A polycrystalline phase SnSe / NiSe / Ni3Se2 hybrid nanorod array material and a preparation method and application thereof

Abstract

The application discloses a kind of polycrystalline phase SnSe / NiSe / Ni3Se2 Hybrid nanorod array materials and its preparation method and application.The method is under N2 saturated atmosphere, by NaBH4Se powder is reduced to transparent solution, then SnCl2·2H2O and NaOH mixed solution, NH4F solution and foamed nickel are added, and polycrystalline phase SnSe / NiSe / Ni3Se2 Hybrid nanorod array electrocatalyst in situ grown in foamed nickel framework can be obtained by high-temperature hydrothermal reaction.The preparation process of the application is simple and environmental protection, raw material is easy to obtain, synthesis controllability is strong, product repeatability is good.The prepared advanced polycrystalline phase SnSe / NiSe / Ni3Se2 Hybrid nanorod array has specific active component and uniform morphology structure, and is easy to high-throughput preparation.Meanwhile, the uniform nanorod array structure has large specific surface area, can provide more reactive sites, and shows excellent electrocatalytic urea oxidation reaction, hydrogen evolution reaction and urea oxidation reaction assisted electrolytic water catalytic performance, provides important help for the development of high-efficiency energy-saving hydrogen production field.

Description

Technical Field

[0001] This invention relates to a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material, its preparation method and application, belonging to the field of nanomaterials and their preparation and application in catalysis. Background Technology

[0002] Against the backdrop of global energy structure transformation, hydrogen energy, due to its cleanliness, efficiency, and renewability, is considered a crucial vehicle for promoting rapid energy structure transformation and achieving environmental protection. Currently, traditional methane steam reforming for hydrogen production heavily relies on fossil fuels, releasing large amounts of carbon dioxide and failing to guarantee continuous production. In contrast, water electrolysis for hydrogen production offers significant advantages such as abundant raw materials, low carbon emissions, and environmental friendliness. The entire water electrolysis process consists of two half-reactions: the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER). The OER reaction, with its slow kinetics and high overpotential barrier, severely limits hydrogen production efficiency. Therefore, finding an advanced reaction to replace OER is crucial for advancing hydrogen production technology. Recently, the urea oxidation reaction (UOR) has attracted considerable attention due to its low theoretical thermodynamic potential (0.37V). Replacing OER with UOR in hydrogen production can significantly reduce energy consumption and achieve highly efficient energy conversion. In particular, urea is widely present in industrial wastewater; UOR can not only effectively treat wastewater but also convert urea into energy, thus achieving the dual benefits of wastewater treatment and energy production. Furthermore, in terms of screening active components for catalysts, nickel selenide possesses unique Ni... 2+ (t 2g 6 e g 2 Its electronic structure allows it to exhibit excellent electrocatalytic UOR activity, but its related catalytic activity and operational stability still need to be further improved.

[0003] Polycrystalline phase hybridization design can not only inherit the unique catalytic properties of different components, but also synergistically construct multiple active centers. In particular, polycrystalline phase hybridization interfaces often create more high-energy active sites and more compatible electron densities, which provides more possibilities for optimizing the interface electronic structure and significantly improving catalytic performance. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention aims to provide a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material, its preparation method, and its applications. The preparation method is simple to operate, with controllable reaction conditions and high reproducibility. The obtained material is a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material with an in-situ grown nickel foam framework. The SnSe / NiSe / Ni3Se2 hybrid nanorod array of the present invention shows promising application prospects in urea oxidation, hydrogen evolution reaction, and urea oxidation-assisted water electrolysis for hydrogen production.

[0005] To address the problems in the existing technology, the technical solution adopted by this invention is as follows:

[0006] A method for preparing a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material includes the following steps:

[0007] (1) Under the atmosphere of continuous N2, NaBH4 was completely dissolved in deionized water, and then Se powder was added until it was reduced to a clear and transparent solution.

[0008] (2) SnCl2·2H2O and NaOH mixed solution, NH4F solution and nickel foam were added sequentially to the clear and transparent solution in step (1), followed by hydrothermal reaction, and finally polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorods were obtained in situ vertically grown on the nickel foam skeleton.

[0009] As an improvement, the amount of NaBH4 in step (1) is 1-6 mmol, the amount of Se powder is 1-4 mmol, and the volume of deionized water is 1-6 mL.

