Novel nickel phosphate electrolytic water hydrogen evolution catalyst and preparation method thereof
The preparation of porous nickel phosphate electrode materials by electrochemical deposition and low-temperature phosphation on titanium sheets has solved the problems of high cost and poor durability of precious metal catalysts, and achieved low overpotential and high stability electrocatalytic performance, which is suitable for hydrolyzing hydrogen evolution reactions .
Patent Information
- Application Number
- CN202411314999.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2024-12-13
AI Technical Summary
The existing precious metal catalysts have high cost and poor durability in electrolytic hydrogen evolution reactions, and the stability and hydrogen evolution performance of nickel phosphate electrocatalysts need to be further improved to suit industrial applications.
Porous amorphous nickel phosphate (p-NiPO) electrode material was prepared by electrochemically depositing porous nickel hydroxide (p-Ni(OH)2) on a titanium sheet and phosphating at low temperature to form a unique nanosheet/nanogroup Cluster crosslinking structure improves electrocatalytic stability and hydrogen evolution performance.
The optimized p-NiPO catalyst exhibits low overpotential and high stability in alkaline water, and significantly improves charge transfer and catalytic performance, making it suitable for industrial applications.
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Figure CN119121290A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of catalysts, and in particular to a novel nickel phosphate water electrolysis hydrogen evolution catalyst and a preparation method thereof. Background Art
[0002] Hydrogen energy is regarded as an important direction for future energy development due to its advantages of high energy density, cleanness, pollution-free, easy storage and transportation. As an efficient and environmentally friendly energy conversion method, the electrocatalytic hydrogen production process can convert electricity generated from renewable energy sources (such as solar energy, wind energy, etc.) into hydrogen energy, providing important support for sustainable energy systems. In industrial applications, the catalysts commonly used for water electrolysis are catalysts based on precious metals (such as platinum), which usually exhibit extremely low overpotentials and high exchange current densities. However, high cost, low crustal reserves and poor durability still limit its further application in hydrogen evolution reaction (HER).
[0003] Transition metal materials have a unique d-orbital electronic structure, which can provide empty orbitals and lone pairs of electrons in chemical reactions, thereby reducing the activation energy of the reaction. Transition metal ions interact with ligands through coordination bonds, which regulate the electronic state and charge distribution of transition metals, determine the structure and properties of active sites, and increase the reaction rate. In addition, transition metal catalysts can participate in the reaction process through redox reactions, acid-base reactions, and the formation and breaking of coordination bonds, showing a variety of catalytic reaction mechanisms and significant performance. Currently, popular transition metal electrocatalysts include transition metal hydroxides / oxides, nitrides, sulfides, phosphides and MXenes materials.
[0004] Among these transition metal catalysts, transition metal phosphides (TMPs) exhibit excellent conductivity, electrochemical activity, stability and enhanced electrochemical performance, and have broader application prospects in the field of electrocatalysis. In particular, nickel phosphate materials with a three-dimensional network structure, whose unique Ni-OP and POP bonds provide abundant active sites and provide efficient pathways for electron transport and catalytic reactions. However, before industrial application, the electrocatalytic stability and hydrogen evolution performance of nickel phosphate still need to be further improved. Summary of the invention
[0005] The object of the present invention is to provide a novel nickel phosphate water electrolysis hydrogen evolution catalyst and a preparation method thereof, so as to solve the problems raised in the above background technology.
[0006] In order to solve the above technical problems, the present invention provides the following technical solutions: a method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst, which adopts two strategies to improve the electrocatalytic stability and hydrogen evolution performance of nickel phosphate.
[0007] Including S1-1, preparation of porous (p)-Ni(OH)2 / Ti:
[0008] S1-2, preparation of smooth (s)-Ni(OH)2 / Ti;
[0009] S2. Preparation of p / s-NiPO / Ti.
[0010] According to the above technical scheme, in S1-S2, a titanium sheet is used as a substrate, and a layer of porous nickel hydroxide (p-Ni(OH)2) nanomaterial is deposited on the surface of the titanium sheet by electrochemical deposition, and then the p-Ni(OH)2 is converted into a porous amorphous nickel phosphate (p-NiPO) electrode material by a simple low-temperature phosphating process.
