A method for synthesizing MoS2 / TaS2 composite materials
By preparing MoS2/TaS2 composite materials as electrocatalysts, the problem of low abundance and high cost of platinum catalysts was solved, achieving efficient electrocatalytic hydrogen evolution, reducing costs and improving electrocatalytic performance.
Patent Information
- Application Number
- CN202210816912.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-07-12
- Publication Date
- 2025-10-28
- Estimated Expiration
- 2042-07-12
AI Technical Summary
In existing technologies, platinum (Pt) is used as an electrocatalyst for hydrogen production, but its low abundance and high cost limit its widespread applicability.
Using MoS2/TaS2 composite material as an electrocatalyst, the MoS2/TaS2 composite material was prepared by dissolving molybdenum source and sulfur source in deionized water, adding TaS2 nanosheets and NMP solution, ultrasonically mixing and then immersing in a carbon cloth electrode for hydrothermal reaction.
MoS2/TaS2 composites exhibit good electrical conductivity and charge carrier mobility, reduce charge transfer resistance, increase the specific surface area of active sites, improve hydrogen evolution efficiency, and significantly reduce costs.
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Figure CN115161663B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of nanomaterials technology, and in particular to a MoS2 / TaS2 composite material and its synthesis method. Background Technology
[0002] Hydrogen (H2) is renewable and clean, and as a highly efficient energy carrier with the highest energy density (142 MJ / kg) among all chemical fuels, it is considered one of the most promising green energy sources. Large-scale sustainable hydrogen production requires a suitable electrocatalyst with good natural abundance.
[0003] In the prior art, platinum (Pt) is usually used as an electrocatalyst. The inventors found that although platinum (Pt) has excellent electrocatalytic stability and efficiency, its low abundance and high cost severely limit its wide applicability. Summary of the Invention
[0004] In view of this, the present disclosure provides a MoS2 / TaS2 composite material and a method for synthesizing the same. Using the MoS2 / TaS2 composite material as a catalyst for the hydrogen evolution reaction can improve the efficiency of hydrogen evolution and reduce costs.
[0005] In a first aspect, embodiments of this disclosure provide a MoS2 / TaS2 composite material and a method for synthesizing the same, employing the following technical solution:
[0006] The synthesis method of the MoS2 / TaS2 composite material includes:
[0007] Step S1: Dissolve the molybdenum source and sulfur source in deionized water to form a solution;
[0008] Step S2: Add TaS2 nanosheets and NMP solution to the solution, and mix by ultrasonication to obtain a mixture;
[0009] Step S3: Add a carbon cloth electrode to the mixture, immersing the carbon cloth electrode in the mixture;
[0010] Step S4: Transfer the mixture and carbon cloth electrode to the reaction vessel;
[0011] Step S5: Place the sealed reactor into a forced-air drying oven to carry out the hydrothermal reaction;
[0012] Step S6: After the reactor is cooled, the carbon cloth electrode is removed to obtain a carbon cloth electrode with MoS2 / TaS2 composite material grown on it.
[0013] Optionally, the molybdenum source is sodium molybdate or ammonium molybdate, and the sulfur source is thiourea.
[0014] Optionally, in step S1, the molar ratio of molybdenum to sulfur is 1:0.5-2.5.
[0015] Optionally, in step S2, the molar ratio of molybdenum to tantalum is 5 to 20:1.
[0016] Optionally, the synthesis method further includes: before step S2, ultrasonically treating TaS2 powder in deionized water to obtain TaS2 nanosheets.
[0017] Optionally, the synthesis method further includes: pretreating the carbon cloth electrode before step S3;
[0018] The preprocessing includes:
[0019] A 10% nitric acid solution and a 10% sulfuric acid solution are mixed at a volume ratio of 3:1 to obtain a mixed acid solution.
[0020] After immersing the carbon cloth electrode in the mixed acid solution, it is removed after soaking at room temperature for a certain period of time.
[0021] The removed carbon cloth electrode is placed in a container filled with deionized water and ultrasonically vibrated to remove residual sulfuric acid and nitric acid from the carbon cloth electrode.
[0022] Optionally, in step S4, the mixture and the carbon cloth electrode are transferred to a stainless steel reactor; in step S5, the sealed reactor is placed in a 180℃~220℃ forced-air drying oven and kept at that temperature for 20h~24h to carry out a hydrothermal reaction.
[0023] Optionally, the synthesis method further includes the following steps after step S6:
[0024] Step S7: Clean the carbon cloth electrode sequentially with deionized water and ethanol;
[0025] Step S8: Place the cleaned carbon cloth electrode into a vacuum drying oven for heat preservation and drying;
[0026] Step S9: After the carbon cloth electrode has cooled to room temperature, add Nafion solution to the surface of the carbon cloth electrode and allow it to air dry naturally.
[0027] Optionally, the synthesis method further includes the following steps after step S6:
[0028] Step S10: Centrifuge the remaining solution in the reactor to obtain a black precipitate;
[0029] Step S11: The black precipitate is washed sequentially with deionized water and ethanol;
[0030] Step S12: Place the cleaned black precipitate into a vacuum drying oven and keep it warm to dry;
[0031] Step S13: Collect the dried black precipitate and grind it in a mortar until it is evenly mixed to obtain the MoS2 / TaS2 composite material.
[0032] Secondly, embodiments of this disclosure provide a MoS2 / TaS2 composite material, which is synthesized using the synthesis method for MoS2 / TaS2 composite materials described in any of the above embodiments.