[0010] As an improvement, in step (2), the amount of SnCl2·2H2O is 0.05 mmol, the amount of NaOH is 0.5-1.5 mmol, the amount of NH4F is 1-2 mmol, the volume of the SnCl2·2H2O and NaOH mixed solution is 1 mL, and the volume of the NH4F solution is 25 mL.

[0011] As an improvement, the temperature of the hydrothermal reaction in step (2) is 120-200°C and the reaction time is 4-12 hours.

[0012] As an improvement, the area of ​​the nickel foam mentioned in step (2) is in the range of 1×2 to 2×4 cm. 2 .

[0013] The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared by the above method is composed of orthorhombic SnSe, hexagonal NiSe and rhombohedral Ni3Se2, wherein the diameter of the SnSe / NiSe / Ni3Se2 hybrid nanorod is 100-300 nm.

[0014] Applications of any of the above-mentioned polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials as electrocatalysts in urea oxidation, hydrogen evolution reaction, and urea oxidation-assisted water electrolysis for hydrogen production.

[0015] As an improvement, in the urea oxidation-assisted water electrolysis for hydrogen production, a SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolyzer is used, achieving a 10mA drive at voltages of 1.37V and 1.54V. -2 and 100mA cm -2 .

[0016] Beneficial effects:

[0017] Compared with existing technologies, the present invention provides a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material, its preparation method, and its applications, which have the following advantages:

[0018] 1. This invention prepares an advanced polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material through a one-step hydrothermal reaction method. This material has advanced orthorhombic SnSe, hexagonal NiSe and rhombohedral Ni3Se2 polycrystalline phase structures. Moreover, its synthesis process is simple and environmentally friendly, the raw materials are easy to obtain, the synthesis is highly controllable, and the product is reproducible.

[0019] 2. The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in this invention exhibits excellent catalytic performance at high current densities in HER, UOR, and UOR-assisted water electrolysis for hydrogen production. For HER, it shows excellent catalytic performance at 10, 100, and 500 mA cm⁻¹. -2 The overpotentials at the current densities are 116mV, 237mV, and 311mV, respectively, and the Tafel slope is 39mV dec. -1 For UOR, it is at 10, 500, and 1000 mA cm -2 The voltages at the current densities are 1.31V, 1.39V, and 1.44V, respectively, and the Tafel slope is 31mV dec. -1 The further assembled SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolytic cells only require 1.41V and 1.61V to drive 10 and 100mA cm⁻¹, respectively.-2 The excellent bifunctional electrocatalytic activity is mainly due to the promoting effect of the novel heterogeneous hybrid structure design, which significantly improves the kinetics of the catalytic reaction. In particular, its outstanding electrocatalytic performance at high current densities is expected to further expand its commercial applications.

[0020] 3. In addition to employing a multi-phase hybridization strategy to regulate the microstructure of the electrocatalyst, this invention integrates the photothermal effect into the electrocatalytic reaction process by locally irradiating the catalyst surface with near-infrared light (NIR), synergistically improving the thermodynamics and interfacial electron transfer rate of the reaction, and enhancing mass transfer. For UOR, under NIR irradiation, multi-phase SnSe / NiSe / Ni3Se2 hybrid nanorods can achieve 10, 500, and 1000 mA cm⁻¹ amperes with only 1.28 V, 1.34 V, and 1.37 V. -2 The Tafel slope is 22mVdec -1 The further assembled SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolytic cells only require 1.37V and 1.54V to drive 10 and 100mA cm⁻¹, respectively. -2 Furthermore, this method of heating via localized NIR irradiation can suppress the overall temperature rise of the electrolyte, significantly reducing energy consumption and extending the stability of the electrocatalyst during long-term cycling tests. This allows the SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolyzer to operate at 100 mA cm⁻¹. -2 It can operate stably for 120 hours at a current density without significant degradation, demonstrating its ability to operate stably for a long period of time. Attached Figure Description

[0021] Figure 1 This is a SEM image of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention;

[0022] Figure 2 This is the XRD pattern of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention;

[0023] Figure 3 These are HRTEM images (a) and (b) of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention, which are further magnified.

[0024] Figure 4 This is an HADDF-STEM image of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention;

[0025] Figure 5 This is a mapping diagram of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention;

[0026] Figure 6 This is a SEM image of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 2 of this invention;

[0027] Figure 7 This is a SEM image of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 3 of this invention;

[0028] Figure 8 Here is a SEM image of the rhombohedral NiSe / Ni3Se2 hybrid nanorod array material prepared in Comparative Example 1 of this invention;

[0029] Figure 9 This is the XRD pattern of the rhombohedral NiSe / Ni3Se2 hybrid nanorod array material prepared in Comparative Example 1 of this invention;

[0030] Figure 10 The LSV polarization curves of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention and the rhombohedral NiSe / Ni3Se2 hybrid nanorod array material prepared in Comparative Example 1 are shown in the figure.

