Morphology-controllable molybdenum sulfide hydrogen evolution electrode and preparation method thereof

Abstract

The application relates to the technical field of hydrogen evolution electrode materials, in particular to a morphology-controllable molybdenum sulfide hydrogen evolution electrode and a preparation method thereof, which comprises the following steps: selecting a base material from which surface grease and rust are removed, fixing the base material, and then placing the base material into a vacuum chamber of a magnetron sputtering coating system; starting a unipolar HALL source, and performing plasma cleaning; starting the magnetron sputtering coating system to deposit a molybdenum sulfide coating on the cleaned base material, wherein, during the deposition process, the reaction vacuum degree of the vacuum chamber cabin of the magnetron sputtering coating system is 0.5-2 Pa, the film forming temperature is 80-200 DEG C, the unipolar pulse magnetron sputtering power is 1-5 kW, and the deposition time is 5-180 min. The catalytic electrode prepared based on the temperature regulation method has a significantly enhanced hydrogen evolution catalytic activity, exhibits a lower overpotential and good running stability. The method realizes vertical orientation of the coating with high consistency, high purity and firm bonding strength between the coating and the base material, and provides an effective solution for manufacturing of high-performance hydrogen evolution electrodes.

Description

Technical Field

[0001] This invention relates to the field of hydrogen evolution electrode materials technology, and in particular to a molybdenum sulfide hydrogen evolution electrode with controllable morphology and its preparation method. Background Technology

[0002] Catalysts play a crucial role in numerous industrial processes. In hydrogen production, whether it's natural gas reforming, methanol conversion, or water electrolysis, the economics and efficiency heavily rely on the application of high-performance catalysts. Although precious metal catalysts such as platinum exhibit excellent activity, their high cost severely limits large-scale industrial application. Therefore, developing efficient and stable non-precious metal alternatives has become a key research direction for promoting a clean hydrogen economy.

[0003] Among numerous candidate materials, molybdenum sulfide (MoS2) is considered a highly promising electrocatalyst for the hydrogen evolution reaction (HER) due to its abundant reserves, low cost, and the fact that its hydrogen adsorption Gibbs free energy at edge sites is close to that of platinum. Currently, the preparation of molybdenum sulfide catalysts mainly relies on chemical synthesis methods such as hydrothermal methods and chemical vapor deposition. While these methods can control the morphology of materials at the laboratory scale, they generally suffer from complex processes, poor reproducibility, and difficulty in precisely controlling coating thickness and uniformity, severely restricting their industrial-scale mass production and application. In contrast, magnetron sputtering, as a physical vapor deposition technique, has significant advantages such as good film uniformity, precise control of coating composition and thickness, strong adhesion, and ease of large-area continuous production, making it more suitable for the requirements of industrial manufacturing for consistency, reliability, and cost control.

[0004] However, applying magnetron sputtering technology to prepare molybdenum sulfide hydrogen evolution catalytic coatings still faces significant challenges. Catalytic performance depends not only on the intrinsic activity of the material but also on its microstructure. Studies have shown that the catalytically active sites of molybdenum sulfide are mainly concentrated at the edges of its two-dimensional lamellar structures. However, coatings obtained under conventional magnetron sputtering process parameters typically exhibit a layered stacked structure with the basal plane parallel to the substrate. This results in a large number of active edges being buried, limiting the exposure and utilization efficiency of active sites. Furthermore, existing conventional magnetron sputtering processes, when preparing molybdenum sulfide coatings, usually preferentially obtain a more thermodynamically stable layered stacked structure with the basal plane parallel to the substrate. This horizontal growth mode leads to the burial of most active edges, severely limiting the effective utilization of active sites and failing to fully leverage the intrinsic material advantages of molybdenum sulfide. While adjusting parameters such as power and gas pressure can influence coating morphology to some extent, there is still a lack of clear and effective solutions in existing technologies for actively and stably achieving a paradigm shift from horizontal to vertical growth of molybdenum sulfide coatings through a systematic and controllable combination of process parameters—especially the precise control of the key kinetic factor of substrate temperature—and for elucidating the influence of parameters such as temperature on growth orientation and final surface morphology. This results in inherent bottlenecks in the active site exposure density and catalytic efficiency of molybdenum sulfide catalytic electrodes prepared by existing magnetron sputtering processes, failing to meet the dual requirements of high performance, low cost, and large-scale manufacturing.