[0033] This invention provides a MoS2 / TaS2 composite material and its synthesis method. The synthesis method includes: firstly, dissolving a molybdenum source and a sulfur source in deionized water to form a solution; then adding TaS2 nanosheets and NMP solution to the solution, ultrasonically mixing to obtain a mixture; then adding a carbon cloth electrode to the mixture, immersing the carbon cloth electrode in the mixture; then transferring the mixture and carbon cloth electrode to a reaction vessel; then placing the sealed reaction vessel in a forced-air drying oven for hydrothermal reaction; after cooling the reaction vessel, removing the carbon cloth electrode to obtain a carbon cloth electrode with the MoS2 / TaS2 composite material grown on it. On the one hand, the MoS2 / TaS2 composite material prepared by this synthesis method not only has good conductivity, effectively reducing charge transfer resistance in electrochemical reactions, but also has excellent charge carrier mobility, resulting in a low Tafel slope. When used as an electrocatalyst, it provides more interfaces that promote charge transport, and the small size of the MoS2 / TaS2 nanosheets increases the specific surface area of the active sites, thus exhibiting excellent electrocatalytic performance and improving hydrogen evolution efficiency. On the other hand, the cost of MoS2 / TaS2 composite materials is significantly lower than that of Pt, which can further reduce costs.
[0034] The above description is merely an overview of the technical solution disclosed herein. In order to better understand the technical means of this disclosure and to implement it in accordance with the contents of the specification, and to make the above and other objects, features and advantages of this disclosure more apparent and understandable, preferred embodiments are described below in detail with reference to the accompanying drawings. Attached Figure Description
[0035] To more clearly illustrate the technical solutions of the embodiments of this disclosure, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this disclosure. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0036] Figure 1 Flowchart of the synthesis method provided in the embodiments of this disclosure Figure 1 ;
[0037] Figure 2 Flowchart of the synthesis method provided in the embodiments of this disclosure Figure 2 ;
[0038] Figure 3 Flowchart of the synthesis method provided in the embodiments of this disclosure Figure 3 ;
[0039] Figure 4 Raman spectra provided for embodiments of this disclosure;
[0040] Figure 5 X-ray diffraction patterns provided in embodiments of this disclosure;
[0041] Figure 6 X-ray photoelectron spectroscopy provided in the embodiments of this disclosure;
[0042] Figure 7a Polarization curves provided for embodiments of this disclosure;
[0043] Figure 7b Provided for the embodiments of this disclosure Figure 7a A magnified view of a portion of the image;
[0044] Figure 8a Scanning electron microscope images provided for embodiments of this disclosure;
[0045] Figure 8b Provided for the embodiments of this disclosure Figure 8a A magnified view of a portion of the image. Detailed Implementation
[0046] The present disclosure will now be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for illustrative purposes only and are not intended to limit the scope of the disclosure. Furthermore, it should be noted that, for ease of description, only the parts relevant to the present disclosure are shown in the accompanying drawings.
[0047] It should be noted that, where there is no conflict, the embodiments and features described in this disclosure can be combined with each other. The technical solutions of this disclosure will now be described in detail with reference to the accompanying drawings and embodiments.
[0048] Unless otherwise stated, the exemplary implementations / embodiments shown are to be understood as providing exemplary features of various details that provide ways in which the technical concepts of this disclosure can be implemented in practice. Therefore, unless otherwise stated, the features of various implementations / embodiments may be additionally combined, separated, interchanged and / or rearranged without departing from the technical concepts of this disclosure.
[0049] The terminology used herein is for the purpose of describing particular embodiments and is not intended to be limiting. As used herein, unless the context clearly indicates otherwise, the singular forms “a” and “the” are intended to include the plural forms as well. Furthermore, when the terms “comprising” and / or “including” and variations thereof are used in this specification, it indicates the presence of the stated features, integrals, steps, operations, parts, components, and / or groups thereof, but does not exclude the presence or addition of one or more other features, integrals, steps, operations, parts, components, and / or groups thereof. It should also be noted that, as used herein, the terms “substantially,” “about,” and other similar terms are used as approximate terms rather than as terms of degree, thus explaining the inherent biases in measurements, calculated values, and / or provided values that would be recognized by one of ordinary skill in the art.
[0050] The inventors have discovered that novel two-dimensional composite structures formed by stacking two different types of two-dimensional nanosheets not only possess novel properties but also exhibit superior performance in the electrocatalytic evolution of hydrogen. For example, the composite material formed by preparing MoS2 nanosheets and MoSe2 nanosheets via a hydrothermal method demonstrates superior electrocatalytic performance compared to individual MoS2 and MoSe2 nanosheets.
[0051] Since 2H-MoS2 and 2H-TaS2 have the same crystal structure, similar lattice constants, and small lattice mismatch rates, they can be easily stitched together to form a composite material. Therefore, it is believed that the unique properties of constructing MoS2 / TaS2 composite materials may be achieved, such as improving the conductivity of MoS2 and obtaining higher electrocatalytic hydrogen evolution performance.
[0052] In this composite material, the 1T phase of TaS2 exhibits greater catalytic activity than the 2H phase because its metallic properties reduce charge transfer resistance, and it also possesses excellent basal surface activity. The hydrogen production rate (or turnover frequency, TOF) of MoS2 is limited because its catalytic activity is largely confined to the edge sites, while the overall basal surface is relatively inert. Therefore, the exposed active edges play a crucial role in the HER reaction. The formation of this structure provides more active sites for hydrogen adsorption, suggesting the existence of more interfaces that promote charge transport within the composite material.
[0053] Based on the above analysis, this disclosure provides a method for synthesizing MoS2 / TaS2 composite materials, specifically, as follows: Figure 1 As shown, the synthesis method of this MoS2 / TaS2 composite material includes:
[0054] Step S1: Dissolve the molybdenum source and sulfur source in deionized water to form a solution.
[0055] Optionally, the molybdenum source is sodium molybdate or ammonium molybdate, and the sulfur source is thiourea.
[0056] Optionally, in step S1, the molar ratio of molybdenum to sulfur is 1:0.5, 1:1, 1:1.5, 1:2, or 1:2.5, that is, the obtained MoS2 can be MoS2(Mo:S=1:0.5), MoS2(Mo:S=1:1), MoS2(Mo:S=1:1.5), MoS2(Mo:S=1:2), or MoS2(Mo:S=1:2.5).