[0031] Figure 11 The graphs show the HER Tafel slope (a) and UOR Tafel slope (b) of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention and the rhombohedral NiSe / Ni3Se2 hybrid nanorod array material prepared in Comparative Example 1.

[0032] Figure 12 This is the UOR LSV polarization curve of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention under NIR near-infrared irradiation;

[0033] Figure 13 The hydrogen production performance of urea oxidation reaction-assisted water electrolysis is achieved by assembling a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention.

[0034] Figure 14 This is a stability test of a urea oxidation reaction-assisted electrolytic water electrolysis for hydrogen production, assembled from a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 of this invention. Detailed Implementation

[0035] The technical solution of the present invention will be further described in detail below through specific embodiments. However, it should be noted that the following embodiments are only used to describe the content of the invention and do not constitute a limitation on the scope of protection of the present invention.

[0036] Example 1: Preparation of polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials

[0037] (1) Under the atmosphere of continuous N2, 2 mmol NaBH4 was completely dissolved in 3 mL of deionized water, and then 1 mmol Se powder was added until it was reduced to a clear and transparent solution.

[0038] (2) Add, in sequence, the following solutions to the clear and transparent solution obtained in step (1): a mixed solution of 0.05 mmol SnCl2·2H2O and 0.5 mmol NaOH (1 mL), a 1.5 mmol NH4F solution (25 mL), and a solution with an area of ​​1×4 cm². 2 Nickel foam was then subjected to a hydrothermal reaction at 180℃ for 12 hours to finally obtain a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material.

[0039] The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 was analyzed by scanning electron microscopy. Figure 1 As shown, the prepared polycrystalline SnSe / NiSe / Ni3Se2 nanorod array is uniformly and vertically grown on a nickel foam framework with gaps between the rods.

[0040] XRD analysis was performed on the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1. Figure 2 As shown, its characteristic peaks agree well with three standard cards: orthorhombic SnSe (standard card JCPDS 48-1224), hexagonal NiSe (standard card JCPDS 75-0610), and rhombohedral Ni3Se2 (standard card JCPDS 19-0841), indicating the successful preparation of the polycrystalline structure. Furthermore, HRTEM images vividly demonstrate the multiphase structure of SnSe / NiSe / Ni3Se2, such as... Figure 3 As shown, the lattice spacings of 0.27 nm, 0.21 nm, and 0.29 nm correspond to the (101) crystal plane of the hexagonal NiSe, the (202) crystal plane of the rhombohedral Ni3Se2, and the (111) crystal plane of the orthorhombic SnSe, respectively, which is consistent with the XRD results.

[0041] The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1 was analyzed using HADDF-STEM and elemental mapping. Figure 4 (HADDF-STEM diagram) and Figure 5 As shown in the elemental mapping analysis, Ni, Se, and Sn are uniformly distributed in the nanorods.

[0042] Example 2: Preparation of polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials

[0043] Except for the amount of NaOH in step (2), which is 1.0 mmol / L, the rest is the same as in Example 1.

[0044] The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 2 was analyzed by scanning electron microscopy. Figure 6 As shown, the prepared polycrystalline SnSe / NiSe / Ni3Se2 nanorod array is uniformly and vertically grown on a nickel foam framework with gaps between the rods.

[0045] Example 3: Preparation of polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials

[0046] Except for the amount of NaOH in step (2), which is 1.5 mmol, the rest is the same as in Example 1.

[0047] The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 3 was analyzed by scanning electron microscopy. Figure 7 As shown, the prepared polycrystalline SnSe / NiSe / Ni3Se2 nanorod array is uniformly and vertically grown on a nickel foam framework with gaps between the rods.

[0048] Example 4: Preparation of polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials

[0049] (1) Under a continuous N2 atmosphere, 6 mmol NaBH4 was completely dissolved in 3 mL of deionized water, and then 2 mmol Se powder was added until it was reduced to a clear and transparent solution.

