An amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode regulated by an interface and a preparation method and application thereof

Abstract

This invention relates to an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties, its preparation method, and its application. The electrode comprises: a conductive substrate; and an amorphous nickel-molybdenum-phosphorus alloy catalytic coating grown in situ on the conductive substrate; wherein the nickel-molybdenum-phosphorus alloy catalytic coating comprises the following molar percentage components: 73.3~84.4 mol% Ni, 2.3~21.0 mol% Mo, and 5.4~14.5 mol% P; the in-situ growth is carried out in a precursor solution containing a nickel source, a molybdenum source, a phosphate source, and an ammonium source, the pH of the precursor solution being 2~3, and the ammonium source being ammonium chloride. This invention solves the problems of decreased activity and insufficient stability of existing nickel-molybdenum-based catalysts under high current density and fluctuating operating conditions.

Description

Technical Field

[0001] This invention relates to the field of water electrolysis for hydrogen production technology, and in particular to an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface controlled, its preparation method, and its application. Background Technology

[0002] With the global energy structure transformation and the advancement of the "dual carbon" goal, hydrogen energy, as a clean and efficient secondary energy source, has become a research hotspot in the energy field. Alkaline water electrolysis (AWE) is one of the mainstream technologies for large-scale hydrogen production due to its mature technology and relatively low cost. However, under dynamic operating conditions driven by renewable energy sources (such as wind and solar power), AWE systems often face challenges such as frequent start-stop cycles and power fluctuations. This leads to problems such as structural degradation, dissolution of active components, and catalytic activity decay of electrode materials under conditions such as reverse current and potential cycling, which seriously restricts its long-term stable operation under fluctuating conditions.

[0003] Currently, platinum-based catalysts are widely studied due to their excellent hydrogen evolution reaction (HER) activity, but their high cost and scarcity limit their large-scale industrial application. Nickel-based catalysts are considered potential alternatives due to their abundant resources, low cost, and good conductivity. Among them, nickel-molybdenum alloys have attracted much attention due to their good HER catalytic activity; however, in actual operation, molybdenum is prone to dissolution and precipitation in alkaline media, leading to the gradual loss of active sites and insufficient stability, making it difficult to meet the requirements of long-term dynamic operation. Summary of the Invention

[0004] The purpose of this invention is to provide an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface control, its preparation method and application, which solves the problems of decreased activity and insufficient stability of existing nickel-molybdenum-based catalysts under high current density and fluctuating operating conditions.

[0005] To achieve the above objectives, the technical solution adopted by this invention is: an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties, comprising: Conductive substrate; and An amorphous nickel-molybdenum-phosphorus alloy catalytic coating grown in situ on the conductive substrate; The nickel-molybdenum-phosphorus alloy catalytic coating comprises the following components in molar percentage: 73.3–84.4 mol% Ni, 2.3–21.0 mol% Mo, and 5.4–14.5 mol% P; The in-situ growth is carried out in a precursor solution containing a nickel source, a molybdenum source, a phosphate source, and an ammonium source. The pH of the precursor solution is 2-3, and the ammonium source is ammonium chloride.

[0006] Furthermore, the thickness of the amorphous nickel-molybdenum-phosphorus alloy catalytic coating is 20~45μm.

[0007] Furthermore, the conductive substrate is nickel foam or nickel mesh.

[0008] A second aspect of this invention provides a method for preparing an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface controlled characteristics, comprising the following steps: S1: Pretreatment of the conductive substrate; S2: Nickel source, molybdenum source, phosphate source and ammonium source are mixed and dissolved in a solvent, the temperature is raised and the pH value of the solution is adjusted to obtain an electrodeposition precursor solution; S3: Using the pretreated conductive substrate as the working electrode, place it in the electrodeposition precursor solution, and simultaneously use a platinum sheet as the counter electrode to perform electrochemical deposition. S4: The electrode after electrochemical deposition is removed, washed with deionized water and dried to obtain the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode.