[0005] Furthermore, on the one hand, there are differences in understanding among those skilled in the art; on the other hand, the inventors studied a large number of documents and patents when making this invention, but due to space limitations, not all details and contents were listed in detail. However, this does not mean that the present invention does not possess the features of these prior art. On the contrary, the present invention already possesses all the features of the prior art, and the applicant reserves the right to add relevant prior art to the background art. Summary of the Invention

[0006] This invention relates to the field of hydrogen evolution electrode materials technology, and in particular to a molybdenum sulfide hydrogen evolution electrode with controllable morphology and its preparation method.

[0007] To address the aforementioned technical problems, one objective of this invention is to provide a method for preparing a molybdenum sulfide hydrogen evolution electrode with controllable morphology, comprising the following steps: Select a substrate with surface grease and rust removed, fix the substrate and place it in the vacuum chamber of the magnetron sputtering coating system, start the unipolar HALL source and perform plasma cleaning; The magnetron sputtering coating system is started to deposit a molybdenum sulfide coating on the cleaned substrate. During the deposition process, the vacuum degree of the vacuum chamber of the magnetron sputtering coating system is 0.5~2 Pa, the film formation temperature is 80-200℃, the unipolar pulse magnetron sputtering power is 1~5 kW, and the deposition time is 5~180 min.

[0008] According to a preferred embodiment, the film-forming temperature is 150°C.

[0009] According to a preferred embodiment, during the deposition process, the vacuum chamber of the magnetron sputtering coating system has a reaction vacuum of 1.0 Pa, a pulsed magnetron power of 2 kW, a film formation temperature of 80°C, and a deposition time of 30 min.

[0010] According to a preferred embodiment, the mechanical pump, Roots pump, and molecular pump of the magnetron sputtering coating system are sequentially started to evacuate the vacuum chamber. After the chamber vacuum reaches the background vacuum level, high-purity argon gas with a purity of 99.99% is introduced to adjust the reaction vacuum level in the chamber.

[0011] According to a preferred embodiment, during plasma cleaning, the background vacuum level of the vacuum chamber in the magnetron sputtering coating system is 5 × 10⁻⁶. -4 ~5×10 -3 The chamber reaction vacuum is 0.1~2 Pa, the plasma cleaning power is 600~2000 W, and the cleaning time is 10~20 min. Preferably, the chamber background vacuum is set to 5×10 Pa. -4 Argon gas was introduced to create a reaction vacuum of 1 Pa in the chamber. The HALL plasma cleaning power was set to 800 W, and the plasma cleaning time was set to 20 min.

[0012] According to a preferred embodiment, the substrate is nickel foam or nickel mesh. The substrate size is 500. 500 mm. Substrate thickness 0.3 mm. Substrate porosity 88.8%.

[0013] According to a preferred embodiment, the substrate is ultrasonically cleaned before use, using a 10-20% (w / w) concentration of CY-1003A cleaning agent. Preferably, the cleaning agent temperature is maintained at 50-70°C. The ultrasonic vibration frequency is 28 kHz. Cleaning continues until the substrate surface is free of surface grease and rust. More preferably, the cleaning time is 5-10 minutes.

[0014] According to a preferred embodiment, after cleaning with the cleaning agent, the substrate is rinsed with deionized water until the cleaning agent is completely removed. Then, the substrate is ultrasonically cleaned with anhydrous ethanol to remove surface moisture for 5-10 minutes. Finally, the substrate is cleaned again with anhydrous ethanol to further maintain surface cleanliness for another 5-10 minutes. After cleaning, the substrate is removed and dried with nitrogen for later use. Preferably, a 20% (w / w) concentration of 1003A cleaning agent is prepared, heated to 60°C in the ultrasonic bath, and an ultrasonic vibration frequency of 28 kHz is selected for 10 minutes. The ultrasonic cleaning time with anhydrous ethanol is 5 minutes in all cases.

[0015] It should be noted that nickel foam, nickel mesh, and other mesh substrates used as coating materials require a cleaning process before coating to remove grease and rust from the material surface, ensuring a firm coating adhesion.