[0011] According to the above technical solution, S1 is specifically:
[0012] First, the titanium sheet (Ti) was cut into a specified size and ultrasonically cleaned with 2M hydrochloric acid solution, acetone and anhydrous ethanol for 15 minutes in sequence to remove organic matter and oxide layer that may remain on the surface of the titanium sheet during processing. It was then rinsed with deionized water. Then, a three-electrode system was used, with the titanium sheet as the working electrode, the graphite electrode as the counter electrode, and the Ag / AgCl (3M KCl) electrode as the reference electrode. In an electrolyte of 0.1M NiCl2·6H2O, the solution temperature was controlled at 30°C. The electrodeposition experiment was carried out using the chronoamperometry (It) on a CHI 760E electrochemical workstation. The deposition potential was -1.0V and the deposition charge was -0.25C. After the deposition was completed, the surface of the titanium sheet was repeatedly rinsed with deionized water and dried to obtain a rough Ni(OH)2 / Ti nanoelectrode material, which was recorded as p-Ni(OH)2 / Ti.
[0013] According to the above technical solution, in S1-1, the specified size of the titanium sheet (Ti) is: 0.5×0.5cm 2 .
[0014] According to the above technical solution, S1-2 includes the preparation of Ni nano-electrode material, specifically:
[0015] Using the same preparation method as above, in an electrolyte composed of 0.1M NiCl2·6H2O and 0.1M H3BO3, the solution temperature was controlled at 30°C, and the electrodeposition experiment was carried out using chronoamperometry (It) on a CHI 760E electrochemical workstation. The deposition potential was -1.0V and the deposition charge was -0.25C to obtain a smooth Ni nanoelectrode material.
[0016] According to the above technical scheme, in S2, the obtained Ni nanomaterial is used as the working electrode, the graphite electrode is used as the counter electrode, and the Hg / HgO (1M KOH) electrode is used as the reference electrode. Cyclic voltammetry is used to oxidize for 2 hours in a 1M KOH solution at a voltage range of 0 to 1.0V, and then the surface of the titanium sheet is repeatedly rinsed with deionized water. After drying, a smooth Ni(OH)2 / Ti nanoelectrode material is obtained, which is recorded as s-Ni(OH)2 / Ti.
[0017] According to the above technical solution, S2 is specifically:
[0018] The prepared p / s-Ni(OH)2 / Ti precursor and 0.012g NaH2PO2 were placed in two porcelain boats respectively. The porcelain boat containing p / s-Ni(OH)2 / Ti was placed in the center of the tube furnace, and the porcelain boat containing NaH2PO2 was placed upstream of the p / s-Ni(OH)2 / Ti. Under argon protective atmosphere, the temperature was increased to 300°C at a heating rate of 5°C / min and kept warm for 10 minutes. After naturally cooling to room temperature, the prepared sample was taken out and repeatedly rinsed with anhydrous ethanol and deionized water to obtain p / s-NiPO / Ti electrode material.
[0019] According to the above technical solution, in S2, the p-Ni(OH)2 / Ti and s-Ni(OH)2 / Ti precursors are phosphated to obtain nanomaterials which are respectively recorded as p-NiPO / Ti and s-NiPO / Ti.
[0020] Compared with the prior art, the beneficial effects achieved by the present invention are: the p-NiPO / Ti electrocatalyst prepared by the method has a unique nanosheet / nanocluster cross-linked structure. The optimized p-NiPO / Ti electrocatalyst exhibits excellent charge transfer performance and catalytic performance in the alkaline water splitting process. The electrocatalytic results show that the optimized p-NiPO / Ti has a lower HER overpotential (at 10 mA cm -2 128mV at 100mA·cm -2 242mV at 10mAcm -2 The stability was good within 24 hours. In addition, the titanium sheet as a substrate for the controllable growth of catalytic materials helps to enhance the electrode compatibility in industrial applications. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:
[0022] Figure 1 is a SEM image of the material of the present invention;
[0023] Figure 2 In the figure, it is the characteristic diagram of p-NiPO;
[0024] Figure 3 is the XRD spectra of p-Ni(OH)2 / Ti and p-NiPO / Ti of the present invention;
[0025] Figure 4 is the XPS spectrum of p-NiPO / Ti of the present invention;
[0026] Figure 5 It is a hydrogen evolution performance diagram of s-Ni(OH)2 / Ti, p-Ni(OH)2 / Ti, s-NiPO / Ti, and p-NiPO / Ti of the present invention;
[0027] Figure 6 It is a schematic diagram of the process of the present invention. DETAILED DESCRIPTION
[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0029] See also Figure 1-6 The present invention provides a technical solution: a novel nickel phosphate water electrolysis hydrogen evolution catalyst and a preparation method thereof, which adopts two strategies to improve the electrocatalytic stability and hydrogen evolution performance of nickel phosphate: (1) using a titanium sheet known for its excellent conductivity, high stability and corrosion resistance as a substrate; (2) depositing a layer of porous nickel hydroxide (p-Ni(OH)2) nanomaterial on the surface of the titanium sheet by electrochemical deposition, and then converting the p-Ni(OH)2 into a porous amorphous nickel phosphate (p-NiPO) electrode material by a simple low-temperature phosphating process.