[0009] Further, in step S1, the pretreatment involves sequentially cleaning the conductive substrate in anhydrous ethanol and hydrochloric acid for 5-20 minutes, and then sonicating it in distilled water for 10-20 minutes.

[0010] Further, in step S2, the nickel source is one or more selected from nickel sulfate and nickel chloride; the molybdenum source is sodium molybdate; and the phosphoric acid source is sodium hypophosphite.

[0011] Further, in step S2, the solvent is water, and the temperature of the electrodeposition precursor solution is 25~35℃.

[0012] Further, in step S2, the nickel ion concentration in the electrodeposition precursor solution is 0.1~0.25 mol / L; the molybdenum ion concentration is 1~5 mmol / L; and the phosphorus ion concentration is 0.1~0.25 mol / L.

[0013] Furthermore, in step S3, the current density for electrochemical deposition is -20 to -100 mA / cm². 2 The deposition time is 10-30 minutes.

[0014] Furthermore, in step S4, the drying temperature is 60 ℃ and the drying time is 30 min.

[0015] A third aspect of this invention provides the application of an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface controlled properties in the alkaline water electrolysis hydrogen evolution reaction.

[0016] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art: Through the synergistic effect of phosphorus doping and ammonium additives, comprehensive control over the catalyst's surface morphology, crystallinity, and internal stress was achieved. Phosphorus doping optimized the surface morphology and crystallinity, while ammonium effectively refined the grain size of the catalyst layer. This enhanced the interfacial bonding between the catalyst and the substrate and promoted the alloying of P and NiMo. The synergistic effect of both significantly improved the electrode's hydrogen evolution activity while also providing excellent mechanical and chemical stability.

[0017] The resulting amorphous alloy coating has a dense structure and a strong bond with the substrate, which can effectively inhibit the dissolution and loss of active components (especially molybdenum) in strongly alkaline media and under dynamic operating conditions, thereby significantly extending the service life of the electrode during long-term operation.

[0018] The electrode maintains excellent catalytic activity and structural integrity even under harsh conditions such as frequent start-stop and high current density, exhibiting good dynamic response and resistance to reverse current impact, making it particularly suitable for renewable energy-driven fluctuating water electrolysis hydrogen production systems.

[0019] Furthermore, by employing a one-step electrodeposition method to grow a catalytic layer in situ on a commonly used conductive substrate, the process is simple, the conditions are mild, and the raw materials are readily available, making it suitable for large-scale preparation. Attached Figure Description

[0020] The following sections will describe some specific embodiments of the invention in detail by way of example and not limitation, with reference to the accompanying drawings. The same reference numerals in the drawings denote the same or similar parts or portions. Those skilled in the art should understand that these drawings are not necessarily drawn to scale. In the drawings: Figure 1 The graphs show the current density potential curves of the electrodes in Embodiment 1 and Comparative Examples 1-3 of the present invention in a three-electrode system. Figure 2 The potential-time curves for steady-state testing of the electrodes prepared in Example 1 and Comparative Examples 1-3 of this invention are shown. Figure 3 Intermittent potential start-up-shutdown curves for transient testing of the electrodes prepared in Example 1 and Comparative Examples 1-3 of this invention; Figure 4 X-ray diffraction patterns of the electrodes prepared in Example 1 and Comparative Examples 1-3 of this invention; Figure 5 The images show the surface morphology of the electrodes prepared in Example 1 and Comparative Example 3 of this invention before and after ultrasound. Figure 6 The image shows the elemental proportions of the electrodes prepared in Example 1 and Comparative Example 3 of this invention before and after immersion using scanning electron microscopy-energy dispersive spectroscopy (EDS). Figure 7X-ray photoelectron spectroscopy analysis of the electrodes prepared in Example 1 and Comparative Example 3 of this invention. Detailed Implementation

[0021] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] Furthermore, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other. Example 1

[0023] This embodiment provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface controlled, and its preparation method, specifically including the following steps: S1: Cut the nickel foam into 1*1cm pieces. 2 The small pieces were sequentially washed in anhydrous ethanol and hydrochloric acid for 15 minutes, and then ultrasonically washed in distilled water for 20 minutes to obtain the pretreated nickel foam substrate.