[0050] (2) Add, sequentially, a mixed solution of 0.05 mmol / L SnCl2·2H2O and 0.5 mmol / L NaOH (1 mL), 2 mmol / L NH4F solution (25 mL), and a solution with an area of ​​1×4 cm² to the clear and transparent solution obtained in step (1). 2 Nickel foam was then subjected to a hydrothermal reaction at 180°C for 6 hours to finally obtain a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material.

[0051] Example 5: Preparation of polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials

[0052] (1) Under the atmosphere of continuous N2, 2 mmol NaBH4 was completely dissolved in 3 mL of deionized water, and then 4 mmol Se powder was added until it was reduced to a clear and transparent solution.

[0053] (2) Add, sequentially, a mixed solution of 0.05 mmol / L SnCl₂·2H₂O and 0.5 mmol / L NaOH (1 mL), 2 mmol / L NH₄F solution (25 mL), and 2 × 4 cm⁻¹ to the clear and transparent solution obtained in step (1). 2 Nickel foam was then subjected to a hydrothermal reaction at 180°C for 6 hours to finally obtain a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material.

[0054] Comparative Example 1: Preparation of rhombohedral NiSe / Ni3Se2

[0055] (1) Under the atmosphere of continuous N2, 2 mmol NaBH4 was completely dissolved in 3 mL of deionized water, and then 1 mmol Se powder was added until it was reduced to a clear and transparent solution.

[0056] (2) Add 0.5 mmol NaOH solution (1 mL), 1.5 mmol NH4F solution (25 mL), and a solution with an area of ​​1 × 4 cm² to the clear and transparent solution obtained in step (1). 2 Nickel foam was then subjected to a hydrothermal reaction at 180℃ for 12 hours to finally obtain a rhombohedral NiSe / Ni3Se2 hybrid nanorod array material.

[0057] Scanning electron microscopy and XRD analysis were performed on the rhombohedral NiSe / Ni3Se2 hybrid nanorod array material prepared in Example 1. Figure 8 As shown in the scanning electron microscope image, the prepared rhombohedral NiSe / Ni3Se2 hybrid nanorod array is grown on a nickel foam framework, and the morphology of the rods is relatively irregular. Figure 9 The image shows the XRD pattern of the rhombohedral NiSe / Ni3Se2 hybrid nanorod array material. The characteristic peaks correspond to the rhombohedral NiSe (standard card JCPDS18-0887) and the rhombohedral Ni3Se2 (standard card JCPDS19-0841), indicating the successful preparation of the rhombohedral NiSe / Ni3Se2.

[0058] Example 6: Application of polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array materials as electrocatalysts in HER, UOR, and UOR-assisted water electrolysis for hydrogen production.

[0059] Using a CHI 660E electrochemical workstation, performance tests were conducted in HER, UOR, and UOR-assisted water electrolysis for hydrogen production in 1.0M KOH, 1.0M KOH+0.5M urea, and 1.0M KOH+0.5M urea electrolytes, respectively.

[0060] For HER and UOR, the polycrystalline SnSe / NiSe / Ni3Se2 and rhombohedral NiSe / Ni3Se2 (0.25 cm × 0.25 cm) grown on a nickel foam framework prepared in Example 1 were used as working electrodes, and a graphite rod electrode and a Hg / HgO electrode were used as the counter electrode and reference electrode, respectively. Linear sweep voltammetry (LSV) curves were obtained in potential windows of -0.8 to -1.5 V (HER) and 0.1 to 0.7 V (UOR), respectively. The LSV curves were compensated with iR to eliminate the influence of solution impedance.

[0061] For UOR-assisted water electrolysis for hydrogen production, the polycrystalline SnSe / NiSe / Ni3Se2 grown on a nickel foam framework prepared in Example 1 was used as the cathode and anode for electrocatalytic testing.

[0062] Figure 10 a and Figure 10 b represents the HER and UOR LSV polarization curves for the polycrystalline SnSe / NiSe / Ni3Se2 and rhombohedral NiSe / Ni3Se2, respectively. It can be seen that, compared to the rhombohedral NiSe / Ni3Se2 control sample, the polycrystalline SnSe / NiSe / Ni3Se exhibits higher current density and lower voltage in both HER and UOR reactions, highlighting its superior HER and UOR catalytic activity. The Tafel slope is an important parameter reflecting reaction kinetics. To further reveal the relative reaction kinetics of the polycrystalline SnSe / NiSe / Ni3Se2 and rhombohedral NiSe / Ni3Se2, the relevant Tafel slopes were calculated.

