of the preparation method of the eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells provided in this embodiment of the invention;

[0053] Figure 2(a) is a schematic diagram of the pseudo-lattice structure sample prepared by photopolymerization 3D printing provided in Example 1; Figure 2(b) is a schematic diagram of the pseudo-lattice structure sample prepared by photopolymerization 3D printing provided in Example 2; Figure 2(c) is a schematic diagram of the pseudo-lattice structure sample prepared by photopolymerization 3D printing provided in Example 3; and Figure 2(d) is a schematic diagram of the pseudo-lattice structure sample prepared by photopolymerization 3D printing provided in Example 4.

[0054] Figure 3(a) is a scanning electron microscope (SEM) image of a eutectic high-entropy alloy with a multi-level nanoporous structure prepared by heat treatment-assisted SLM in Example 1; Figure 3(b) is a scanning electron microscope (SEM) image of a eutectic high-entropy alloy with a multi-level nanoporous structure prepared by heat treatment-assisted SLM in Example 2; Figure 3(c) is a scanning electron microscope (SEM) image of a eutectic high-entropy alloy with a multi-level nanoporous structure prepared by heat treatment-assisted SLM in Example 3; and Figure 3(d) is a scanning electron microscope (SEM) image of a eutectic high-entropy alloy with a multi-level nanoporous structure prepared by heat treatment-assisted SLM in Example 4.

[0055] Figure 4(a) is the stress-strain curve of the compressive mechanical properties provided in Example 1, Figure 4(b) is the stress-strain curve of the compressive mechanical properties provided in Example 2, Figure 4(c) is the stress-strain curve of the compressive mechanical properties provided in Example 3, and Figure 4(d) is the stress-strain curve of the compressive mechanical properties provided in Example 4.

[0056] Figure 5(a) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 1; Figure 5(b) is the Tafel slope graph corresponding to HER, the electrolysis performance test result of water provided in Example 1; Figure 5(c) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 1, at 50 mA cm⁻¹. -2 The stability test diagrams at current density are shown in Figure 5(d), which is the polarization curve of the OER (outcome efficiency) of the water electrolysis performance test results provided in Example 1; Figure 5(e) is the Tafel slope diagram corresponding to the OER of the water electrolysis performance test results provided in Example 1; and Figure 5(f) is the OER of the water electrolysis performance test results provided in Example 1 at 50 mA cm⁻¹. -2 Stability test results at current density;

[0057] Figure 6(a) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 2; Figure 6(b) is the Tafel slope graph corresponding to HER, the electrolysis performance test result of water provided in Example 2; Figure 6(c) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 2, at 50 mA cm⁻¹. -2 The stability test diagrams at current density are shown in Figure 6(d), which is the polarization curve of the OER (outcome efficiency) of the water electrolysis performance test results provided in Example 2; Figure 6(e) is the Tafel slope diagram corresponding to the OER of the water electrolysis performance test results provided in Example 2; and Figure 6(f) is the OER of the water electrolysis performance test results provided in Example 2 at 50 mA cm⁻¹. -2 Stability test results at current density;

[0058] Figure 7(a) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 3; Figure 7(b) is the Tafel slope of HER, the electrolysis performance test result of water provided in Example 3; Figure 7(c) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 3, at 50 mA cm⁻¹. -2 The stability test diagrams at current density are shown in Figure 7(d), which is the polarization curve of the OER (outcome efficiency) of the water electrolysis performance test results provided in Example 3; Figure 7(e) is the Tafel slope diagram corresponding to the OER of the water electrolysis performance test results provided in Example 3; and Figure 7(f) is the OER of the water electrolysis performance test results provided in Example 3 at 50 mA cm⁻¹. -2 Stability test results at current density;

[0059] Figure 8(a) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 4; Figure 8(b) is the Tafel slope of HER, the electrolysis performance test result of water provided in Example 4; Figure 8(c) is the polarization curve of HER, the electrolysis performance test result of water provided in Example 4, at 50 mA cm⁻¹. -2 The stability test results at current density are shown in Figure 8(d), which is the polarization curve of the OER (Optical Emission Rate) of the water electrolysis performance test results provided in Example 4; Figure 8(e) is the Tafel slope diagram corresponding to the OER of the water electrolysis performance test results provided in Example 4; and Figure 8(f) is the OER of the water electrolysis performance test results provided in Example 4 at 50 mA cm⁻¹. -2 Stability test results at current density. Detailed Implementation

[0060] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention can be practiced in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0061] The innovation of this invention lies in:

[0062] (1) Material system innovation: using AlFeCoCrNi with a specific stoichiometric ratio 2.1 Eutectic high-entropy alloys, as basic materials, possess a unique two-phase layered structure that maintains the multi-element synergistic effect of high-entropy alloys while also having abundant phase interface active sites, thus achieving highly efficient intrinsic catalytic activity of the material itself.

[0063] (2) Structural design innovation: Through machine learning-assisted design, a superstructured gas diffusion layer with three-dimensional ordered porous structure was constructed, realizing precise control of pore size, porosity and pore morphology, and optimizing gas-liquid transport path and electron conduction network.

[0064] (3) Innovative manufacturing process: Selective laser melting technology was applied to the superstructure forming of this material. Through optimized process parameter combination and unique heat treatment system, forming stress was effectively eliminated, microstructure was refined, and high-precision, high-performance integrated manufacturing was achieved.

[0065] (4) Functional integration innovation: It breaks through the traditional electrode construction mode of "substrate + coating" and realizes the integration of the three major functions of mechanical support, gas-liquid transport and catalytic activity of gas diffusion layer, fundamentally solving the inherent problems such as easy detachment of catalyst layer and large interface resistance.

[0066] (5) Innovation in design methods: A complete technology chain has been established from material calculation, structural optimization, forming process to post-processing, forming a system solution of "material-structure-function" collaborative design, providing a new paradigm for the development of high-performance water electrolysis electrodes.

[0067] These innovations together constitute a complete technical system, enabling the prepared gas diffusion layer to exhibit significant advantages in catalytic activity, structural stability, and mass transfer efficiency, providing a practical and feasible technical path for improving the performance of the AEMWE electrolyzer.

[0068] Example 1, such as Figure 1 As shown, the method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolyzer provided in this embodiment of the invention includes the following steps:

[0069] S1, prepared by gas atomization method, has the composition AlFeCoCrNi. 2.1 Eutectic high-entropy alloy spherical powder;

[0070] S2, using the SLM process, a model with a three-dimensional lattice-like superstructure is established under optimized parameters;

[0071] S3, using selective laser melting technology, under a protective atmosphere, the eutectic high-entropy alloy spherical powder is integrally formed into a gas diffusion layer component according to the model;

[0072] S4, the gas diffusion layer component is heat-treated, and then electrochemically dealloyed in an acidic solution to form a three-dimensional bicontinuous nanoporous structure on the surface.

[0073] 1. Preparation of metal powder

[0074] (1) Select blocky high-purity metal raw materials Al, Fe, Co, Cr and Ni with a purity of not less than 99.95% and weigh them accurately according to the atomic ratio Al:Fe:Co:Cr:Ni=1:1:1:1:2.1.