[0024] S2: Add 0.25 mol nickel chloride hexahydrate, 5 mmol sodium molybdate, 0.25 mol sodium hypophosphite monohydrate and 0.25 mol ammonium chloride to a 1 L beaker, add deionized water to make up to 1 L, stir well, adjust the pH of the solution to 2, and raise the temperature of the solution to 30℃ to obtain the electrodeposition precursor solution.

[0025] S3: Electrochemical deposition was performed using a three-electrode system. The pretreated nickel foam from step S1 was used as the working electrode, a platinum sheet as the counter electrode, and an Ag / AgCl electrode as the reference electrode, all placed in the precursor solution prepared in step S2. The electrode was set at -80 mA / cm². 2 Deposit at the current density for 15 min.

[0026] S4: After deposition, the electrode is removed, rinsed with deionized water, and dried at 60 °C for 30 min to obtain the interface-controlled amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode of this embodiment. EDX measurements showed that the molar percentages of phosphorus, nickel, and molybdenum in the deposited coating were 8.46%, 84.39%, and 7.15%, respectively. Example 2

[0027] This embodiment provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface control and its preparation method. The preparation method is basically the same as that in Example 1, except that the amount of nickel chloride hexahydrate added in the electroplating solution in Example 2 is 0.1 mol, the amount of sodium molybdate added is 1 mmol / L, and the amount of sodium hypophosphite monohydrate added is 0.1 mol. Example 3

[0028] This embodiment provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface control and its preparation method. The preparation method is basically the same as that in Example 1, except that the amount of nickel chloride hexahydrate added in the electroplating solution of Example 3 is 0.15 mol, the amount of sodium molybdate added is 3 mmol / L, and the amount of sodium hypophosphite monohydrate added is 0.15 mol. Example 4

[0029] This embodiment provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled surface and interface, and its preparation method. The preparation method is basically the same as that in Example 1, except that the current density of the electrochemical deposition reaction in Example 4 is -40 mA / cm². 2 The deposition time was 30 minutes. Comparative Example 1

[0030] This embodiment provides a hydrogen evolution electrode and its preparation method, which is basically the same as the preparation method of Example 1, except that sodium hypophosphite monohydrate and ammonium chloride are not added when preparing the precursor solution in step S2. Comparative Example 2

[0031] This embodiment provides a hydrogen evolution electrode and its preparation method, which is basically the same as the preparation method of Example 1, except that sodium hypophosphite monohydrate is not added when preparing the precursor solution in step S2. Comparative Example 3

[0032] This embodiment provides a hydrogen evolution electrode and its preparation method, which is basically the same as the preparation method of Example 1, except that: ammonium chloride is not added when preparing the precursor solution in step S2. Comparative Example 4

[0033] This example provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface control and its preparation method. The preparation method is basically the same as that in Example 1, except that in step S2, the amount of nickel chloride hexahydrate added to the precursor solution is 0.05 mol, the amount of sodium molybdate added is 3 mmol / L, and the amount of sodium hypophosphite monohydrate added is 0.2 mol.

[0034] Ultimately, EDX measured the molar percentages of phosphorus, nickel, and molybdenum in the deposited coating to be 23.5%, 65.9%, and 10.6%, respectively. Comparative Example 5

[0035] This example provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface control and its preparation method. The preparation method is basically the same as that in Example 1, except that in step S2, the amount of nickel chloride hexahydrate added to the precursor solution is 0.35 mol, the amount of sodium molybdate added is 3 mmol / L, and the amount of sodium hypophosphite monohydrate added is 0.1 mol.