[0057] For example, in step S1, 294–309 mg of molybdenum source and 57–285 mg of sulfur source can be dissolved in 20 mL of deionized water and stirred on a magnetic stirrer for 30 min to form a clear solution. Further, the amount of molybdenum source in the solution formed in step S1 can be selected as 1.5 mmol.
[0058] Step S2: Add TaS2 nanosheets and NMP solution to the solution, and mix by ultrasonication to obtain a mixture.
[0059] Optionally, the amount of TaS2 nanosheets added in step S2 satisfies the following molar ratio: molybdenum to tantalum is 5–20:1, for example, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 12:1, 14:1, 16:1, 18:1, or 20:1. This range of molar ratios allows the MoS2 nanoflowers to effectively coat the TaS2 nanosheets during growth. The amount of NMP solution added in step S2 is 1–5 mL. Adding a solution within this range allows the generated material to be more firmly adsorbed onto the carbon cloth.
[0060] For example, when the molybdenum source and sulfur source of the above mass are added in step S1, 18-74 mg of TaS2 and 3 mL of NMP solution are added in step S2. Further, the sonication time is 10-20 min.
[0061] Optionally, the synthesis method of the MoS2 / TaS2 composite material in this embodiment further includes: before step S2, ultrasonically treating TaS2 powder in deionized water to obtain TaS2 nanosheets. Exemplarily, to obtain TaS2 nanosheets with the aforementioned mass, 18–74 mg of TaS2 powder can be ultrasonically treated in 5–10 mL of deionized water for 24–36 h. The purpose of ultrasonic treatment is to pulverize the TaS2 bulk into nanosheets of approximately several hundred nanometers in size, thereby further increasing the number of active sites and improving catalytic performance.
[0062] Step S3: Add a carbon cloth electrode to the mixture, immersing the carbon cloth electrode in the mixture.
[0063] The reason for choosing carbon cloth electrodes in step S3 is that carbon cloth electrodes have good conductivity and a resistivity of less than 5 mΩ / cm. 2 Furthermore, carbon fiber is relatively hydrophilic and more stable than nickel foam electrodes, making it less likely to react with experimental materials and suitable for growth. Compared to glassy carbon electrodes, carbon cloth electrodes are softer, stronger, and less prone to breakage, making them more suitable as catalyst supports.
[0064] Optionally, the synthesis method of MoS2 / TaS2 composite material in this embodiment further includes: pretreating the carbon cloth electrode before step S3 to improve its surface activity. After treatment, the loaded material can grow uniformly on the carbon cloth electrode and achieve sufficient contact with the aqueous electrolyte, thereby improving the catalytic performance of the electrocatalyst.
[0065] For example, the above preprocessing includes:
[0066] A 10% nitric acid solution and a 10% sulfuric acid solution are mixed at a volume ratio of 3:1 to obtain a mixed acid solution.
[0067] After immersing the carbon cloth electrode in the mixed acid solution, soak it at room temperature for a certain period of time (e.g., 24–36 hours) before removing it.
[0068] Place the removed carbon cloth electrode in a container (such as a beaker) filled with deionized water and sonicate it (e.g., for 10-15 minutes, repeated 2-3 times) to remove residual sulfuric acid and nitric acid from the carbon cloth electrode.
[0069] Step S4: Transfer the mixture and carbon cloth electrode to the reactor.
[0070] Optionally, in step S4, the mixture and carbon cloth electrode are transferred to a stainless steel reactor. The inner liner of the stainless steel reactor can be a polytetrafluoroethylene liner, and the volume of the stainless steel reactor is 50 mL. After the mixture and carbon cloth electrode are transferred to the stainless steel reactor, their volume does not exceed 80% of the volume of the stainless steel reactor.
[0071] Step S5: Place the sealed reactor into a forced-air drying oven to carry out the hydrothermal reaction.
[0072] Optionally, in step S5, the sealed reactor is placed in a forced-air drying oven at 180–220°C and kept at that temperature for 20–24 hours to carry out a hydrothermal reaction. This temperature and time range allows the reaction to proceed more fully, making it easier to grow MoS2 nanoflower-like morphology, more easily coat TaS2 nanosheets, and less prone to detachment during electrocatalytic hydrogen evolution. It also provides more active sites and improves electrocatalytic performance.
[0073] Step S6: After the reactor is cooled, the carbon cloth electrode is removed to obtain a carbon cloth electrode with MoS2 / TaS2 composite material grown on it.
[0074] Optionally, such as Figure 2 As shown, the synthesis method of MoS2 / TaS2 composite material in this embodiment further includes the following steps after step S6:
[0075] Step S7: Clean the carbon cloth electrode with deionized water and ethanol in sequence.
[0076] For example, the carbon cloth electrode can be cleaned 2 to 6 times with deionized water and 1 to 3 times with ethanol. In step S7, cleaning with deionized water and ethanol can remove powder and impurities that are easily detached from the surface of the carbon cloth electrode.
[0077] It should be noted that in the steps after step S6, the carbon cloth electrode must be coated with MoS2 / TaS2 composite material. Any operation performed on the carbon cloth electrode must mean that the same operation is performed on the MoS2 / TaS2 composite material.
[0078] Step S8: Place the cleaned carbon cloth electrode into a vacuum drying oven and keep it warm to dry.
[0079] For example, the carbon cloth electrode is placed in a vacuum drying oven at 50–70°C for 6–8 hours. In step S8, the vacuum drying oven can remove moisture from the carbon cloth electrode and also make the carbon cloth electrode more stable.
[0080] Step S9: After the carbon cloth electrode has cooled to room temperature, add Nafion solution to the surface of the carbon cloth electrode and let it air dry naturally.
[0081] For example, 10–15 μL of Nafion solution is dropped onto the surface of a carbon cloth electrode and then allowed to air dry. The Nafion solution added in step S9, after air drying, forms a polymer film with selective permeability. Simultaneously, after absorbing water, it only allows hydrogen ions to pass through, thus protecting the carbon cloth electrode.