[0030] in Figure 1 SEM images of materials: (a) p-Ni(OH)2 / Ti, (b) s-Ni(OH)2 / Ti, (c) p-NiPO / Ti, (d) s-NiPO / Ti;
[0031] Figure 2 (a) TEM image, (b) HRTEM image, (c) EDS elemental mapping image and (d) SAED diffraction pattern of p-NiPO;
[0032] Figure 4 XPS spectra of p-NiPO / Ti: (a) overall spectrum; (b)-(d) Ni 2p, P 2p, O 1s spectra;
[0033] Figure 5 Hydrogen evolution performance of s-Ni(OH)2 / Ti, p-Ni(OH)2 / Ti, s-NiPO / Ti, and p-NiPO / Ti: (a) LSV polarization curves; (b) 10 mA·cm -2 and 100mA·cm -2 (c) Tafel slope; (d) electrochemical impedance spectroscopy; (e) stability test; (f) LSV curves before and after the stability test;
[0034] Including S1-1, preparation of porous (p)-Ni(OH)2 / Ti:
[0035] S1-2, preparation of smooth (s)-Ni(OH)2 / Ti;
[0036] Preparation of S2, p / s-NiPO / Ti;
[0037] In S1-S2, a layer of porous nickel hydroxide (p-Ni(OH)2) nanomaterial is deposited on the surface of the titanium sheet by electrochemical deposition using a titanium sheet as a substrate, and then the p-Ni(OH)2 is converted into a porous amorphous nickel phosphate (p-NiPO) electrode material by a simple low-temperature phosphating process;
[0038] S1 is specifically:
[0039] First, the titanium sheet (Ti) was cut into a specified size, and ultrasonically cleaned with 2M hydrochloric acid solution, acetone and anhydrous ethanol for 15 minutes in sequence to remove organic matter and oxide layer that may remain on the surface of the titanium sheet during processing, and then rinsed with deionized water. Then, a three-electrode system was used, with the titanium sheet as the working electrode, the graphite electrode as the counter electrode, and the Ag / AgCl (3M KCl) electrode as the reference electrode. In an electrolyte of 0.1M NiCl2·6H2O, the solution temperature was controlled at 30°C. The electrodeposition experiment was carried out using the chronoamperometry (It) on a CHI 760E electrochemical workstation. The deposition potential was -1.0V and the deposition charge was -0.25C. After the deposition was completed, the surface of the titanium sheet was repeatedly rinsed with deionized water and dried to obtain a rough Ni(OH)2 / Ti nanoelectrode material, which was recorded as p-Ni(OH)2 / Ti.
[0040] In S1-1, the specified size of the titanium sheet (Ti) is: 0.5×0.5cm 2 ;
[0041] S1-2 includes the preparation of Ni nano-electrode materials, specifically:
[0042] The same preparation method as above was used to obtain a smooth Ni nanoelectrode material in an electrolyte consisting of 0.1M NiCl2·6H2O and 0.1M H3BO3, with the solution temperature controlled at 30°C, and the electrodeposition experiment was carried out on a CHI 760E electrochemical workstation using chronoamperometry (It), with a deposition potential of -1.0V and a deposition charge of -0.25C.