[0036] Ultimately, EDX measured the molar percentages of phosphorus, nickel, and molybdenum in the deposited coating to be 7.6%, 88.3%, and 4.1%, respectively. Comparative Example 6

[0037] This example provides an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface control and its preparation method. The preparation method is basically the same as that in Example 1, except that in step S2, ammonium sulfate is used instead of ammonium chloride in the same molar amount. Performance testing and results analysis:

[0038] To verify the excellent performance of the electrodes prepared in the embodiments of the present invention, a series of tests were conducted on the electrodes prepared in Examples 1-4 and Comparative Examples 1-3.

[0039] (1) Overpotential test Linear sweep voltammetry tests were performed on Examples 1-4 and Comparative Examples 1-3 using a three-electrode system in a 1 M KOH electrolyte at 65 °C, and the current density (A / cm²) was calculated. 2 Overpotentials under certain conditions were obtained, as shown in Table 1 and Figure 1 data, Figure 1 These are the LSV curves for Example 1 and Comparative Examples 1-3. The results are as follows... Figure 1 As shown, the electrode in Example 1 requires only a 175 mV overpotential to drive -1 A / cm. 2 The current density of the catalyst was significantly higher than that of Comparative Example 1 (344 mV), Comparative Example 2 (272 mV), and Comparative Example 3 (243 mV). This indicates that the synergistic introduction of phosphorus and ammonium effectively optimized the electronic structure and surface properties of the catalyst, significantly improving the hydrogen evolution reaction activity. Comparing Example 1 and Comparative Example 6, it is evident that adding NH4Cl to the precursor solution resulted in a lower and more stable pH value during deposition, which is beneficial for enhancing the hydrogen evolution reaction activity.

[0040] Table 1 Performance of electrodes in Examples 1-4 and Comparative Examples 1-6 <![CDATA[HER overpotential (mV @ 1000 mA / cm 2 )]]> Example 1 175 Example 2 205 Example 3 221 Example 4 231 Comparative Example 1 344 Comparative Example 2 272 Comparative Example 3 243 Comparative Example 4 265 Comparative Example 5 292 Comparative Example 6 277 (2) Steady-state operation stability test At 1000 mA / cm 2Long-term steady-state operation tests were conducted under constant current density, and the results are as follows: Figure 2 As shown, the anion exchange membrane water electrolyzer using the electrode of Example 1 as the cathode exhibited a voltage increase of only slightly from 1.845 V to 1.864 V during a 240-hour operating period, with a decay rate as low as 0.08 mV / h. In contrast, the electrolyzer using the electrode of Comparative Example 1 rapidly increased its voltage from 2.298 V to 2.418 V within 24 hours, with a decay rate as high as 5.0 mV / h; the electrolyzer using the electrode of Comparative Example 2 increased its voltage from 1.951 V to 2.002 V within 24 hours, with a decay rate of 2.08 mV / h; and the electrolyzer using the electrode of Comparative Example 3 increased its voltage from 2.015 V to 2.087 V within 24 hours, with a decay rate of 2.96 mV / h. This demonstrates that the electrode prepared in Example 1 of this invention possesses excellent long-term operational stability.

[0041] (3) Accelerated stress test (AST) Accelerated stress testing was conducted to simulate fluctuating operating conditions driven by renewable energy sources. The test mode was 1000 mA / cm². 2 After running for 10 seconds, maintain 0 V for 10 seconds, and repeat this cycle. The result is as follows: Figure 3 As shown, the current density of Comparative Example 1 electrode decreased to 60% and 36% of its initial value after 5,000 and 10,000 start-stop cycles, respectively; the current density of Comparative Example 2 electrode decreased to 66% and 61% of its initial value after 5,000 and 10,000 start-stop cycles, respectively; and the current density of Comparative Example 3 electrode decreased to 82% and 75% of its initial value after 5,000 and 10,000 start-stop cycles, respectively. In contrast, the current density of Example 1 electrode hardly decreased in the same tests, demonstrating excellent mechanical and chemical stability and strong adaptability to dynamic operating conditions.