[0016] According to a preferred embodiment, the substrate is fixed by using a clamp to install and fix the substrate. After fixing, the workpiece is placed in the vacuum chamber of the magnetron sputtering coating system and adjusted to a suitable position. After confirming that all components of the coating system are functioning normally, the vacuum chamber door is closed.

[0017] To address the aforementioned technical problems, one objective of this invention is to provide a hydrogen evolution electrode comprising a substrate and a molybdenum sulfide catalytic coating grown vertically on the substrate, wherein the molybdenum sulfide catalytic coating is deposited on the substrate using the aforementioned method for controlling the morphology of the molybdenum sulfide coating of the hydrogen evolution electrode.

[0018] One of the objectives of this invention is to provide the use of the above-mentioned molybdenum sulfide hydrogen evolution electrode in hydrogen production.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention breaks through the limitation that molybdenum sulfide coatings mainly grow in horizontal layers under conventional process parameters. Through a specific combination of process parameters, it achieves for the first time the regulation of the directional growth of molybdenum sulfide catalyst layer perpendicular to the substrate.

[0020] First, this invention achieves a fundamental shift in the growth of molybdenum sulfide catalyst layers from conventional horizontal layered growth to directional growth perpendicular to the substrate through magnetron sputtering physical vapor deposition, particularly by precisely controlling the substrate temperature. By precisely setting the temperature, thermal activation is achieved, altering the surface migration behavior of the growth units.

[0021] It should be noted that this unique vertical growth structure enhances the catalytic effect of the coating. When used as a hydrogen evolution electrode, the coating exposes an order-of-magnitude increase in catalytically active edge sites and forms open three-dimensional porous channels. This significantly increases the contact area between the electrode and the electrolyte, greatly promoting reaction mass transfer and the rapid release of hydrogen bubbles. Simultaneously, this structure optimizes the electron conduction path, enhancing the adhesion between the coating and the substrate, as well as its structural stability.

[0022] The catalytic electrode prepared based on this temperature control method exhibits significantly enhanced hydrogen evolution catalytic activity, demonstrating lower overpotential and better operational stability. Furthermore, this method combines controllable microstructure design with industrially compatible physical vapor deposition (PVD) processes, achieving highly consistent vertical orientation, high purity, and strong adhesion between the coating and the substrate. This provides an effective solution for the large-scale, controllable fabrication of high-performance, low-cost hydrogen evolution electrodes. Attached Figure Description

[0023] Figure 1 The image shows a scanning electron microscope (SEM) image of the coating surface prepared according to Example 1 of the method described in this invention (film formation temperature 150°C), where ac represents the surface morphology of the molybdenum sulfide catalyst layer at different magnifications, namely 1 k, 10 k, and 100 k times. Figure 2 The image shows a scanning electron microscope (SEM) image of the coating surface prepared according to Example 3 of the method described in this invention (film formation temperature 200℃), where ac represents the surface morphology of the molybdenum sulfide catalyst layer at different magnifications, namely 1 k, 10 k, and 100 k times. Figure 3 The image shown is a scanning electron microscope (SEM) image of the coating surface prepared in Comparative Example 1 (film formation temperature room temperature) according to the method described in this invention. Here, ac represents the surface morphology of the molybdenum sulfide catalyst layer at different magnifications, namely 1 k, 10 k, and 100 k times. Figure 4 X-ray diffraction (XRD) patterns of molybdenum sulfide coatings prepared in Examples 1, 3 and Comparative Example 1 of the present invention; Figure 5 The linear sweep voltammetric curves obtained by using an electrochemical workstation to perform electrochemical hydrogen evolution tests on the hydrogen evolution electrodes prepared in Examples 1-3 and Comparative Example 1 are shown below. Figure 5 A is a linear sweep voltammetry curve. Figure 5 B is a graph showing the relationship between film formation temperature and overpotential; Figure 6Raman spectra of molybdenum sulfide coatings prepared at room temperature (Comparative Example 1), 150°C (Example 1), and 200°C (Example 3). Detailed Implementation

[0024] In the description of this invention, terminology is used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly defined.

[0025] Unless otherwise specified, the experimental methods used in the following examples are all conventional methods; the materials, reagents or instruments used, unless otherwise specified by the manufacturer, are all commercially available reagents and materials; the conditions not specified in the examples are all carried out according to conventional conditions or conditions recommended by the manufacturer. At the same time, the present invention does not limit the source of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are all commercially available products in this technical field.