[0075] (2) Place the weighed metal raw material into a beaker containing alcohol and clean it in an ultrasonic cleaner for 15 minutes to remove surface grease and oxides. Then dry it in a vacuum drying oven at 80°C for 2 hours.

[0076] (3) Load the cleaned and dried raw materials into the graphite crucible of the vacuum induction melting furnace. Evacuate the melting chamber to 5×10⁻⁶. -3 The pressure is then reduced to -0.05 MPa, followed by the introduction of high-purity argon gas (99.999% purity) to ensure the oxygen content inside the furnace remains below 10%. -2 Pa. Melting then proceeded at a temperature controlled at 1600℃ (approximately 200℃ above the alloy's estimated liquidus line), held for 10 minutes, and stirred electromagnetically to homogenize the composition. To obtain a highly homogeneous alloy ingot, the above melting process was repeated five times.

[0077] (4) Spherical alloy powder is prepared by high-pressure gas atomization. After the alloy ingot is remelted, the molten metal is guided to the atomizing nozzle through a guide tube and broken and atomized into fine droplets under an ultra-high pressure argon gas flow of 6 MPa. This high-pressure condition is suitable for the SLM process, which has strict requirements for powder sphericity and low oxygen content, and can effectively reduce splashing and incomplete fusion defects during the printing process.

[0078] (5) The atomized powder is cooled in a collection container under an inert atmosphere. Then, the powder is sieved using a standard vibrating sieve in an argon-protected glove box, and powder with a particle size range of 15-53 μm is selected for SLM printing. This particle size range is optimized: too fine a particle size will easily lead to poor flowability, uneven powder spreading and increased oxygen content; too coarse a particle size will affect the melting effect and the surface quality of the formed part.

[0079] (6) Characterization of the sieved powder: Scanning electron microscopy (SEM) showed that the powder was regularly spherical with few satellite spheres; the average particle size (D50) measured by laser particle size analyzer was 38 μm; the flow time measured by Hall flow meter was 55 s / 50 g, showing good flowability, which is crucial for achieving thin, uniform and stable powder spreading in the SLM process, and is a prerequisite for ensuring the consistency and high precision of the printed structure; the energy dispersive spectroscopy (EDS) results showed that the content of each element was consistent with the designed composition AlFeCoCrNi 2.1 The results were largely consistent, proving the effectiveness of the preceding melting and atomization processes and ensuring the accuracy of the chemical composition of the subsequent SLM-formed parts.

[0080] 2. Design and Modeling of Simulated Lattice Superstructures

[0081] A biomimetic three-dimensional porous structure model based on a body-centered cubic (BCC) lattice was established using computer-aided design software. Key geometric parameters were set as follows: lattice rod diameter 300 μm, unit cell size 1.5 mm × 1.5 mm × 1.5 mm, and theoretical porosity 70%. The three-dimensional model was exported as an STL file, and a preliminary prototype was verified using photopolymerization 3D printing technology with resin material, confirming the feasibility and accuracy of the structural design, as shown in Figure 2(a). This step solved the technical problems of the traditional GDL structure being singular and having random and uncontrollable pore distribution. Through lattice-like design, precise programming of porosity, pore size, and shape was achieved, creating ideal three-dimensional channels for the rapid and orderly transport of reactants and products, while also providing a large loading area and stable mechanical support for the catalyst.

[0082] 3. SLM printing

[0083] (1) Import the BCC pseudo-lattice STL model designed above into the processing software of the SLM device (e.g., EOS M290).

[0084] (2) Place the model in the forming chamber along the Z-axis to minimize the support structure and ensure a high printing success rate. The software automatically generates the necessary supports.

[0085] (3) Slice the model and set the layer thickness to 30μm.

[0086] (4) Select a sandblasted 304 stainless steel substrate and preheat it to 100°C. Substrate preheating can effectively reduce the temperature gradient during the printing process, which is one of the key measures to control the warping deformation and residual stress of the formed parts. Use recycled AlFeCoCrNi 2.1 Alloy powder is used as raw material to lay a 30μm thick powder layer on the substrate.

[0087] (5) Select parameter combination #4 in Table 1 as the optimized process: laser power 150W, scanning speed 850mm / s -1 The scanning spacing was 0.07 mm, the layer thickness was 30 μm, and the laser scanning direction of adjacent layers was rotated by 67°. This parameter combination was optimized for the characteristics of AlFeCoCrNi2.1EHEA material, aiming to achieve a balance between the "keyhole" effect and the "conductive" melting mode. This ensures complete melting and densification of the powder while avoiding defects such as porosity and spheroidization caused by excessive energy input. The 67° scanning rotation strategy between layers helps to disperse heat accumulation, refine grains, and reduce anisotropy.

[0088] (6) In a high-purity argon protective atmosphere with oxygen content strictly controlled at <100ppm, the SLM equipment lays powder layer by layer and selectively melts it according to the set path, repeating the process until multiple gas diffusion layer samples with BCC pseudo-lattice structure are finally integrally formed. The overall size of the sample is 18mm×5mm×3mm and 20mm×20mm×20mm. The SLM technology solves the problem that traditional processing methods (such as sintering and pressing) cannot manufacture complex three-dimensional integrated GDLs, realizing the integrated manufacturing of "material-structure-function", and avoiding the problem of weak interfacial bonding between the catalyst coating and the substrate due to the mismatch of thermal expansion coefficients.

[0089] Table 1. SLM process parameter screening experiment

[0090]

[0091] 4. Post-processing stage

[0092] (1) Take out the 18mm×5mm×0.5mm sample of the simulated lattice GDL from the SLM forming substrate by wire cutting.

[0093] (2) Select parameter combination #3 in Table 2 for heat treatment: heat treatment temperature 800℃, heating rate 5℃ min -1 The heat preservation time is 4 hours, followed by 2℃ min. -1 The temperature is slowly reduced to below 300°C, and finally cooled to room temperature in the furnace. This heat treatment regime is specifically designed for SLM-formed EHEA-GDL: the temperature of 800°C is sufficient to drive atomic diffusion, effectively eliminating the residual stress of up to 165 MPa accumulated during the SLM process (reducing it by 64%), while also inhibiting eutectic coarsening and promoting the formation of a stable two-phase structure. The slow heating and cooling rates are designed to avoid introducing new thermal stresses, ensuring the dimensional stability and structural integrity of the material. This step addresses the risk of long-term service failure caused by high internal stress and metastable microstructure in SLM parts, significantly improving the durability of GDL under dynamic operating conditions in the electrolytic cell.

[0094] Table 2. Screening Experiment of Heat Treatment Process Parameters

[0095]

[0096] 5. Performance Characterization and Test Results

[0097] (1) Residual stress: The residual stress on the surface of the SLM state was measured to be 165 MPa (tensile stress) by XRD method, and the residual stress on the surface after heat treatment was 59.5 MPa (tensile stress), which was reduced by 64%. The significant reduction in residual stress directly improved the fatigue resistance and stress corrosion cracking resistance of GDL, which is crucial for maintaining structural stability in the electrolytic cell environment with frequent start-up and shutdown.