[0042] (4) Structural characterization and mechanical stability analysis The crystal structure of each electrode was analyzed by X-ray diffraction. Figure 4 The electrode of Comparative Example 1 exhibits typical diffraction peaks of crystalline nickel. Besides the two peaks generated by the carbon fiber substrate, the electrode prepared in Comparative Example 1 shows three diffraction peaks at 44.5°, 51.8°, and 76.3°, corresponding to the (111), (200), and (220) crystal planes of metallic nickel, respectively. The diffraction peaks of the electrode of Comparative Example 3 are significantly broadened, with a lower intensity at 44.5°, while the diffraction peaks at 51.8° and 76.3° disappear, indicating the formation of an amorphous nickel-molybdenum-phosphorus alloy. The diffraction peak intensities of the electrodes of Example 1 and Comparative Example 2 are increased and sharper, indicating that the introduction of ammonium ions refines the grains and improves crystallinity, which helps to enhance mechanical stability.

[0043] To further investigate mechanical stability, each electrode was subjected to ultrasonic treatment and its surface morphology changes were observed. Figure 5 ).

[0044] Before ultrasound, the electrode of Comparative Example 1 ( Figure 5 a1) exhibits a thin film morphology with cracks and loose particles on its surface; Comparative Example 2 electrode ( Figure 5 b1) Surface cracks are reduced, and particles are more densely packed; Comparative Example 3 electrode ( Figure 5 c1) The surface is relatively smooth.

[0045] After ultrasound, comparative examples 1-3 electrodes ( Figure 5 a2~ Figure 5 The nickel foam substrate of c2) was exposed to varying degrees, and the coating peeled off. However, the electrode of Example 1 ( Figure 5 The coating morphology of d2) remained intact after ultrasonication, proving that the synergistic effect of ammonium and phosphorus significantly enhanced the adhesion between the coating and the substrate and the overall mechanical strength.

[0046] (5) High chemical stability test Each electrode was immersed in 30% KOH solution at 85℃ for 24 hours, and the elemental changes were analyzed by energy dispersive spectroscopy (EDS). Figure 6 After immersion, the atomic percentage of molybdenum in the electrodes of Comparative Example 1 and Comparative Example 2 decreased sharply from 19.89% and 20.73% to 0.44% and 5.71%, respectively, indicating severe dissolution and loss of molybdenum. In contrast, the molybdenum content in the electrodes of Comparative Example 3 and Example 1 remained relatively stable. Furthermore, the retention rate of phosphorus in the electrode of Example 1 was significantly higher than that in the electrode of Comparative Example 3. This demonstrates that phosphorus doping effectively inhibits molybdenum dissolution, while the further introduction of ammonium ions synergistically reduces the loss of both phosphorus and molybdenum.

[0047] (6) X-ray photoelectron spectroscopy (XPS) test X-ray photoelectron spectroscopy analysis ( Figure 7 This further confirms the above conclusion.

[0048] In the Ni 2p spectrum, the electrodes prepared in Comparative Example 3 and Example 1 both exhibited characteristic Ni values ​​at 853.0 and 870.2 eV, respectively. 0 The peaks, and the two characteristic responses at 856.7 and 874.3 eV, indicate the presence of Ni. 2+ After the immersion test, the Ni content in the electrode prepared in Comparative Example 3 was... 2+ The proportion of characteristic signals increased significantly, while the electrode prepared in Example 1 remained almost unchanged.

[0049] In the Mo 3d spectra, both samples showed Mo 3d... 3 / 2 and Mo 3d 5 / 2 The two peaks can be identified as Mo.6+ (231.8 and 235.1 eV), Mo 4+ (230.3 and 232.8 eV) and Mo 0 (229.1 and 231.6 eV). In the electrode of Example 1, only Mo after immersion test 0 The weakened signal indicates slight oxidation on its surface. However, for Comparative Example 3, only Mo was present. 6+ The signal peaks indicate that the Mo elements on its surface have undergone severe dissolution and oxidation.