[0082] Optionally, such as Figure 3 As shown, the synthesis method of MoS2 / TaS2 composite material in this embodiment further includes the following steps after step S6:
[0083] Step S10: Centrifuge the remaining solution in the reactor to obtain a black precipitate.
[0084] Step S11: Clean the black precipitate with deionized water and ethanol in sequence.
[0085] For example, wash with deionized water 2 to 6 times, or with ethanol 1 to 3 times.
[0086] Step S12: Place the cleaned black precipitate into a vacuum drying oven and keep it warm to dry.
[0087] For example, place the cleaned black precipitate in a vacuum drying oven at 50–70°C and keep it warm for 6–8 hours.
[0088] Step S13: Collect the dried black precipitate and grind it in a mortar until it is evenly mixed to obtain the MoS2 / TaS2 composite material.
[0089] For example, grind thoroughly in an agate mortar until well mixed.
[0090] It should be noted that steps S7 to S9 can be executed before, after, or simultaneously with steps S10 to S13; no limitation is made here.
[0091] The synthesis method of MoS2 / TaS2 composite material in this disclosure has the following technical advantages:
[0092] On the one hand, the MoS2 / TaS2 composite material prepared by this synthesis method not only has good conductivity, which can effectively reduce the charge transfer resistance in electrochemical reactions, but also has excellent charge carrier mobility, resulting in a low Tafel slope. When used as an electrocatalyst, it provides more interfaces that promote charge transport. Furthermore, the small size of the MoS2 / TaS2 nanosheets increases the specific surface area of the active sites, thus exhibiting excellent electrocatalytic performance and improving the efficiency of hydrogen evolution.
[0093] On the other hand, the cost of MoS2 / TaS2 composites is significantly lower than that of Pt, which could further reduce costs. However, the layered transition metal group chalcogenide structure is very attractive. Studies have shown that the formation of larger active regions in the layered structure generates larger edges, which are key active surfaces for achieving superior electrochemical water splitting performance.
[0094] Furthermore, this disclosure provides a MoS2 / TaS2 composite material, which is synthesized using any of the above-described methods for synthesizing MoS2 / TaS2 composite materials.
[0095] In this embodiment, the MoS2 / TaS2 composite material attached to the carbon cloth electrode can be used as an electrocatalyst for electrochemical testing.
[0096] For example, electrochemical testing includes the following steps:
[0097] a. Electrochemical tests were performed in a standard three-electrode test system, in which a carbon cloth electrode with MoS2 / TaS2 composite material was used as the working electrode, a platinum sheet electrode was used as the counter electrode, an Ag / AgCl electrode was used as the reference electrode, and a 0.5M H2SO4 solution was used as the electrolyte.
[0098] b. Tests were conducted on a CHI660E electrochemical workstation.
[0099] This step can involve one or more of the following: linear sweep voltammetry, cyclic voltammetry, and electrochemical impedance spectroscopy. When performing linear sweep voltammetry, the potential scan range relative to the reversible hydrogen electrode is 0 to -1.2 V, and the scan rate is 5 mV / s.
[0100] Test results show that the MoS2 / TaS2 composite material exhibits excellent catalytic performance as a catalyst for the hydrogen evolution reaction, with MoS2 (Mo:S = 1:1) / TaS2 showing the best performance at 10 mA / cm². 2 The overpotential at the given current density is 87 mV, the Tafel slope is 63 mV / dec, and the electrochemical active area is 145.74 mF / cm², derived from the cyclic voltammetry curve. 2 The charge transfer resistance obtained from electrochemical impedance spectroscopy is 3.25 Ω, and its catalytic performance is higher than that of other MoS2 / TaS2 ratios. The overpotentials of MoS2(Mo:S=1:0.5) / TaS2, MoS2(Mo:S=1:1.5) / TaS2, MoS2(Mo:S=1:2) / TaS2 and MoS2(Mo:S=1:2.5) / TaS2 are 238 mV, 193 mV, 166 mV and 212 mV, respectively.
[0101] To help those skilled in the art to better understand the performance advantages and synthesis methods of the MoS2 / TaS2 composite material in the embodiments of this disclosure, the following embodiments of this disclosure are described with reference to several specific examples.
[0102] Example 1
[0103] The preparation process of the MoS2 / TaS2 composite material in this embodiment includes:
[0104] (1) Dissolve 294 mg of (NH4)2MoO4 and 57 mg of CH4N2S in 20 mL of deionized water, and stir on a magnetic stirrer for 30 min to form a clear solution. The molar ratio of molybdenum to sulfur in the solution is 1:1.
[0105] (2) 73 mg of TaS2 powder was ultrasonically treated in 10 ml of deionized water for 24 h. Then, the ultrasonically treated TaS2 nanosheets and 3 mL of NMP solution were added to the solution in (1) to make the molar ratio of molybdenum to tantalum in the mixture 5:1. After ultrasonic treatment for 20 min, the mixture was homogeneous and a mixture was obtained.
[0106] (3) Mix 10% nitric acid and 10% sulfuric acid solution at a volume ratio of 3:1. After soaking the carbon cloth electrode in the mixture at room temperature for 24 hours, remove it and place it in a beaker containing deionized water for ultrasonic vibration for 20 minutes to fully remove sulfuric acid and nitric acid from the carbon cloth electrode. Add the treated carbon cloth electrode to the mixture in (2) and immerse it in the mixture. Transfer it to a 50ml polytetrafluoroethylene inner liner, tighten the lid, and then put it into a stainless steel reactor and tighten the seal. Place the sealed reactor in a 200℃ drying oven and keep it warm for 24 hours.
[0107] (4) Cool the reaction vessel obtained from the hydrothermal reaction in (3), remove the carbon cloth electrode, and obtain a carbon cloth electrode with MoS2 (Mo:S = 1:0.5) / TaS2 composite material grown on it. Wash it three times with deionized water and three times with ethanol. Place the obtained carbon cloth electrode in a vacuum drying oven at 60°C and keep it warm for 8 hours. After cooling to room temperature, add 15 μL of Nafion solution to the surface of the carbon cloth electrode and let it air dry naturally.