[0098] (2) The compressive mechanical properties of the prepared GDL structure (sample size 20mm×20mm×20mm) were evaluated. The specific steps are as follows:

[0099] Quasi-static uniaxial compression tests (strain rate 1×10⁻⁶) were performed on the heat-treated pseudo-lattice GDL structure on a universal testing machine. -4 s -1 This structure exhibits excellent mechanical properties, with a compressive yield strength of 1071 MPa and a compressive strength as high as 1522 MPa. It did not collapse even at 30% strain, as shown in Figure 4(a), demonstrating good plasticity and energy absorption capacity. These properties indicate that this GDL not only meets the enormous compressive stress requirements generated by bolt tightening during electrolytic cell assembly, preventing structural crushing, but also maintains its morphological integrity under operational vibration or accidental impact. It solves the technical problems of insufficient mechanical strength and susceptibility to damage during assembly and operation of traditional porous metal GDLs or carbon-based GDLs.

[0100] (3) Electrolysis performance of water:

[0101] The SLM-printed alloy block was fabricated into a sample with dimensions of 18 mm × 5 mm × 0.5 mm. To construct a high specific surface area nanoporous structure on the surface to further enhance catalytic activity, the sample underwent electrochemical dealloying. The principle is to selectively corrode the active metal elements (such as Al) in the alloy, leaving a three-dimensional bicontinuous nanoporous framework rich in transition metals (Fe, Co, Cr, Ni). Electrochemical dealloying was performed using a dual-electrode system: working electrode: test sample; counter electrode: carbon rod; dealloying solution: 0.5 mol / L. -1 Sulfuric acid (H2SO4) was used. Using CHI760e software, the parameters were set as follows: constant voltage 4V for electrochemical dealloying experiment for 60 minutes. The morphology after dealloying is shown in Figure 3(a). Micro-nano-scale pores were successfully introduced into the macroscopic pseudo-lattice structure surface, forming a unique "macro-micro-nano" hierarchical porous structure, which greatly increased the electrochemical active area. The experiment was conducted in 1.0M KOH electrolyte using a standard three-electrode system.

[0102] 1) Hydrogen evolution reaction performance:

[0103] a. Polarization curve: As shown in Figure 5(a), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 140mV, which is far below the invention target (≤150mV).

[0104] b. The slope of Tafel is 154.3 mV dec -1As shown in Figure 5(b), this indicates that its HER reaction kinetics are rapid.

[0105] c. Stability: As shown in Figure 5(c), at 50 mA cm -2 After 120 hours of continuous electrolysis at a constant current density, the activity decay rate was approximately 3.8%, demonstrating excellent long-term stability. This addresses the common problem of poor stability of non-precious metal catalysts in alkaline HER, thanks to the excellent corrosion resistance of EHEA itself and the stable nanoframework formed after dealloying.

[0106] 2) Oxygen evolution reaction performance:

[0107] a. Polarization curve: As shown in Figure 5(d), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 279mV, which is better than the invention target (≤300mV).

[0108] b. The slope of Tafel is 69.9mV dec -1 As shown in Figure 5(e), it demonstrates excellent OER reaction kinetics.

[0109] c. Stability: As shown in Figure 5(f), at 50 mA cm -2 After operating continuously for 120 hours at high current density, the activity decay rate was approximately 2.8%, meeting the stability requirements. This demonstrates that the material exhibits excellent resistance to passivation and dissolution even under harsh OER environments (high potential, strong oxidizing properties), achieving highly efficient dual-function catalysis for both HER and OER.

[0110] This embodiment is designed for industrial-grade electrolytic cells with stringent requirements for mechanical strength and long-term robustness. By employing a body-centered cubic (BCC) lattice (300 μm rod diameter), a robust mechanical framework is constructed. A medium-temperature heat treatment regime of 800°C effectively eliminates 64% of residual stress while precisely stabilizing the eutectic structure and inhibiting excessive coarsening, perfectly balancing stress relief and retention of mechanical properties. Its high compressive yield strength of 1071 MPa successfully solves the problem of traditional porous electrodes (such as sintered metals or carbon paper) being easily crushed under bolt clamping forces of tens of megapascals, leading to pore structure failure and a sharp decline in mass transfer performance. This GDL provides excellent long-term dimensional stability and operational safety to cope with the harsh industrial conditions of frequent start-stop cycles and load fluctuations.

[0111] Example 2, the preparation method of the eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells provided in this embodiment of the invention includes the following steps:

[0112] 1. Preparation of metal powder

[0113] (1) Select blocky high-purity metal raw materials Al, Fe, Co, Cr and Ni with a purity of not less than 99.95% and weigh them accurately according to the atomic ratio Al:Fe:Co:Cr:Ni=1:1:1:1:2.1.

[0114] (2) Place the weighed metal raw material into a beaker containing alcohol and clean it in an ultrasonic cleaner for 15 minutes to remove surface grease and oxides. Then dry it in a vacuum drying oven at 80°C for 2 hours.

[0115] (3) Load the cleaned and dried raw materials into the graphite crucible of the vacuum induction melting furnace. Evacuate the melting chamber to 5×10⁻⁶. -3 The pressure is then reduced to -0.05 MPa, followed by the introduction of high-purity argon gas (99.999% purity) to ensure the oxygen content inside the furnace remains below 10%. -2 Pa. Melting then proceeded at a temperature controlled at 1600℃ (approximately 200℃ above the alloy's estimated liquidus line), held for 10 minutes, and stirred electromagnetically to homogenize the composition. To obtain a highly homogeneous alloy ingot, the above melting process was repeated five times.

[0116] (4) Spherical alloy powder was prepared by high-pressure gas atomization. After the alloy ingot was remelted, the molten metal was guided to the atomizing nozzle through the guide tube and broken and atomized into fine droplets under the ultra-high pressure argon gas flow of 6MPa.

[0117] (5) The atomized powder is cooled in a collection container under an inert atmosphere. Then, the powder is sieved in an argon-protected glove box using a standard vibrating sieve to select powder with a particle size range of 15-53 μm for SLM printing.

[0118] (6) Characterization of the sieved powder: Scanning electron microscopy (SEM) showed that the powder was regularly spherical with few satellite spheres; the average particle size (D50) measured by laser particle size analyzer was 38 μm; the flow time measured by Hall flow meter was 55 s / 50 g, showing good flowability; the energy dispersive spectroscopy (EDS) results showed that the content of each element was consistent with the designed composition AlFeCoCrNi 2.1 Basically the same.

[0119] 2. Design and Modeling of Simulated Lattice Superstructures

[0120] A biomimetic three-dimensional porous structure model based on a face-centered cubic (FCC) lattice was established using computer-aided design software. Key geometric parameters were set as follows: lattice rod diameter 200 μm, unit cell size 1.2 mm × 1.2 mm × 1.2 mm, and theoretical porosity 65%. The three-dimensional model was exported as an STL file, and a preliminary prototype was verified using resin material via photopolymerization 3D printing technology to confirm the feasibility and accuracy of the structural design, as shown in Figure 2(b).