[0050] In the P 2p spectrum, compared with Comparative Example 3, the electrode prepared in Example 1 showed additional double peaks at 129.5 and 130.4 eV, which can be attributed to the P 2p... 3 / 2 and P 2p 1 / 2 This indicates that the addition of ammonium ions is beneficial for the alloying of phosphorus with other metals. Furthermore, the continued observation of metallic phosphorus bonds after immersion testing further demonstrates the high chemical stability of the electrode prepared in Example 1.

[0051] The above embodiments are only for illustrating the technical concept and features of the present invention. Their purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly. They should not be used to limit the scope of protection of the present invention. All equivalent changes or modifications made in accordance with the spirit and essence of the present invention should be covered within the scope of protection of the present invention.

Claims

1. An amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties, characterized in that, include: Conductive substrate; as well as An amorphous nickel-molybdenum-phosphorus alloy catalytic coating grown in situ on the conductive substrate; The nickel-molybdenum-phosphorus alloy catalytic coating comprises the following components in molar percentage: 73.3–84.4 mol% Ni, 2.3–21.0 mol% Mo, and 5.4–14.5 mol% P; The in-situ growth is carried out in a precursor solution containing a nickel source, a molybdenum source, a phosphate source, and an ammonium source. The pH of the precursor solution is 2-3, and the ammonium source is ammonium chloride.

2. The amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled surface and surface regulation according to claim 1, characterized in that, The thickness of the amorphous nickel-molybdenum-phosphorus alloy catalytic coating is 20~45μm.

3. The amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled surface and surface as described in claim 1, characterized in that, The conductive substrate is nickel foam or nickel mesh.

4. A method for preparing an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties as described in any one of claims 1 to 3, characterized in that, Includes the following steps: S1: Pretreatment of the conductive substrate; S2: Mix and dissolve the nickel source, molybdenum source, phosphate source and ammonium source in a solvent, heat and adjust the pH of the solution to obtain an electrodeposition precursor solution; S3: Using the pretreated conductive substrate as the working electrode, place it in the electrodeposition precursor solution, and simultaneously use a platinum sheet as the counter electrode to perform electrochemical deposition. S4: The electrode after electrochemical deposition is removed, washed with deionized water and dried to obtain the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode.

5. The method for preparing the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties according to claim 4, characterized in that, In step S1, the pretreatment involves sequentially cleaning the conductive substrate in anhydrous ethanol and hydrochloric acid for 5-20 minutes, and then sonicating it in distilled water for 10-20 minutes.

6. The method for preparing the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties according to claim 4, characterized in that, In step S2, the nickel source is one or more selected from nickel sulfate and nickel chloride; the molybdenum source is sodium molybdate; and the phosphoric acid source is sodium hypophosphite.

7. The method for preparing the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled properties according to claim 4, characterized in that, In step S2, the solvent is water, and the temperature of the electrodeposition precursor solution is 25~35℃.

8. The method for preparing the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with interface-controlled surface according to claim 4, characterized in that, In step S2, the electrodeposition precursor solution contains nickel ions at a concentration of 0.1–0.25 mol / L, molybdenum ions at a concentration of 1–5 mmol / L, and phosphorus ions at a concentration of 0.1–0.25 mol / L.

9. The method for preparing the amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface controlled according to claim 4, characterized in that, In step S3, the current density for electrochemical deposition is -20 to -100 mA / cm². 2 The deposition time is 10-30 minutes.

10. The application of an amorphous nickel-molybdenum-phosphorus alloy hydrogen evolution electrode with surface and interface controlled as described in any one of claims 1 to 3 in the alkaline water electrolysis hydrogen evolution reaction.

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