[0026] Example 1 A hydrogen evolution cathode was prepared by depositing a molybdenum sulfide coating on a substrate at a film formation temperature of 150℃. The specific preparation process is as follows: S1: Clean the substrate to remove grease and rust from its surface and ensure a firm adhesion of the catalyst layer. Cleaning removes grease and rust from the substrate surface and ensures a firm adhesion of the catalyst layer.

[0027] Specifically, first, prepare a 10% concentration (mass fraction) CY-1003A cleaning agent in an ultrasonic cleaning tank and heat it to 60°C. Place the substrate in the ultrasonic cleaning tank and set the ultrasonic vibration frequency to 28 kHz and the ultrasonic cleaning time to 10 min. After setting, begin ultrasonic cleaning. Subsequently, remove the substrate from the cleaning solution and rinse it with deionized water until the CY-1003A cleaning agent is completely removed. The number of cleaning cycles can be 3-5 times, and can be adjusted as needed; no specific limit is specified here.

[0028] The substrate was ultrasonically cleaned using anhydrous ethanol to remove any moisture adhering to it from the previous step. The ultrasonic vibration frequency was 28 kHz, and the ultrasonic cleaning time was 10 min. The substrate was then ultrasonically cleaned again using anhydrous ethanol to further ensure surface cleanliness. The ultrasonic vibration frequency was 28 kHz, and the ultrasonic cleaning time was 10 min.

[0029] Finally, the substrate was removed and dried with nitrogen. The substrate was 500 mm in size. Nickel foam (NF) with a diameter of 500 mm, a thickness of 0.3 mm, and a porosity of 88.8%.

[0030] S2: Clamping of substrate and target.

[0031] Specifically, a fixture is used to install and fix the mesh substrate and target material. After fixing, the workpiece is placed in the vacuum chamber of the magnetron sputtering coating system. The vertical distance (i.e., target distance) from the target surface to the substrate surface is controlled at 5 cm. After confirming that all components of the coating system are installed, the vacuum chamber door is closed. The fixture is a stainless steel cylinder with a diameter of 15 cm and a height of 50 cm.

[0032] The magnetron sputtering coating system is started, and the vacuum chamber is evacuated until the vacuum level reaches the background vacuum of 6×10⁻⁶. -4 After Pa, high-purity argon gas (working gas) with a purity of 99.99% is introduced, the reaction vacuum in the chamber is adjusted to 1.0 Pa, and heating is started to bring the ambient temperature to 80℃.

[0033] S3: Magnetron sputtering catalyst layer Step S3.1: Perform plasma etching cleaning on the pretreated substrate. Specifically, start the unipolar HALL source, activate the workpiece rotation, and perform plasma etching cleaning on the surface of the pretreated substrate. The chamber's base vacuum level is 5 × 10⁻⁶. -4 The vacuum level in the chamber was 1.0 Pa, followed by the introduction of 99.99% pure argon gas to achieve a reaction vacuum of 1.0 Pa. The plasma cleaning power was 800 W, and the cleaning time was 20 min. Plasma cleaning removes the oxide layer on the surface of the pretreated substrate, enhances the substrate's activity, and thus helps improve the adhesion between the substrate and the molybdenum sulfide coating.

[0034] Step S3.2: Deposition of molybdenum sulfide coating. Specifically, a unipolar pulsed magnetron power supply is started to deposit the molybdenum sulfide coating. During the deposition process, the chamber vacuum is 1.0 Pa, the pulsed magnetron power is 2 kW, the film formation temperature is 80℃, and the deposition time is 30 min, resulting in a molybdenum sulfide coating with a thickness of 1500 nm. After deposition, the magnetron power supply is turned off, and the magnetron sputtering coating system is shut down.

[0035] like Figure 1 As shown, the molybdenum sulfide coating in the hydrogen evolution electrode prepared by the method in Example 1 of the present invention has a worm-like structure, which is uniformly dispersed and grows vertically (longitudinally).

[0036] Example 2 The hydrogen evolution electrode was prepared using the same method as in Example 1, with the only difference being that the temperature at which the molybdenum sulfide coating was deposited was 80°C.

[0037] Example 3 The hydrogen evolution electrode was prepared using the same method as in Example 1, with the only difference being that the temperature at which the molybdenum sulfide coating was deposited was 200°C.