[0121] 3. SLM printing

[0122] (1) Import the FCC lattice-like STL model designed above into the processing software of the SLM equipment (e.g., EOS M290).

[0123] (2) Place the model in the forming chamber along the Z-axis to minimize the support structure and ensure a high printing success rate. The software automatically generates the necessary supports.

[0124] (3) Slice the model and set the layer thickness to 40μm.

[0125] (4) Select a sandblasted 304 stainless steel substrate and preheat it to 90°C. Use recycled AlFeCoCrNi from the above-mentioned materials. 2.1 Alloy powder is used as raw material to lay a 40μm thick powder layer on the substrate.

[0126] (5) Select parameter combination #6 in Table 1 as the optimized process: laser power 200W, scanning speed 600mm / s -1 The scanning interval is 0.08 mm, the layer thickness is 40 μm, and the laser scanning direction of adjacent layers is rotated by 67°.

[0127] (6) In a high-purity argon protective atmosphere with oxygen content strictly controlled at <100ppm, the SLM equipment lays powder layer by layer according to the set path, selectively melts it, and repeats the process until multiple gas diffusion layer samples with FCC pseudo-lattice structure are finally integrally formed. The overall size of the sample is 18mm×5mm×3mm and 20mm×20mm×20mm.

[0128] 4. Post-processing stage

[0129] (1) Take out the 18mm×5mm×0.5mm sample of the simulated lattice GDL from the SLM forming substrate by wire cutting.

[0130] (2) Select parameter combination #4 in Table 2 for heat treatment: heat treatment temperature 900℃, heating rate 5℃ min -1 The heat preservation time is 6 hours, followed by 2℃ min. -1 The temperature is slowly reduced to below 300°C, and finally cooled to room temperature along with the furnace.

[0131] 5. Performance Characterization and Test Results

[0132] (1) Residual stress: The residual stress on the surface of the SLM formed state was 195 MPa (tensile stress) measured by XRD. After heat treatment, it was reduced to 32 MPa (tensile stress), a reduction of 83.6%. This result shows that the 900℃ heat treatment regime is extremely effective in eliminating the high residual stress generated during the SLM forming process. The extremely low residual stress level (32 MPa) means that the GDL has extremely high dimensional stability and stress corrosion resistance in subsequent processing and long-term service, solving the risk of deformation or early cracking of SLM components due to internal stress.

[0133] (2) The compressive mechanical properties of the prepared GDL structure (sample size 20mm×20mm×20mm) were evaluated. The specific steps are as follows:

[0134] Quasi-static uniaxial compression tests (strain rate 1×10⁻⁶) were performed on the heat-treated pseudo-lattice GDL structure on a universal testing machine. -4 s -1 This structure exhibits excellent mechanical properties, with a compressive yield strength of 810 MPa and a compressive strength as high as 1202 MPa. It did not collapse even at 32% strain, as shown in Figure 4(b). While maintaining high strength, the structure demonstrates excellent plasticity and energy absorption capacity, thanks to the inherent high symmetry of the FCC lattice, which gives it superior ductility compared to the BCC structure under load. This characteristic ensures that GDL can adapt well to stress fluctuations and potential impacts during electrolytic cell assembly and operation, effectively avoiding the brittle fracture or crushing that is common in traditional rigid porous materials, thus meeting the stringent mechanical stability requirements of electrolytic cells.

[0135] (3) Electrolysis performance: The SLM-printed alloy block after the above treatment was made into a sample with a size of 18mm×5mm×0.5mm. In order to construct a high specific surface area nanoporous structure on the surface to further enhance the catalytic activity, the sample was subjected to electrochemical dealloying treatment. The principle is to selectively corrode the active metal elements (such as Al) in the alloy, thereby leaving a three-dimensional bicontinuous nanoporous framework rich in transition metals (Fe, Co, Cr, Ni). Electrochemical dealloying was performed using a dual electrode. Working electrode: test sample; counter electrode: carbon rod; dealloying solution: 0.5mol L -1 Sulfuric acid (H2SO4) was used. Using CHI760e software, the parameters were set as follows: constant voltage 4V for electrochemical dealloying experiment for 60 minutes. The morphology after dealloying is shown in Figure 3(b). The test was conducted in a 1.0M KOH electrolyte using a standard three-electrode system.

[0136] 1) Hydrogen evolution reaction performance:

[0137] a. Polarization curve: As shown in Figure 6(a), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 143mV, which is far below the invention target (≤150mV).

[0138] b. The Tafel slope is 164.3 mV dec -1 As shown in Figure 6(b), this indicates that its HER reaction kinetics are rapid.

[0139] c. Stability: As shown in Figure 6(c), at 50 mA cm -2 After continuous electrolysis at a constant current density for 120 hours, the activity decay rate is about 4.5%, demonstrating excellent long-term stability.

[0140] 2) Oxygen evolution reaction performance:

[0141] a. Polarization curve: As shown in Figure 6(d), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 271mV, which is better than the invention target (≤300mV).

[0142] b. The Tafel slope is 61.2mV dec -1 As shown in Figure 6(e), it demonstrates excellent OER reaction kinetics.

[0143] c. Stability: As shown in Figure 6(f), at 50 mA cm -2 After operating continuously for 120 hours at high current density, the activity decay rate is approximately 3.3%, meeting the stability requirements.

[0144] This embodiment targets high-performance electrolyzers that prioritize high mass transfer efficiency and reaction kinetics. By employing a face-centered cubic (FCC) lattice (200 μm rod diameter), its highly symmetrical unit cell structure forms a three-dimensional mass transfer channel with excellent connectivity and low detour. Combined with high-temperature heat treatment at 900℃, this promotes sufficient element diffusion and the formation of a stable equilibrium phase, laying an ideal foundation for subsequent dealloying to prepare a highly active catalytic surface layer. Its extremely low OER overpotential (271 mV) and minimal OER Tafel slope (61.2 mV / dec) directly solve the core bottleneck of a sharp increase in mass transfer overpotential caused by bubble blockage and limited electrolyte diffusion inside the electrode during high current density operation. This makes it particularly suitable for improving the energy conversion efficiency of the electrolyzer across the entire load range.

[0145] Example 3, the preparation method of the eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells provided in this embodiment of the invention includes the following steps:

[0146] 1. Preparation of metal powder

[0147] (1) Select blocky high-purity metal raw materials Al, Fe, Co, Cr and Ni with a purity of not less than 99.95% and weigh them accurately according to the atomic ratio Al:Fe:Co:Cr:Ni=1:1:1:1:2.1.

[0148] (2) Place the weighed metal raw material into a beaker containing alcohol and clean it in an ultrasonic cleaner for 15 minutes to remove surface grease and oxides. Then dry it in a vacuum drying oven at 80°C for 2 hours.

[0149] (3) Load the cleaned and dried raw materials into the graphite crucible of the vacuum induction melting furnace. Evacuate the melting chamber to 5×10⁻⁶. -3 The pressure is then reduced to -0.05 MPa, followed by the introduction of high-purity argon gas (99.999% purity) to ensure the oxygen content inside the furnace remains below 10%. -2 Pa. Melting then proceeded at a temperature controlled at 1600℃ (approximately 200℃ above the alloy's estimated liquidus line), held for 10 minutes, and stirred electromagnetically to homogenize the composition. To obtain a highly homogeneous alloy ingot, the above melting process was repeated five times.