[0063] like Figure 11 a and Figure 11 As shown in b, the Tafel slopes of the polycrystalline phases SnSe / NiSe / Ni3Se in the HER and UOR reactions are 39 mV dec, respectively. -1 and 31mV dec -1 It is significantly lower than the Tafel slope of the rhombohedral NiSe / Ni3Se (the Tafel slope of HER is 82 mV dec). -1 The Tafel slope of UOR is 45mV dec. -1 This indicates that the polycrystalline SnSe / NiSe / Ni3Se2 exhibits faster HER and UOR reaction kinetics.

[0064] When NIR light is irradiated on the SnSe / NiSe / Ni3Se2 surface, its UOR performance is significantly improved. Figure 12 UOR LSV polarization curves are presented under no NIR irradiation and under different NIR irradiation intensities. As the NIR irradiation intensity increases from NIR1 to NIR2, NIR3, and NIR4, the UOR catalytic performance of the polycrystalline SnSe / NiSe / Ni3Se2 reaches its optimal level, requiring only 1.28V, 1.34V, and 1.37V to achieve 10, 500, and 1000 mA cm⁻¹, respectively. -2 It outperforms performance without NIR irradiation.

[0065] Furthermore, under NIR4 irradiation, the SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolytic cells constructed from the polycrystalline SnSe / NiSe / Ni3Se2 phase require only 1.37V and 1.54V to drive 10 and 100mA cm⁻¹ electrolytic cells, respectively. -2 This is far superior to the performance without NIR irradiation (1.41V and 1.61V) (e.g. Figure 13 As shown in the figure, the introduction of the photothermal effect significantly enhances the intrinsic catalytic activity of the catalyst. Simultaneously, under NIR4 irradiation, the SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolyzer can achieve an efficiency of 100 mA cm⁻¹. -2 It operated stably for 120 hours at a current density without significant voltage decay, demonstrating the significant promoting effect of photothermal effect on stability (e.g., Figure 14 (As shown).

[0066] In summary, the synthesis process of this invention is simple, highly controllable, and uses abundant and readily available raw materials. The novel polycrystalline structure of the prepared multiphase SnSe / NiSe / Ni3Se2 hybrid nanorod array material creates more high-energy active sites and synergistic catalytic centers, thus exhibiting excellent performance in electrocatalytic HER, UOR, and UOR-assisted water electrolysis for hydrogen production. In particular, the photothermal effect introduced by NIR light significantly improves the kinetics and thermodynamics of the UOR catalytic reaction, providing important support for the efficient operation of the catalytic reaction and demonstrating broad commercial application potential.

[0067] The above description is merely a preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto. Any simple changes or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the scope of the technology disclosed in the present invention shall fall within the scope of protection of the present invention.

Claims

1. A method for preparing a polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material, characterized in that, Includes the following steps: (1) Under a continuous N2 atmosphere, 1~6 mmol NaBH4 was completely dissolved in 1~6 mL of deionized water, and then 1~4 mmol Se powder was added until it was reduced to a clear and transparent solution; (2) Add, sequentially to the clear and transparent solution from step (1), a mixed solution of 0.05 mmol / L SnCl2·2H2O and 0.5~1.5 mmol / L NaOH, 1~2 mmol / L NH4F solution, and a solution with an area ranging from 1 × 2 to 2 × 4 cm². 2 Nickel foam was then subjected to a hydrothermal reaction at a temperature of 120~200 ℃ for 4~12 h, ultimately yielding polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorods grown in situ vertically on a nickel foam framework. The volume of the SnCl2·2H2O and NaOH mixed solution was 1 mL, and the volume of the NH4F solution was 25 mL.

2. The polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material prepared by any one of the preparation methods in claim 1, is composed of orthorhombic SnSe, hexagonal NiSe, and rhombohedral Ni3Se2, wherein, The diameter of the SnSe / NiSe / Ni3Se2 hybrid nanorods is 100~300 nm.

3. The application of the polycrystalline SnSe / NiSe / Ni3Se2 hybrid nanorod array material as described in claim 2 as an electrocatalyst in urea oxidation, water electrolysis for hydrogen evolution, and water electrolysis for hydrogen production assisted by urea oxidation.

4. The application according to claim 3, characterized in that, In the urea oxidation-assisted water electrolysis for hydrogen production, a SnSe / NiSe / Ni3Se2||SnSe / NiSe / Ni3Se2 electrolyzer is used, and a 10 mA cm⁻¹ drive is achieved at voltages of 1.37 V and 1.54 V. -2 and 100 mA cm -2 .

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