[0108] (5) Centrifuge the remaining solution in the reaction vessel obtained by the hydrothermal reaction in (3). The black precipitate obtained is washed three times with deionized water and three times with ethanol. Then it is placed in a vacuum drying oven at 60°C and kept warm for 8 hours. The product is then collected and ground thoroughly in an agate mortar until it is evenly mixed to obtain MoS2 (Mo:S = 1:0.5) / TaS2 composite material powder.
[0109] Figure 4 The Raman spectrum of the MoS2 (Mo:S = 1:0.5) / TaS2 composite powder from Example 1 is shown. Figure 4 It can be seen that the MoS2 (Mo:S = 1:0.5) / TaS2 powder obtained in Example 1 has a density of 389.9 cm⁻¹. -1 and 413.6cm -1 The characteristic peak at 111.2 cm⁻¹ is basically consistent with that of 2H-type MoS₂. -1 122.9cm -1 145.7cm -1 194.5cm -1 278.4cm -1 and 335.3cm -1 The characteristic peak at 91.1 cm⁻¹ is basically consistent with that of 1T-type MoS₂. -1 and 307.9cm-1 The characteristic peaks at this location are basically consistent with those at TaS2.
[0110] Figure 5 The X-ray diffraction pattern of the MoS2 / TaS2 composite powder in Example 1 is shown. Figure 5 It can be seen that the XRD pattern of the MoS2 (Mo:S = 1:0.5) / TaS2 powder obtained in Example 1 is consistent with the 2H type of molybdenum sulfide in standard card #37-1492, and the diffraction peak at 9.9° is consistent with the 2H type of tantalum sulfide in standard card #21-0569 and standard card #80-0685. Figure 5 The flat peak of (100) in MoS2 indicates poor growth in the planar direction. The (002) peak of TaS2 is more obvious. The weakening of (004), (006) and (008) peaks indicates that most of the TaS2 bulk has been ultrasonically shaped into nanosheets.
[0111] The carbon cloth electrode with MoS2 (Mo:S = 1:0.5) / TaS2 composite material prepared in step (4) is used as a catalyst for electrochemical testing (taking linear sweep voltammetry as an example), including the following steps:
[0112] A carbon cloth electrode with MoS2 (Mo:S = 1:0.5) / TaS2 composite material was used as the working electrode, a platinum sheet electrode as the counter electrode, an Ag / AgCl electrode as the reference electrode, and a 0.5M H2SO4 solution as the electrolyte.
[0113] Linear scanning voltammetry was performed on a CHI660E electrochemical workstation, with a potential scanning range of 0 to -1.2 V relative to the reversible hydrogen electrode and a scanning rate of 5 mV / s.
[0114] Figure 7a The polarization curves obtained from the scan are shown. Figure 7b for Figure 7a A magnified view of a local area (x(-0.6~0.1)y(-100~10)) at 10mA / cm 2 The overpotential at the given current density is 238 mV, meaning that the prepared MoS2 (Mo:S = 1:0.5) / TaS2 composite material has an overpotential of 238 mV as a catalyst for the hydrogen evolution reaction.
[0115] Example 2
[0116] The preparation process of the MoS2 / TaS2 composite material in this embodiment includes:
[0117] (1) Dissolve 294 mg of (NH4)2MoO4 and 114 mg of CH4N2S in 20 mL of deionized water, and stir on a magnetic stirrer for 30 min to form a clear solution. The molar ratio of molybdenum to sulfur in the solution is 1:1.
[0118] (2) 73 mg of TaS2 powder was ultrasonically treated in 10 ml of deionized water for 24 h. Then, the ultrasonically treated TaS2 nanosheets and 3 mL of NMP solution were added to the solution in (1) to make the molar ratio of molybdenum to tantalum in the mixture 5:1. After ultrasonic treatment for 20 min, the mixture was homogeneous and a mixture was obtained.
[0119] (3) Mix 10% nitric acid and 10% sulfuric acid solution at a volume ratio of 3:1. After soaking the carbon cloth electrode in the mixture at room temperature for 24 hours, remove it and place it in a beaker containing deionized water for ultrasonic vibration for 20 minutes to fully remove sulfuric acid and nitric acid from the carbon cloth electrode. Add the treated carbon cloth electrode to the mixture in (2) and immerse it in the mixture. Transfer it to a 50ml polytetrafluoroethylene inner liner, tighten the lid, and then put it into a stainless steel reactor and tighten the seal. Place the sealed reactor in a 220℃ drying oven and keep it warm for 24 hours.
[0120] (4) Cool the reaction vessel obtained from the hydrothermal reaction in (3), remove the carbon cloth electrode, and obtain a carbon cloth electrode with MoS2 (Mo:S = 1:1) / TaS2 composite material grown on it. Wash it three times with deionized water and three times with ethanol. Place the obtained carbon cloth electrode in a vacuum drying oven at 60°C for 8 hours. After cooling to room temperature, add 15 μL of Nafion solution to the surface of the carbon cloth electrode and let it air dry naturally.
[0121] (5) Centrifuge the remaining solution in the reaction vessel obtained by the hydrothermal reaction in (3), and wash the black precipitate three times with deionized water and three times with ethanol. Then, place it in a vacuum drying oven at 60°C and keep it warm for 8 hours. Then collect the product and grind it thoroughly in an agate mortar until it is evenly mixed to obtain MoS2 (Mo:S = 1:1) / TaS2 composite material powder.
[0122] Figure 8a and Figure 8b The image shown is a scanning electron microscope image of a carbon cloth electrode with a MoS2 (Mo:S = 1:1) / TaS2 composite material grown in Example 2. Figure 8a and Figure 8b It can be seen that the MoS2 (Mo:S = 1:1) / TaS2 composite material obtained in Example 2 exhibits nanoflowers formed by nanosheets on the carbon cloth, providing more active sites.