[0043] In S1-2, the obtained Ni nanomaterial was used as the working electrode, the graphite electrode was used as the counter electrode, and the Hg / HgO (1M KOH) electrode was used as the reference electrode. The cyclic voltammetry method was used to oxidize the titanium sheet in a 1M KOH solution at a voltage range of 0 to 1.0 V for 2 h, and then the surface of the titanium sheet was repeatedly rinsed with deionized water. After drying, a smooth Ni(OH)2 / Ti nanoelectrode material was obtained, which was recorded as s-Ni(OH)2 / Ti.
[0044] S2 is specifically:
[0045] The prepared p / s-Ni(OH)2 / Ti precursor and 0.012g NaH2PO2 were placed in two porcelain boats respectively, the porcelain boat containing p / s-Ni(OH)2 / Ti was placed in the center of the tube furnace, and the porcelain boat containing NaH2PO2 was placed upstream of the p / s-Ni(OH)2 / Ti. Under an argon protective atmosphere, the temperature was increased to 300°C at a heating rate of 5°C / min and kept warm for 10 minutes. After naturally cooling to room temperature, the prepared sample was taken out and repeatedly rinsed with anhydrous ethanol and deionized water to obtain a p / s-NiPO / Ti electrode material.
[0046] In S2, the p-Ni(OH)2 / Ti and s-Ni(OH)2 / Ti precursors are phosphated to obtain nanomaterials, which are denoted as p-NiPO / Ti and s-NiPO / Ti, respectively.
[0047] This patent synthesized p-NiPO / Ti electrocatalyst by electrochemically depositing p-Ni(OH)2 nanostructures on titanium plates, followed by short-time high-temperature phosphating. The p-NiPO / Ti electrocatalyst prepared by this method has a unique nanosheet / nanocluster cross-linked structure. The optimized p-NiPO / Ti electrocatalyst exhibits excellent charge transfer and catalytic performance in alkaline water splitting. The electrocatalytic results show that the optimized p-NiPO / Ti has a lower HER overpotential (at 10mA·cm -2 128mV at 100mA·cm -2 242mV at 10mA·cm -2 The stability was good within 24 hours. In addition, the titanium sheet, which serves as a substrate for the controllable growth of catalytic materials, helps to enhance the electrode compatibility in industrial applications.
[0048] Embodiment 1:
[0049] SEM analysis
[0050] In order to study the morphology of the samples, SEM tests were carried out on Ni(OH)2 / Ti and NiPO / Ti. Figure 1 (a) and (b) are SEM images of p-Ni(OH)2 / Ti and s-Ni(OH)2 / Ti precursors. It can be seen from the figures that Ni(OH)2 grows uniformly on the surface of the titanium sheet, among which p-Ni(OH)2 / Ti is composed of nanoclusters of different sizes piled together with many cracks to form a rough surface; the surface of s-Ni(OH)2 / Ti is tightly stacked to form a dense film with significantly reduced roughness. Figure 1 (c) and (d) are SEM images of p-NiPO / Ti and s-NiPO / Ti. As can be seen from Figure (c), after low-temperature phosphating, the nanocluster stacking structure has basically not changed. Nanosheets with a thickness of 30-50nm grow in the stacking cracks. The nanosheets are vertically arranged in the cracks. The huge difference between the Ni(OH)2 / Ti precursor and NiPO / Ti indicates that Ni(OH)2 has been successfully phosphated; Figure (d) shows that s-NiPO / Ti is composed of a dense nanofilm and tiny nano-protrusions on the surface. The unique nanosheet / nanocluster cross-linked structure gives the catalytic electrode a rich surface area, expands the contact area between the catalyst and the electrolyte, and exposes the active sites to the maximum extent, accelerating the diffusion of electrolyte / ions and the release of gas, thereby improving the electrocatalytic activity.
[0051] TEM analysis
[0052] In order to further explore the microstructure of the prepared catalyst, p-NiPO was peeled off from the titanium sheet and subjected to transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) tests. Figure 2 As can be seen from (a) and (b), p-NiPO is dispersed in ethanol to form a typical flake structure. The HRTEM image shows that the p-NiPO sample has a loose structure and a large number of microporous structures. These nanopores increase the specific surface area of the catalyst, which is conducive to the contact between the catalyst and the electrolyte and the exposure of more active sites. Figure 2 From the element distribution diagram (c), it can be found that Ni, O, and P elements are evenly distributed in the sample. Figure 2 There are no obvious electron diffraction rings in the electron area diffraction pattern (d), indicating that the generated NiPO has an amorphous structure, which is consistent with the results of XRD and XPS.