[0038] like Figure 2 As shown, the molybdenum sulfide coating in the hydrogen evolution electrode prepared by the method in Example 3 has an island-like structure and exhibits a large number of agglomerates. The presence of these agglomerated particles affects the catalytic performance of the molybdenum sulfide coating.

[0039] Comparative Example 1 The hydrogen evolution electrode was prepared using the same method as in Example 1, with the only difference being that the temperature at which the molybdenum sulfide coating was deposited was room temperature, 25°C.

[0040] like Figure 3 As shown, the molybdenum sulfide coating in the hydrogen evolution electrode prepared using the method in Comparative Example 1 also exhibits a worm-like structure similar to that in Example 1. From the above... Figure 1-3 It can be seen that as the temperature of molybdenum sulfide coating deposition increases, the molybdenum sulfide coating changes from a vertical (or longitudinal) loose worm-like structure to an island agglomeration growth structure, and the grain size decreases. This is because the sufficient heat obtained causes atoms in the adjacent structures of the molybdenum sulfide film to diffuse into each other and gradually fuse and agglomerate.

[0041] The crystal phases of the hydrogen evolution electrodes in Examples 1, 3, and Comparative Example 1 were analyzed using X-ray diffraction. The specific test results are as follows. Figure 4 As shown.

[0042] Figure 4 The X-ray diffraction (XRD) patterns of the molybdenum sulfide coatings prepared in Examples 1, 3 and Comparative Example 1 of this invention are shown.

[0043] like Figure 4 As shown, (002) and (100) diffraction peaks appeared at 14.3° and 33.7°, respectively, consistent with the standard diffraction peaks of molybdenum sulfide (PDF#37-1492). With the gradual increase in film-forming temperature during molybdenum sulfide deposition, compared to the room temperature sample, the diffraction peaks on the (100) substrate of the sample at an ambient temperature of 150°C were significantly enhanced. Furthermore, the relative intensity of the (100) diffraction peak in the molybdenum sulfide coating first increased and then decreased with increasing film-forming temperature, with the highest relative intensity observed at a deposition temperature of 150°C. This indicates that the vertical (or longitudinal) growth trend is enhanced and then weakened with increasing film-forming temperature, which is consistent with... Figures 1-3 The corresponding SEM image is shown. The appearance of the (100) diffraction peak indicates that there are unsaturated Mo and S edges on the vertically grown molybdenum sulfide coating, which has more active sites for catalysis compared to the horizontally grown molybdenum sulfide coating. On the other hand, it also shows that the growth orientation and morphology of the molybdenum sulfide coating can be controlled by adjusting the temperature of molybdenum sulfide deposition.

[0044] Furthermore, the hydrogen evolution electrodes prepared in Examples 1-3 and Comparative Example 1 were subjected to electrochemical hydrogen evolution tests using an electrochemical workstation. The linear sweep voltammetric curves of the hydrogen evolution electrodes were obtained, and the test results are as follows: Figure 5 A- Figure 5 As shown in B.

[0045] Figure 5 A is the linear sweep voltammetry curve of the hydrogen evolution cathode in Examples 1-3 and Comparative Example 1 of this invention. Figure 5 B is a graph showing the relationship between the temperature and overpotential of the hydrogen evolution cathode in Examples 1-3 and Comparative Example 1 of this invention.

[0046] like Figure 5 As shown in A and 5B, at 100 mA / cm 2 At the specified current densities, the overpotentials of the molybdenum sulfide coatings deposited at room temperature (25℃), 80℃, 150℃, and 200℃ were 255.2 mV, 240.2 mV, 218.2 mV, and 277.2 mV, respectively, exhibiting superior electrocatalytic activity compared to the NF substrate's overpotential of 422.2 mV. Notably, at the same current density, a lower voltage indicates better hydrogen evolution performance of the electrode. The molybdenum sulfide coating deposited at 150℃ showed the best hydrogen evolution catalytic performance.