[0150] (4) Spherical alloy powder was prepared by high-pressure gas atomization. After the alloy ingot was remelted, the molten metal was guided to the atomizing nozzle through the guide tube and broken and atomized into fine droplets under the ultra-high pressure argon gas flow of 6MPa.

[0151] (5) The atomized powder is cooled in a collection container under an inert atmosphere. Then, the powder is sieved in an argon-protected glove box using a standard vibrating sieve to select powder with a particle size range of 15-53 μm for SLM printing.

[0152] (6) Characterization of the sieved powder: Scanning electron microscopy (SEM) showed that the powder was regularly spherical with few satellite spheres; the average particle size (D50) measured by laser particle size analyzer was 38 μm; the flow time measured by Hall flow meter was 55 s / 50 g, showing good flowability; the energy dispersive spectroscopy (EDS) results showed that the content of each element was consistent with the designed composition AlFeCoCrNi 2.1 Basically the same.

[0153] 2. Design and Modeling of Simulated Lattice Superstructures

[0154] A biomimetic three-dimensional porous structure model based on a cross-composite body-centered cubic (BCC) and face-centered cubic (FCC) lattice structure was established using computer-aided design software. Key geometric parameters were set as follows: lattice bar diameter 400 μm, unit cell size 2 mm × 2 mm × 2 mm, and theoretical porosity 75%. The three-dimensional model was exported as an STL file, and a preliminary prototype was verified using resin material via photopolymerization 3D printing technology to confirm the feasibility and accuracy of the structural design, as shown in Figure 2(c).

[0155] 3. SLM printing

[0156] (1) Import the BCC / FCC composite lattice STL model designed above into the processing software of the SLM device (e.g., EOS M290).

[0157] (2) Place the model in the forming chamber along the Z-axis to minimize the support structure and ensure a high printing success rate. The software automatically generates the necessary supports.

[0158] (3) Slice the model and set the layer thickness to 20μm.

[0159] (4) Select a sandblasted 304 stainless steel substrate and preheat it to 110°C. Use recycled AlFeCoCrNi as described above. 2.1 Alloy powder is used as raw material to lay a 20μm thick powder layer on the substrate.

[0160] (5) Select parameter combination #2 in Table 1 as the optimized process: laser power 120W, scanning speed 850mm / s -1 The scanning spacing is 0.07 mm, the layer thickness is 30 μm, and the laser scanning direction of adjacent layers is rotated by 67°.

[0161] (6) In a high-purity argon protective atmosphere with oxygen content strictly controlled at <100ppm, the SLM equipment lays powder layer by layer according to the set path, selectively melts it, and repeats the process until multiple gas diffusion layer samples with BCC / FCC composite pseudo-lattice structure are finally integrally formed. The overall size of the sample is 18mm×5mm×3mm and 20mm×20mm×20mm.

[0162] 4. Post-processing stage

[0163] (1) Take out the 18mm×5mm×0.5mm sample of the simulated lattice GDL from the SLM forming substrate by wire cutting.

[0164] (2) Select parameter combination #5 in Table 2 for heat treatment: heat treatment temperature 1000℃, heating rate 5℃ min -1 The heat preservation time is 4 hours, followed by 2℃ min. -1The temperature is slowly reduced to below 300°C, and finally cooled to room temperature along with the furnace.

[0165] 5. Performance Characterization and Test Results

[0166] (1) Residual stress: The residual stress on the surface of the SLM state was measured to be 210 MPa (tensile stress) by XRD method. After heat treatment, it was reduced to 18 MPa (tensile stress), a reduction of 91.4%.

[0167] (2) The compressive mechanical properties of the prepared GDL structure (sample size 20mm×20mm×20mm) were evaluated. The specific steps are as follows:

[0168] Quasi-static uniaxial compression tests (strain rate 1×10⁻⁶) were performed on the heat-treated pseudo-lattice GDL structure on a universal testing machine. -4 s -1 This structure exhibits excellent mechanical properties, with a compressive yield strength of 1903 MPa and a compressive strength of 2983 MPa. It did not collapse even when the strain reached 22%, as shown in Figure 4(c). It demonstrates good plasticity and energy absorption capacity. These mechanical properties far exceed those of conventional porous metals or carbon-based GDLs, which is sufficient to meet the extremely high requirements for crush resistance and deformation resistance of electrode components in space-constrained electrolytic cells.

[0169] (3) Electrolysis performance: The SLM-printed alloy block after the above post-treatment was made into a sample with a size of 18mm×5mm×0.5mm. In order to construct a high specific surface area nanoporous structure on the surface to further enhance the catalytic activity, the sample was subjected to electrochemical dealloying treatment. The principle is to selectively corrode the active metal elements (such as Al) in the alloy, thereby leaving a three-dimensional bicontinuous nanoporous framework rich in transition metals (Fe, Co, Cr, Ni). Electrochemical dealloying was performed using a dual electrode. Working electrode: test sample; counter electrode: carbon rod; dealloying solution: 0.5mol L -1 Sulfuric acid (H2SO4) was used. The dealloying experiment was conducted using CHI760e software with the following parameters set: constant voltage 4V for 60 minutes. The morphology after dealloying is shown in Figure 3(c). The test was performed using a standard three-electrode system in 1.0M KOH electrolyte.

[0170] 1) Hydrogen evolution reaction performance:

[0171] a. Polarization curve: As shown in Figure 7(a), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 76mV, which is far below the invention target (≤150mV).

[0172] b. The Tafel slope is 142.6 mV dec-1 As shown in Figure 7(b), this indicates that its HER reaction kinetics are rapid.

[0173] c. Stability: As shown in Figure 7(c), at 50 mA cm -2 After continuous electrolysis for 120 hours at a constant current density, it exhibits excellent long-term stability under harsh operating conditions.

[0174] 2) Oxygen evolution reaction performance:

[0175] a. Polarization curve: As shown in Figure 7(d), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value is 253mV, which is better than the invention target (≤300mV).

[0176] b. The slope of Tafel is 98.3mV dec -1 As shown in Figure 7(e), it demonstrates excellent OER reaction kinetics.

[0177] c. Stability: As shown in Figure 7(f), at 50 mA cm -2 After operating continuously for 120 hours at high current density, the activity decay rate was approximately 2.2%, further demonstrating its durability as an integrated electrode under dynamic load.