[0053] X-ray diffraction (XRD)
[0054] Figure 3The results of X-ray diffraction (XRD) analysis of the crystal structure of p-Ni(OH)2 / Ti and p-NiPO / Ti samples show that neither shows obvious p-Ni(OH)2 and p-NiPO diffraction peaks, which preliminarily proves that the p-Ni(OH)2 and p-NiPO synthesized by this method are amorphous structures.
[0055] XPS analysis
[0056] In order to further clarify the chemical composition and valence state of the main elements of p-NiPO / Ti, X-ray photoelectron spectroscopy (XPS) analysis was performed. Figure 4 is the XPS spectrum of rough NiPO. Figure 4 The total spectrum shown in a confirms the presence of three elements: Ni, P, and O. In the high-resolution XPS spectrum of Ni 2p ( Figure 4 In b), NiPO has two orbital peaks at 856.5 eV and 874.1 eV, which are attributed to Ni 2p 3 / 2 and Ni 2p 1 / 2 The spin-orbit splitting of the divalent nickel ion (Ni 2+ ), the peaks at 861.8eV and 879.7eV are the corresponding two satellite peaks. High-resolution XPS spectrum of P 2p ( Figure 4 In c), only one signal at 133.3 eV can be observed, which is attributed to the PO bond in the phosphate group. Figure 4 d) Two peaks can be fitted, and the peaks at 531.5eV and 533.0eV are attributed to the PO-Ni bond and the PO bond, respectively. Based on the above analysis, it can be confirmed that we have successfully synthesized the NiPO catalyst.
[0057] Analysis of electrocatalytic hydrogen evolution performance
[0058] In order to study the electrochemical hydrogen evolution performance of the material, the p-NiPO / Ti catalyst was electrochemically tested for HER using a three-electrode system in a 1.0 M KOH aqueous solution, with s-Ni(OH)2 / Ti, p-Ni(OH)2 / Ti and s-NiPO / Ti catalysts as controls. Figure 5 a shows the iR corrected polarization curves of these electrocatalysts. It can be seen from the figure that p-NiPO / Ti has a good conductivity at a current density of 10 mA cm -2 (η10) and 100 mA cm -2 (η 100) were 128 mV and 242 mV, respectively, which were significantly lower than s-Ni(OH)2 / Ti (368 mV and 484 mV), p-Ni(OH)2 / Ti (240 mV and 315 mV), and s-NiPO / Ti (236 mV and 356 mV), showing good HER catalytic performance. Figure 5 b is the catalyst at 10 mA·cm -2 and 100mA·cm -2 In order to better understand the kinetics of the HER reaction, the Tafel slope is calculated based on the polarization curve, as shown in Figure 5 c. The Tafel slope of p-NiPO / Ti is 79.2 mV·dec -1 , much lower than s-Ni(OH)2 / Ti(138.3mV·dec -1 )、p-Ni(OH)2 / Ti(109.7mV·dec -1 ), and s-NiPO / Ti (116.7mV·dec -1 ) is the Tafel slope of .
[0059] Electrochemical impedance spectroscopy (EIS) provides a method to measure the interfacial charge transfer resistance (Rct) between the catalyst and the electrolyte and the internal resistance (Rs) of the electrode material. The catalyst is tested with a test potential of -0.2V (vs. RHE), a frequency range of 0.1Hz to 105Hz, and an amplitude of 5mV to study the charge transfer dynamics of the material. The smaller the semicircle diameter of the EIS curve, the smaller the charge transfer resistance and the higher the charge transfer efficiency. The test results are as follows: Figure 5 As shown in Figure d, the charge transfer resistance (Rct) of p-NiPO / Ti is 5.26Ω, which is smaller than s-Ni(OH)2 / Ti (88.04Ω), p-Ni(OH)2 / Ti (17.33Ω), and s-NiPO / Ti (36.02Ω), indicating that the conductivity between the p-NiPO / Ti catalyst and the electrolyte is higher and the charge transfer rate is faster during the HER process. This is consistent with the low overpotential and excellent Tafel slope results shown by p-NiPO / Ti. In addition, the long-term stability of the catalyst is also one of the important indicators for evaluating the application development potential of the catalyst. Figure 5 e shows the current density of p-NiPO / Ti in 1 M KOH solution at 10 mA cm -2 The time potential curve shows that after 24 hours of stability test, the overpotential only increased by 7.6% compared with the initial value. Figure 5 f is the LSV curve before and after the stability test, and the change is basically negligible, indicating that p-NiPO / Ti has excellent stability under alkaline conditions.