[0123] Figure 4The Raman spectrum of the MoS2 (Mo:S = 1:1) / TaS2 composite powder from Example 2 is shown. Figure 4 It can be seen that the MoS2 (Mo:S = 1:1) / TaS2 powder obtained in Example 2 has a density of 389.9 cm⁻¹. -1 and 413.6cm -1 The characteristic peak at 112.2 cm⁻¹ is basically consistent with that of 2H-type MoS₂. -1 124.4cm -1 149.3cm -1 196.6cm -1 281.4cm -1 and 337.8cm -1 The characteristic peak at 91.1 cm⁻¹ is basically consistent with that of 1T-type MoS₂. -1 and 304.3cm -1 The characteristic peaks at this location are basically consistent with those at TaS2.
[0124] Figure 5 The X-ray diffraction pattern of the MoS2 (Mo:S = 1:1) / TaS2 composite powder in Example 2 is shown. Figure 5 It can be seen that the XRD pattern of the MoS2 (Mo:S = 1:1) / TaS2 powder obtained in Example 2 is consistent with the 2H type of molybdenum sulfide in standard card #37-1492, consistent with standard card #21-0569, and consistent with the 2H type of tantalum sulfide in standard card #80-0685. Figure 5 The sharp peak of (100) in MoS2 indicates good planar growth. The (002) peak of TaS2 is more obvious. The weakening of (004), (006) and (008) peaks indicates that most of the TaS2 bulk has been ultrasonically shaped into nanosheets.
[0125] Figure 6 The X-ray photoelectron spectroscopy (XPS) of the MoS2 (Mo:S = 1:1) / TaS2 composite powder in Example 2 is shown. Figure 6 As can be seen from a, the MoS2 (Mo:S = 1:1) / TaS2 powder obtained in Example 2 contains Mo, S, Ta, C, and O elements. From Figure 6 b indicates that the characteristic peak is located at approximately 231.9 (Mo 3d). 3 / 2 ) and 228.8eV(Mo 3d 5 / 2 At position ), corresponding to 1T-MoS2, it shows a significant downgrade compared to 2H-MoS2 (peak value approximately 232.8 (Mo 3d)). 3 / 2 ) and 229.6eV(Mo 3d 5 / 2 This also confirms the presence of Mo in the MoS2 (Mo:S = 1:1) / TaS2 powder obtained in Example 2.4+ Ions. From Figure 6 c indicates that the two peaks at 163.8 and 161.9 eV are respectively assigned to the S2p phase of the 2H phase. 3 / 2 and S2p 1 / 2 Two additional features appearing at 162.9 and 161.6 eV are related to the 1T phase of MoS2. Compared to the 2H phase, the XPS characteristic peaks of Mo and S in the 1T phase are determined at a lower binding energy side (approximately 1.0 eV). Therefore, the MoS2 (Mo:S = 1:1) / TaS2 powder obtained in Example 2 has a 1T-2H hybrid structure, with the 1T phase MoS2 content reaching as high as 65.5%. In addition, there is another binding energy peak (S2s) at 226.4 eV. The obtained S2p... 3 / 2 and S2p 1 / 2 The peak is attributed to S 2- The existence of Ta 4f 7 / 2 (21.9eV) and Ta 4f 5 / 2 (24.7eV) peak ( Figure 6 d) corresponds to Ta 4+ In the powder, the proportion of TaS2 is very small, therefore the intensity of the Ta 4f spectrum is not as high as that of Mo 3d and S 2p. Furthermore, considering the oxidation susceptibility of metallic TaS2, the additional peaks at 26.1 and 28.0 eV are attributed to Ta. 5+ The existence of.
[0126] Figure 8 shows a scanning electron microscope image of the MoS2 (Mo:S = 1:1) / TaS2 composite powder from Example 2. As can be seen from Figure 8, the generated MoS2 (Mo:S = 1:1) / TaS2 composite material exhibits a morphology of nanoflowers composed of nanosheets on the carbon cloth, providing more active sites.
[0127] The carbon cloth electrode with MoS2 (Mo:S = 1:1) / TaS2 composite material prepared in step (4) is used as a catalyst for electrochemical testing (taking linear sweep voltammetry as an example), including the following steps:
[0128] A carbon cloth electrode with MoS2 (Mo:S = 1:1) / TaS2 composite material was used as the working electrode, a platinum sheet electrode as the counter electrode, an Ag / AgCl electrode as the reference electrode, and a 0.5M H2SO4 solution as the electrolyte.
[0129] Linear scanning voltammetry was performed on a CHI660E electrochemical workstation, with a potential scanning range of 0 to -1.2 V relative to the reversible hydrogen electrode and a scanning rate of 5 mV / s.
[0130] Figure 7aThe polarization curves obtained from the scan are shown. Figure 7b for Figure 7a A magnified view of a local area (x(-0.6~0.1)y(-100~10)) at 10mA / cm 2 The overpotential at the current density was 87 mV, indicating that the prepared MoS2 (Mo:S = 1:1) / TaS2 composite material exhibited excellent catalytic performance as a catalyst for the hydrogen evolution reaction, with an overpotential of 87 mV, which is higher than that of MoS2 / TaS2 composite materials with other ratios.
[0131] Example 3
[0132] The preparation process of the MoS2 / TaS2 composite material in this embodiment includes:
[0133] (1) Dissolve 294 mg of (NH4)2MoO4 and 171 mg of CH4N2S in 20 mL of deionized water, and stir on a magnetic stirrer for 30 min to form a clear solution. The molar ratio of molybdenum to sulfur in the solution is 1:1.
[0134] (2) 73 mg of TaS2 powder was ultrasonically treated in 10 ml of deionized water for 24 h. Then, the ultrasonically treated TaS2 nanosheets and 3 mL of NMP solution were added to the solution in (1) to make the molar ratio of molybdenum to tantalum in the mixture 5:1. After ultrasonic treatment for 20 min, the mixture was homogeneous and a mixture was obtained.