[0178] This embodiment addresses extreme operating conditions and space-constrained scenarios with stringent requirements for volumetric power density, such as vehicle-mounted and shipboard hydrogen production equipment. By employing a cross-shaped composite of BCC and FCC lattices, it achieves a "truss within a truss" type of ultra-strong mechanical design. This design disperses the load-bearing paths in multiple directions, significantly improving the specific strength and specific stiffness of the structure. It successfully solves the core contradiction in extremely compact electrolyzer stack designs where traditional electrodes, due to insufficient strength, cannot be thinned, thus hindering the improvement of volumetric power density. This allows the electrodes to maintain structural integrity even under ultra-high in-plane compressive forces. Furthermore, it employs ultra-high temperature heat treatment at 1000℃, aiming not only to almost completely eliminate residual stress (reducing it by 91.4%), but more importantly, to drive the full diffusion of alloying elements, achieving extreme homogenization and stabilization of the microstructure. This solves the long-term durability problem where, under harsh conditions such as long-term operation, vibration, and thermal cycling, the material's microstructure may evolve due to metastable states, leading to catalytic performance degradation or structural reliability decline. Crucially, while achieving such ultra-high strength, it still maintains the lowest HER overpotential (76mV), which proves that the solution can break the traditional dilemma of the trade-off between material strength and activity, and provide an unprecedented integrated material and structure solution for the design of high power density electrolyzers.

[0179] Example 4, the preparation method of the eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells provided in this embodiment of the invention includes the following steps:

[0180] 1. Preparation of metal powder

[0181] (1) Select blocky high-purity metal raw materials Al, Fe, Co, Cr and Ni with a purity of not less than 99.95% and weigh them accurately according to the atomic ratio Al:Fe:Co:Cr:Ni=1:1:1:1:2.1.

[0182] (2) Place the weighed metal raw material into a beaker containing alcohol and clean it in an ultrasonic cleaner for 15 minutes to remove surface grease and oxides. Then dry it in a vacuum drying oven at 80°C for 2 hours.

[0183] (3) Load the cleaned and dried raw materials into the graphite crucible of the vacuum induction melting furnace. Evacuate the melting chamber to 5×10⁻⁶. -3 The pressure is then reduced to -0.05 MPa, followed by the introduction of high-purity argon gas (99.999% purity) to ensure the oxygen content inside the furnace remains below 10%. -2 Pa. Melting then proceeded at a temperature controlled at 1600℃ (approximately 200℃ above the alloy's estimated liquidus line), held for 10 minutes, and stirred electromagnetically to homogenize the composition. To obtain a highly homogeneous alloy ingot, the above melting process was repeated five times.

[0184] (4) Spherical alloy powder was prepared by high-pressure gas atomization. After the alloy ingot was remelted, the molten metal was guided to the atomizing nozzle through the guide tube and broken and atomized into fine droplets under the ultra-high pressure argon gas flow of 6MPa.

[0185] (5) The atomized powder is cooled in a collection container under an inert atmosphere. Then, the powder is sieved in an argon-protected glove box using a standard vibrating sieve to select powder with a particle size range of 15-53 μm for SLM printing.

[0186] (6) Characterization of the sieved powder: Scanning electron microscopy (SEM) showed that the powder was regularly spherical with few satellite spheres; the average particle size (D50) measured by laser particle size analyzer was 38 μm; the flow time measured by Hall flow meter was 55 s / 50 g, showing good flowability; the energy dispersive spectroscopy (EDS) results showed that the content of each element was consistent with the designed composition AlFeCoCrNi 2.1 Basically the same.

[0187] 2. Design and Modeling of Simulated Lattice Superstructures

[0188] A porous structure model based on horizontal intersections of face-centered cubic (FCC) and body-centered cubic (BCC) lattices was established using computer-aided design software. Key geometric parameters were set as follows: lattice bar diameter gradually increases from 150 μm at the bottom to 450 μm at the top; unit cell size is 1.8 mm × 1.8 mm × 1.8 mm; and theoretical porosity is 55%. The 3D model was exported as an STL file, and a preliminary prototype was verified using photopolymer 3D printing with resin material, confirming the feasibility and accuracy of the structural design, as shown in Figure 2(d).

[0189] 3. SLM printing

[0190] (1) Import the gradient BCC pseudo-lattice STL model designed above into the processing software of the SLM device (e.g., EOS M290).

[0191] (2) Place the model in the forming chamber along the Z-axis to minimize the support structure and ensure a high printing success rate. The software automatically generates the necessary supports.

[0192] (3) Slice the model and set the layer thickness to 50μm.

[0193] (4) Select a sandblasted 304 stainless steel substrate and preheat it to 80°C. Use recycled AlFeCoCrNi from the above-mentioned materials. 2.1 Alloy powder is used as raw material to lay a 50μm thick powder layer on the substrate.

[0194] (5) Select parameter combination #7 in Table 1 as the optimized process: laser power 250W, scanning speed 800mm / s -1 The scanning interval is 0.1 mm, the layer thickness is 30 μm, and the laser scanning direction of adjacent layers is rotated 90°.

[0195] (6) In a high-purity argon protective atmosphere with oxygen content strictly controlled at <100ppm, the SLM equipment lays powder layer by layer according to the set path, selectively melts it, and repeats the process until multiple gas diffusion layer samples with gradient BCC pseudo-lattice structure are finally integrally formed. The overall size of the sample is 18mm×5mm×3mm and 20mm×20mm×20mm.

[0196] 4. Post-processing stage

[0197] (1) A 18mm×5mm×0.5mm GDL sample with simulated crystal lattice was cut from the SLM forming substrate;

[0198] (2) Select parameter combination #1 in Table 2 for heat treatment: heat treatment temperature 600℃, heating rate 5℃ min -1 The heat preservation time is 4 hours, followed by 2℃ min. -1The temperature is slowly reduced to below 300°C, and finally cooled to room temperature along with the furnace.

[0199] 5. Performance Characterization and Test Results

[0200] (1) Residual stress: The residual stress on the surface of the SLM state was measured to be 175 MPa (tensile stress) by XRD method. After heat treatment, it was reduced to 45 MPa (tensile stress), a reduction of 74.3%.

[0201] (2) The compressive mechanical properties of the prepared GDL structure (sample size 20mm×20mm×20mm) were evaluated. The specific steps are as follows:

[0202] Quasi-static uniaxial compression tests (strain rate 1×10⁻⁶) were performed on the heat-treated pseudo-lattice GDL structure on a universal testing machine. -4 s -1 The structure exhibits excellent mechanical properties, with a compressive yield strength of 1174 MPa and a compressive strength of 1865 MPa. It did not collapse even when the strain reached 28%, as shown in Figure 4(d). It demonstrates good plasticity and energy absorption capacity, which is sufficient to meet the fastening requirements during the assembly of the electrolytic cell and the mechanical stability during long-term operation.

[0203] (3) Electrolysis performance of water:

[0204] The SLM-printed alloy block, after the above post-processing, was fabricated into a sample with dimensions of 18 mm × 5 mm × 0.5 mm. To construct a high specific surface area nanoporous structure on the surface to further enhance catalytic activity, the sample underwent electrochemical dealloying. The principle is to selectively corrode the active metal elements (such as Al) in the alloy, leaving a three-dimensional bicontinuous nanoporous framework rich in transition metals (Fe, Co, Cr, Ni). Electrochemical dealloying was performed using a dual-electrode system: working electrode: test sample; counter electrode: carbon rod; dealloying solution: 0.5 mol / L. -1 Sulfuric acid (H2SO4) was used. The dealloying experiment was conducted using CHI760e software with the following parameters set: constant voltage 4V for 60 minutes. The morphology after dealloying is shown in Figure 3(d). The tests were performed using a standard three-electrode system in 1.0M KOH electrolyte.