[0047] Comparative Example 1 (film formation temperature at room temperature) and Example 1 (film formation temperature at 150°C) both exhibited worm-like surface morphologies (e.g. Figure 1 and Figure 3 (Compared to Example 1), but XRD tests showed that the intensity of the characteristic peak of the (100) crystal plane XRD response in Example 1 was weaker than that in Example 1. This result indicates that Example 1 obtained a molybdenum sulfide coating with a more pronounced vertical growth orientation by optimizing the film-forming temperature process parameter of 150°C, thereby improving the hydrogen evolution catalytic performance. In contrast, the surface morphology of the coating in Example 3 (film-forming temperature 200°C) changed, and the intensity of the characteristic peak of the (100) crystal plane XRD response weakened, indicating that the dominant orientation of vertical growth weakened again, and thus the hydrogen evolution catalytic performance decreased again.

[0048] Figure 6 The images show the Raman spectra of molybdenum sulfide coatings prepared at room temperature (Comparative Example 1), 150°C (Example 1), and 200°C (Example 3), respectively. The curves are shown at 288 cm⁻¹. -1 372 cm -1 and 412 cm -1 Three Raman peaks appeared nearby, corresponding to the vibrations E of two S atoms in the MoS2 plane toward the Mo atoms in between. 1 g The vibration of Mo atoms in the opposite direction E 1 2gout-of-plane vibration A of MoS2 coating 1 g The in-plane vibrations originating from the two S atoms toward and away from the Mo atoms in the space between them, as well as the out-of-plane vibrations, correspond to the response characteristics of molybdenum sulfide in the 2H phase.

[0049] In summary, by changing the temperature of magnetron sputtering deposition of molybdenum sulfide coating, thereby altering the crystal structure and morphology of the molybdenum sulfide coating, the electrochemical hydrogen evolution performance of the obtained hydrogen evolution electrode is significantly better than that of the substrate.

[0050] It should be noted that the specific embodiments described above are exemplary, and those skilled in the art can devise various solutions inspired by the disclosure of this invention. These solutions all fall within the scope of this invention and its protection. Those skilled in the art should understand that this specification and its accompanying drawings are illustrative and not intended to limit the scope of the claims. The scope of protection of this invention is defined by the claims and their equivalents.

Claims

1. A method for controlling the morphology of a molybdenum sulfide coating on a hydrogen evolution electrode, characterized in that, Includes the following steps: Select a substrate with surface grease and rust removed, fix the substrate and place it in the vacuum chamber of the magnetron sputtering coating system, start the unipolar HALL source and perform plasma cleaning; The magnetron sputtering coating system is started to deposit a molybdenum sulfide coating on the cleaned substrate. During the deposition process, the vacuum degree of the vacuum chamber of the magnetron sputtering coating system is 0.5~2 Pa, the film formation temperature is 80-200℃, the unipolar pulse magnetron sputtering power is 1~5 kW, and the deposition time is 5~180 min.

2. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, The film-forming temperature is 150℃.

3. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, During the deposition process, the vacuum chamber of the magnetron sputtering coating system has a reaction vacuum of 1.0 Pa, a pulsed magnetron power of 2 kW, a film formation temperature of 80℃, and a deposition time of 30 min.

4. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, The substrate is nickel foam or nickel mesh.

5. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, The porosity of the substrate is 88.8%.

6. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, During plasma cleaning, the background vacuum level of the vacuum chamber in the magnetron sputtering coating system is 5 × 10⁻⁶. -4 ~5×10 -3 The chamber reaction vacuum is 0.1~2 Pa, the plasma cleaning power is 600~2000 W, and the cleaning time is 10~20 min.

7. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, The substrate is ultrasonically cleaned before use, and the cleaning agent is CY-1003A cleaning agent with a mass fraction of 10-20%.

8. The method for controlling the morphology of the molybdenum sulfide coating on the hydrogen evolution electrode according to claim 1, characterized in that, The cleaning agent temperature is maintained at 50-70℃, the ultrasonic vibration frequency for cleaning is 28 kHz, and cleaning is carried out until there is no surface grease or rust on the substrate surface.

9. A hydrogen evolution electrode, characterized in that, The invention comprises a substrate and a molybdenum sulfide catalytic coating grown vertically on the substrate, wherein the molybdenum sulfide catalytic coating is deposited on the substrate using a method for controlling the morphology of the molybdenum sulfide coating of the hydrogen evolution electrode as described in any one of claims 1 to 8.

10. Use of the molybdenum sulfide hydrogen evolution electrode as described in claim 9 in hydrogen production.

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