[0060] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.
[0061] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. A method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst, characterized in that: include S1-1. Preparation of porous (p)-Ni(OH)2 / Ti: S1-2, preparation of smooth (s)-Ni(OH)2 / Ti; S3. Preparation of p / s-NiPO / Ti.
2. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 1, characterized in that: In S1-S2, a titanium sheet is used as a substrate, and a layer of porous nickel hydroxide (p-Ni(OH)2) nanomaterial is deposited on the surface of the titanium sheet by electrochemical deposition, and then the p-Ni(OH)2 is converted into a porous amorphous nickel phosphate (p-NiPO) electrode material by a simple low-temperature phosphating process.
3. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 2, characterized in that: The S1 is specifically: First, the titanium sheet (Ti) was cut into a specified size and ultrasonically cleaned with 2M hydrochloric acid solution, acetone and anhydrous ethanol for 15 minutes in sequence to remove organic matter and oxide layer that may remain on the surface of the titanium sheet during processing. It was then rinsed with deionized water. Then, a three-electrode system was used, with the titanium sheet as the working electrode, the graphite electrode as the counter electrode, and the Ag / AgCl (3M KCl) electrode as the reference electrode. In an electrolyte of 0.1M NiCl2·6H2O, the solution temperature was controlled at 30°C. The electrodeposition experiment was carried out using the chronoamperometry (It) on a CHI 760E electrochemical workstation. The deposition potential was -1.0V and the deposition charge was -0.25C. After the deposition was completed, the surface of the titanium sheet was repeatedly rinsed with deionized water and dried to obtain a rough Ni(OH)2 / Ti nanoelectrode material, which was recorded as p-Ni(OH)2 / Ti.
4. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 3, characterized in that: In S1-1, the specified size of the titanium sheet (Ti) is: 0.5×0.5 cm 2 .
5. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 4, characterized in that: The S1-2 includes the preparation of Ni nano-electrode materials, specifically: Using the same preparation method as above, in an electrolyte composed of 0.1M NiCl2·6H2O and 0.1M H3BO3, the solution temperature was controlled at 30°C, and the electrodeposition experiment was carried out using chronoamperometry (It) on a CHI 760E electrochemical workstation. The deposition potential was -1.0V and the deposition charge was -0.25C to obtain a smooth Ni nanoelectrode material.
6. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 5, characterized in that: In S1-2, the obtained Ni nanomaterial is used as the working electrode, the graphite electrode is used as the counter electrode, and the Hg / HgO (1M KOH) electrode is used as the reference electrode. The cyclic voltammetry method is used to oxidize the titanium sheet in a 1M KOH solution at a voltage range of 0 to 1.0 V for 2 hours, and then the surface of the titanium sheet is repeatedly rinsed with deionized water. After drying, a smooth Ni(OH)2 / Ti nanoelectrode material is obtained, which is recorded as s-Ni(OH)2 / Ti.
7. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 6, characterized in that: The S3 is specifically: The prepared p / s-Ni(OH)2 / Ti precursor and 0.012g NaH2PO2 were placed in two porcelain boats respectively. The porcelain boat containing p / s-Ni(OH)2 / Ti was placed in the center of the tube furnace, and the porcelain boat containing NaH2PO2 was placed upstream of the p / s-Ni(OH)2 / Ti. Under argon protective atmosphere, the temperature was increased to 300°C at a heating rate of 5°C / min and kept warm for 10 minutes. After naturally cooling to room temperature, the prepared sample was taken out and repeatedly rinsed with anhydrous ethanol and deionized water to obtain p / s-NiPO / Ti electrode material.
8. The method for preparing a novel nickel phosphate water electrolysis hydrogen evolution catalyst according to claim 7, characterized in that: In S2, the p-Ni(OH)2 / Ti and s-Ni(OH)2 / Ti precursors are phosphated to obtain nanomaterials, which are respectively recorded as p-NiPO / Ti and s-NiPO / Ti.