[0205] 1) Hydrogen evolution reaction performance:

[0206] a. Polarization curve: As shown in Figure 8(a), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 126mV, which is far below the invention target (≤150mV).

[0207] b. The slope of Tafel is 114.3 mV dec -1 As shown in Figure 8(b), this indicates that its HER reaction kinetics are rapid.

[0208] c. Stability: As shown in Figure 8(c), at 50 mA cm -2 After continuous electrolysis for 120 hours at a constant current density, the activity decay rate was approximately 3.0%, demonstrating excellent long-term stability. This stability verifies its durability under simulated renewable energy fluctuation input conditions.

[0209] 2) Oxygen evolution reaction performance:

[0210] a. Polarization curve: As shown in Figure 8(d), the polarization curve was measured at 50 mA cm⁻¹. -2 Overpotential (η) at current density 50 The value was 263mV, which is better than the invention target (≤300mV).

[0211] b. The slope of Tafel is 104.1 mV dec -1 As shown in Figure 8(e), it demonstrates excellent OER reaction kinetics.

[0212] c. Stability: As shown in Figure 8(f), at 50 mA cm -2 After operating continuously for 120 hours at high current density, the activity decay rate was approximately 2.3%, meeting the stability requirements. This indicates that the electrode structure can effectively resist damage caused by reverse polarity and sudden potential changes due to power fluctuations.

[0213] This embodiment addresses the gas-liquid transport management challenges faced by electrolyzers directly coupled with fluctuating renewable energy sources such as wind and solar power under dynamic and variable load conditions. By designing a gradient BCC lattice structure, precise control of the pore structure from the catalyst layer-film interface (bottom) to the flow channel side (top) is achieved: a 150μm thin rod diameter at the bottom forms a dense region to maximize the electrochemical active area and optimize current collection, while a 450μm thick rod diameter at the top constitutes an open region, providing a low-resistance channel for the rapid nucleation, convergence, and escape of reactant gases (H2 / O2). This approach effectively solves the "liquid flooding" problem that easily occurs in traditional homogeneous porous electrodes when current density changes frequently. The system addresses two main failure modes: "" (active sites are covered by electrolyte at low current) and "drying out" (air blockage hinders electrolyte replenishment at high current). Simultaneously, a 600℃ low-temperature heat treatment strategy effectively relaxes most residual stress (reducing it by 74.3%) and ensures component dimensional stability. It also consciously preserves the non-equilibrium fine-grained structure and high-density crystal defects unique to SLM ultrafast solidification as highly active catalytic sites. This ensures high intrinsic catalytic activity of the electrode under dynamic conditions and prevents microcrack initiation during frequent thermal cycling through appropriate stress relief, perfectly solving the balance between catalytic activity and structural durability. Ultimately, the synergistic application of the aforementioned technical features enables the GDL in this embodiment to exhibit excellent adaptability to operating conditions and rapid response capabilities: excellent HER reaction kinetics (Tafel slope 114.3 mV / dec) ensures rapid start-up of efficient hydrogen production during surges in renewable energy power, while the optimal gas-liquid management capability brought by the gradient pore structure guarantees stable operation of the electrode over a wide current density range, providing core electrode technology support for building an efficient, robust, and long-life green hydrogen production system that seamlessly integrates with intermittent renewable energy sources.

[0214] To clearly compare and demonstrate the overall performance of the present invention, the key data of the compressive mechanical properties and electrolytic water catalytic performance of the above four embodiments are summarized in Tables 3 and 4, respectively.

[0215] Table 3 Summary of compressive mechanical properties of the four embodiments

[0216]

[0217] Table 4 Summary of the electrochemical performance of the four examples

[0218]

[0219] As shown in Tables 3 and 4, although the four implementation cases differ in their lattice-like structure design, SLM, and heat treatment process parameters, the EHEA-GDLs they prepared all exhibited excellent overall performance.

[0220] First, regarding mechanical properties (see Table 3), the compressive yield strength of all samples ranged from 800 MPa to 2000 MPa, and the compressive strength was above 1200 MPa, reaching a maximum of 2983 MPa, while maintaining a plastic strain rate of 22% to 32%. This indicates that the GDL prepared by this invention has extremely high structural stability, sufficient to withstand the assembly pressure of the electrolytic cell and the physical stress during long-term operation, solving the problem of easy collapse and peeling of traditional porous electrodes or catalytic coatings.

[0221] Secondly, regarding electrochemical catalytic performance (see Table 4), all implementation examples achieved the invention objectives in both the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER). Specifically, 50 mA cm⁻¹ -2 HER overpotential (η) at current density 50 The overpotential (η) is between 76mV and 143mV, far exceeding the design requirement of ≤150mV; 50 The voltage range is between 253mV and 279mV, significantly better than the design requirement of ≤300mV. The corresponding Tafel slope is also at a low level (HER: 114.3-164.3mV dec). -1 OER: 61.2-104.1mV dec -1 This demonstrates its rapid catalytic reaction kinetics. More importantly, all samples showed rapid catalytic reaction kinetics at 10 mA cm⁻¹. -2 After 120 hours of continuous operation at current density, the activity decay rate was less than 5% (data shown in Table 4), demonstrating excellent long-term operational stability.

[0222] Comprehensive analysis shows that this invention, through specific component design (AlFeCoCrNi), 2.1 By optimizing the range of SLM preparation process parameters, subsequent heat treatment regime, and flexible spatial structure design, an EHEA catalytic electrode with low residual stress, unique microstructure, and excellent water electrolysis catalytic performance (low overpotential, small Tafel slope, and high stability) was successfully fabricated. This invention is the first to apply SLM additive manufacturing technology to the integrated forming of a high-entropy alloy catalytic electrode with a multi-level porous structure, solving problems such as high interfacial impedance between the catalytic layer and diffusion layer, poor mechanical stability, and limited mass transfer in traditional electrodes. It provides a novel technical route for the fabrication of high-performance, long-life AEMWE electrolyzers and has promising prospects for industrial application.

[0223] To further demonstrate the positive effects of the above embodiments, the present invention conducts the following experiments based on the above technical solutions.

[0224] First, at the material design level, this invention achieves a breakthrough in the intrinsic performance of catalytic materials through an eutectic high-entropy alloy (EHEA) system. Traditional non-precious metal catalysts generally face the dilemma of balancing activity and stability: single transition metals have limited activity and are easily dissolved, while conventional multi-element alloys are prone to elemental segregation and phase separation, leading to activity decay. The EHEA components used in this invention, such as AlFeCoCrNi2.1, utilize their unique high-entropy effect, lattice distortion effect, and slow diffusion effect to fundamentally suppress the precipitation of harmful phases and promote synergistic catalytic effects among elements. More importantly, its unique two-phase eutectic structure provides an ideal precursor for subsequent electrochemical dealloying, enabling the in-situ construction of a three-dimensional nanoporous catalytic framework with both high specific surface area and excellent stability. This fundamentally resolves the core contradiction between low cost and the incompatibility of high performance and high stability in non-precious metal catalysts.