[0135] (3) Mix 10% nitric acid and 10% sulfuric acid solution at a volume ratio of 3:1. After soaking the carbon cloth electrode in the mixture at room temperature for 24 hours, remove it and place it in a beaker containing deionized water for ultrasonic vibration for 20 minutes to fully remove sulfuric acid and nitric acid from the carbon cloth electrode. Add the treated carbon cloth electrode to the mixture in (2) and immerse it in the mixture. Transfer it to a 50ml polytetrafluoroethylene inner liner, tighten the lid, and then put it into a stainless steel reactor and tighten the seal. Place the sealed reactor in a 220℃ drying oven and keep it warm for 24 hours.
[0136] (4) Cool the reaction vessel obtained from the hydrothermal reaction in (3), remove the carbon cloth electrode, and obtain a carbon cloth electrode with MoS2 (Mo:S = 1:1.5) / TaS2 composite material grown on it. Wash it three times with deionized water and three times with ethanol. Place the obtained carbon cloth electrode in a vacuum drying oven at 60℃ and keep it warm for 8 hours. After cooling to room temperature, add 15μL of Nafion solution to the surface of the carbon cloth electrode and let it air dry naturally.
[0137] (5) Centrifuge the remaining solution in the reaction vessel obtained by the hydrothermal reaction in (3). The black precipitate obtained is washed three times with deionized water and three times with ethanol. Then it is placed in a vacuum drying oven at 60°C and kept warm for 8 hours. The product is then collected and ground thoroughly in an agate mortar until it is evenly mixed to obtain MoS2 (Mo:S = 1:1.5) / TaS2 composite powder.
[0138] Figure 4 The Raman spectrum of the MoS2 (Mo:S = 1:1.5) / TaS2 composite powder from Example 3 is shown. Figure 4 It can be seen that the MoS2 (Mo:S = 1:1.5) / TaS2 powder obtained in Example 4 has a compressive strength of 388.2 cm⁻¹. -1 and 413.6cm -1 The characteristic peak at 117.3 cm⁻¹ is basically consistent with that of 2H-type MoS₂. -1 130.0cm -1 155.5cm -1 200.9cm -1 286.4cm -1 and 342.7cm -1 The characteristic peak at 90.0 cm⁻¹ is basically consistent with that of 1T-type MoS₂. -1 and 308.2cm -1 The characteristic peaks at this location are basically consistent with those at TaS2.
[0139] Figure 5 The X-ray diffraction pattern of the MoS2 (Mo:S = 1:1.5) / TaS2 composite powder in Example 3 is shown. Figure 5 It can be seen that the XRD pattern of the MoS2 (Mo:S = 1:1.5) / TaS2 powder obtained in Example 3 is consistent with the 2H form of molybdenum sulfide in standard card #37-1492, consistent with standard card #21-0569, and consistent with the 2H form of tantalum sulfide in standard card #80-0685. Figure 5 The sharp peak of (100) in MoS2 indicates good planar growth. The (002) peak of TaS2 is more obvious. The weakening of (004), (006) and (008) peaks indicates that most of the TaS2 bulk has been ultrasonically shaped into nanosheets.
[0140] The carbon cloth electrode with MoS2 (Mo:S = 1:1.5) / TaS2 composite material prepared in step (4) is used as a catalyst for electrochemical testing (taking linear sweep voltammetry as an example), including the following steps:
[0141] A carbon cloth electrode with MoS2 (Mo:S = 1:1.5) / TaS2 composite material was used as the working electrode, a platinum sheet electrode as the counter electrode, an Ag / AgCl electrode as the reference electrode, and a 0.5M H2SO4 solution as the electrolyte.
[0142] Linear scanning voltammetry was performed on a CHI660E electrochemical workstation, with a potential scanning range of 0 to -1.2 V relative to the reversible hydrogen electrode and a scanning rate of 5 mV / s.
[0143] Figure 7a The polarization curves obtained from the scan are shown. Figure 7b for Figure 7a A magnified view of a local area (x(-0.6~0.1)y(-100~10)) at 10mA / cm 2 The overpotential at the given current density was 193 mV, meaning that the prepared MoS2 (Mo:S = 1:1.5) / TaS2 composite material, when used as a catalyst for the hydrogen evolution reaction, had an overpotential of 193 mV.
[0144] Example 4
[0145] The preparation process of the MoS2 / TaS2 composite material in this embodiment includes:
[0146] (1) Dissolve 294 mg of (NH4)2MoO4 and 228 mg of CH4N2S in 20 mL of deionized water, and stir on a magnetic stirrer for 30 min to form a clear solution. The molar ratio of molybdenum to sulfur in the solution is 1:2.
[0147] (2) 73 mg of TaS2 powder was ultrasonically treated in 10 ml of deionized water for 24 h. Then, the ultrasonically treated TaS2 nanosheets and 3 mL of NMP solution were added to the solution in (1) to make the molar ratio of molybdenum to tantalum in the mixture 5:1. After ultrasonic treatment for 20 min, the mixture was homogeneous and a mixture was obtained.
[0148] (3) Mix 10% nitric acid and 10% sulfuric acid solution at a volume ratio of 3:1. After soaking the carbon cloth electrode in the mixture at room temperature for 24 hours, remove it and place it in a beaker containing deionized water for ultrasonic vibration for 20 minutes to fully remove sulfuric acid and nitric acid from the carbon cloth electrode. Add the treated carbon cloth electrode to the mixture in (2) and immerse it in the mixture. Transfer it to a 50ml polytetrafluoroethylene inner liner, tighten the lid, and then put it into a stainless steel reactor and tighten the seal. Place the sealed reactor in a 200℃ forced-air drying oven and keep it warm for 22 hours.
[0149] (4) Cool the reaction vessel obtained from the hydrothermal reaction in (3), remove the carbon cloth electrode, and obtain a carbon cloth electrode with MoS2 (Mo:S = 1:2) / TaS2 composite material grown on it. Wash it three times with deionized water and three times with ethanol. Place the obtained carbon cloth electrode in a vacuum drying oven at 60°C for 8 hours. After cooling to room temperature, add 15 μL of Nafion solution to the surface of the carbon cloth electrode and let it air dry naturally.