[0225] Secondly, at the structural manufacturing level, this invention achieves integrated design and manufacturing of "material-structure-function" through selective laser melting (SLM) technology, completely revolutionizing the traditional electrode construction mode. Existing technologies generally employ a step-by-step process of "preparing the diffusion layer first, then coating the catalyst," inevitably introducing problems such as interfacial impedance, weak bonding, and thermal expansion mismatch between the catalyst layer and the substrate. This invention creatively utilizes SLM technology to directly form EHEA materials with catalytic potential into a precisely programmed lattice-like three-dimensional porous structure (GDL). This integrated manufacturing mode not only eliminates the physical interface and achieves seamless and efficient electron / mass transfer, but also integrates the catalytic active sites with the macroscopic conductive and mass transfer framework, achieving a mechanical bonding strength equivalent to that of the bulk material. This fundamentally solves the problems of easy catalyst layer detachment, high interfacial resistance, and interfacial failure under long-term operation.

[0226] Finally, in terms of performance and applicability, this invention demonstrates excellent comprehensive performance and broad adaptability to various scenarios through flexible synergistic control of "composition-process-structure". As shown in the various embodiments and the data in Tables 3 and 4, the EHEA-GDL series products prepared by this invention have mechanical strength (yield strength 810-1903MPa) far exceeding that of traditional carbon-based or sintered metal GDL, completely solving their assembly crushing and long-term mechanical failure problems; their catalytic activity (HER overpotential 76-143mV, OER overpotential 253-279mV) and stability (120-hour decay rate <5%) are comparable to or even better than those of noble metal benchmarks. Most importantly, by optimizing the structure (such as BCC, FCC, composite, gradient lattice) and post-processing (such as heat treatment at 800-1000℃), this invention can directionally prepare special electrodes suitable for different application scenarios such as industrial-grade high robustness, high-efficiency mass transfer, ultra-high power density, and dynamic operating conditions, providing unprecedented customization capabilities and a solid material and device foundation for the diversified and high-performance development of AEMWE electrolyzer technology.

[0227] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any modifications, equivalent substitutions, and improvements made by those skilled in the art within the scope of the technology disclosed in the present invention, and within the spirit and principles of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolyzer, characterized in that, This method Includes the following steps: S1, prepared by gas atomization method, has the composition AlFeCoCrNi. 2.1 The preparation of the eutectic high-entropy alloy spherical powder includes: After weighing the metal raw material with an atomic ratio of Al:Fe:Co:Cr:Ni=1:1:1:1:2.1, it was ultrasonically cleaned with alcohol and dried to remove surface contaminants. The pretreated metal raw materials are placed in a vacuum induction melting furnace for vacuum induction melting. The melting temperature is controlled at 150-300℃ above the alloy liquidus line, and the melting is repeated 4-6 times. Spherical alloy powder was prepared by high-pressure gas atomization under an argon atmosphere of 2-8 MPa, and eutectic high-entropy alloy spherical powder with a particle size of 15-53 μm was obtained by sieving. S2, using SLM technology, a model with a three-dimensional pseudo-lattice superstructure is established under optimized parameters; the pseudo-lattice superstructure adopts a face-centered cubic, body-centered cubic, or multiphase mosaic composite form, with a rod diameter of 100-500μm and a porosity of 50-80%; S3, using selective laser melting technology, under a protective atmosphere, the eutectic high-entropy alloy spherical powder is integrally formed into a gas diffusion layer component according to the model; S4. The gas diffusion layer component is heat-treated, and then electrochemically dealloyed in an acidic solution to form a three-dimensional bicontinuous nanoporous structure on the surface. The heat treatment is carried out under vacuum, with the temperature increased to 600-1100℃ at a rate of 5℃ / min and held for 1-6 hours. After the holding period, the temperature is decreased to below 300℃ at a rate of 2℃ / min and then cooled to room temperature in the furnace. The electrochemical dealloying process uses a dual electrode, with a constant voltage of 4V applied for 60 minutes in a 0.5mol / L sulfuric acid solution.

2. The method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolytic cell according to claim 1, characterized in that, In step S1, before the metal raw material is subjected to vacuum induction melting, the oxygen content in the furnace is reduced to 10% by vacuuming and argon purging circulation. -2 Below Pa.

3. The method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolytic cell according to claim 1, characterized in that, In step S3, the eutectic high-entropy alloy spherical powder is integrally formed into a gas diffusion layer component according to the model, including: Design a 3D model of a lattice structure using CAD software and convert it into a standard triangulation language file; Based on the minimum requirements of Z-axis height, surface roughness, and support structure, the optimal manufacturing direction is adjusted, and the support structure is generated. The model file is sliced ​​into layers of equal thickness according to the set thickness, and the sliced ​​data is transmitted to the SLM device; The 304 stainless steel substrate is preheated at a temperature of 80-120℃, and then a layer of metal with a thickness of 20-50μm is uniformly deposited on the preheated substrate. A high-energy-density laser beam selectively melts metal powder in the xy plane according to path planning data; A powder-spreading scraper spreads another layer of metal powder on the processed layer. The laser beam selectively melts the powder based on the slice data of the next layer. The powder spreading is repeated until a gas diffusion layer component is obtained.

4. The method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolytic cell according to claim 3, characterized in that, The substrate is preheated at 80-120℃, the powder coating thickness is 20-50μm, and the protective atmosphere is argon with an oxygen content of less than 100ppm. The process parameters of the selective laser melting technology are as follows: laser power 100-350W, scanning speed 600-1000mm / s, scanning spacing 0.06-0.1mm, and layer thickness 20-60μm. The overall dimensions of the gas diffusion layer component are 18mm×5mm×3mm and 20mm×20mm×20mm.

5. A eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolyzer, characterized in that, The gas diffusion layer is prepared by the method for preparing a eutectic high-entropy alloy-based gas diffusion layer for an AEMWE electrolytic cell as described in any one of claims 1-4. The material of the gas diffusion layer is AlFeCoCrNi. 2.1 It is a eutectic high-entropy alloy with a three-dimensional pseudo-lattice macroscopic porous structure and a three-dimensional bicontinuous nanoporous structure covering the surface of the macroscopic structural framework.

6. The eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells according to claim 5, characterized in that, In a 1.0M KOH electrolyte, at least one of the following performance indicators must be met: The hydrogen evolution reaction at 50 mA cm -2 Overpotential at current density ≤150mV; The oxygen evolution reaction occurs at 50 mA cm⁻¹ -2 Overpotential at current density ≤300mV; The Tafel slopes for the hydrogen evolution reaction and the oxygen evolution reaction are less than 180 mV / dec and 110 mV / dec, respectively. At 50mA cm -2 After continuous operation at current density for 120 hours, the activity decay rate of both hydrogen evolution reaction and oxygen evolution reaction does not exceed 5%.

7. The eutectic high-entropy alloy-based gas diffusion layer for AEMWE electrolytic cells according to claim 5, characterized in that, It has a multi-level porous structure, and its compressive yield strength is 800-2000MPa, compressive strength is 1000-3200MPa, and strain rate is 20-35%.

Citation Information

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