[0150] (5) Centrifuge the remaining solution in the reaction vessel obtained by the hydrothermal reaction in (3), and wash the black precipitate three times with deionized water and three times with ethanol. Then, place it in a vacuum drying oven at 60°C and keep it warm for 8 hours. Then collect the product and grind it thoroughly in an agate mortar until it is mixed evenly to obtain MoS2 (Mo:S = 1:2) / TaS2 composite material powder.
[0151] Figure 4 The Raman spectrum of the MoS2 (Mo:S = 1:2) / TaS2 composite powder from Example 4 is shown. Figure 4 It can be seen that the MoS2 (Mo:S = 1:2) / TaS2 powder obtained in Example 4 has a density of 389.9 cm⁻¹. -1 and 411.7cm -1 The characteristic peak at 120.2 cm⁻¹ is basically consistent with that of 2H-type MoS₂. -1 131.2cm -1 153.0cm -1 204.0cm -1 293.3cm -1 and 344.3cm -1 The characteristic peak at 87.4 cm⁻¹ is basically consistent with that of 1T-type MoS₂. -1 and 307.9cm -1 The characteristic peaks at this location are basically consistent with those at TaS2.
[0152] Figure 5 The X-ray diffraction pattern of the MoS2 (Mo:S = 1:2) / TaS2 composite powder in Example 4 is shown. Figure 5 It can be seen that the XRD pattern of the MoS2 (Mo:S = 1:2) / TaS2 powder obtained in Example 4 is consistent with the 2H type of molybdenum sulfide in standard card 37-1492, consistent with standard card #21-0569, and consistent with the 2H type of tantalum sulfide in standard card 80-0685. Figure 5 The sharp peaks (100) and (110) of MoS2 indicate good planar growth. The (002) peak of TaS2 is more obvious, and the weakening of the (004), (006) and (008) peaks indicates that most of the TaS2 bulk has been ultrasonically shaped into nanosheets.
[0153] The carbon cloth electrode with MoS2 (Mo:S = 1:2) / TaS2 composite material prepared in step (4) is used as a catalyst for electrochemical testing (taking linear sweep voltammetry as an example), including the following steps:
[0154] A carbon cloth electrode with MoS2 (Mo:S = 1:2) / TaS2 composite material was used as the working electrode, a platinum sheet electrode as the counter electrode, an Ag / AgCl electrode as the reference electrode, and a 0.5M H2SO4 solution as the electrolyte.
[0155] Linear scanning voltammetry was performed on a CHI660E electrochemical workstation, with a potential scanning range of 0 to -1.2 V relative to the reversible hydrogen electrode and a scanning rate of 5 mV / s.
[0156] Figure 7a The polarization curves obtained from the scan are shown. Figure 7b for Figure 7a A magnified view of a local area (x(-0.6~0.1)y(-100~10)) at 10mA / cm 2 The overpotential at the given current density is 166 mV, meaning that the prepared MoS2 (Mo:S = 1:2) / TaS2 composite material has an overpotential of 166 mV as a catalyst for the hydrogen evolution reaction.
[0157] Example 5
[0158] The preparation process of the MoS2 / TaS2 composite material in this embodiment includes:
[0159] (1) Dissolve 294 mg of (NH4)2MoO4 and 285 mg of CH4N2S in 20 mL of deionized water, and stir on a magnetic stirrer for 30 min to form a clear solution. The molar ratio of molybdenum to sulfur in the solution is 1:1.
[0160] (2) 73 mg of TaS2 powder was ultrasonically treated in 10 ml of deionized water for 24 h. Then, the ultrasonically treated TaS2 nanosheets and 3 mL of NMP solution were added to the solution in (1) to make the molar ratio of molybdenum to tantalum in the mixture 5:1. After ultrasonic treatment for 20 min, the mixture was homogeneous and a mixture was obtained.
[0161] (3) Mix 10% nitric acid and 10% sulfuric acid solution at a volume ratio of 3:1. After soaking the carbon cloth electrode in the mixture at room temperature for 24 hours, remove it and place it in a beaker containing deionized water for ultrasonic vibration for 20 minutes to fully remove sulfuric acid and nitric acid from the carbon cloth electrode. Add the treated carbon cloth electrode to the mixture in (2) and immerse it in the mixture. Transfer it to a 50ml polytetrafluoroethylene inner liner, tighten the lid, and then put it into a stainless steel reactor and tighten the seal. Place the sealed reactor in a 220℃ drying oven and keep it warm for 24 hours.
[0162] (4) Cool the reaction vessel obtained from the hydrothermal reaction in (3), remove the carbon cloth electrode, and obtain a carbon cloth electrode with MoS2 (Mo:S = 1:2.5) / TaS2 composite material grown on it. Wash it three times with deionized water and three times with ethanol. Place the obtained carbon cloth electrode in a vacuum drying oven at 60°C for 8 hours. After cooling to room temperature, add 15 μL of Nafion solution to the surface of the carbon cloth electrode and let it air dry naturally.
[0163] (5) Centrifuge the remaining solution in the reaction vessel obtained by the hydrothermal reaction in (3). The black precipitate obtained is washed three times with deionized water and three times with ethanol. Then, it is placed in a vacuum drying oven at 60°C and kept warm for 8 hours. The product is then collected and ground thoroughly in an agate mortar until it is evenly mixed to obtain MoS2 (Mo:S = 1:2.5) / TaS2 composite material powder.
[0164] The carbon cloth electrode with MoS2 (Mo:S = 1:2.5) / TaS2 composite material prepared in step (4) is used as a catalyst for electrochemical testing (taking linear sweep voltammetry as an example), including the following steps:
[0165] A carbon cloth electrode with MoS2 (Mo:S = 1:2.5) / TaS2 composite material was used as the working electrode, a platinum sheet electrode as the counter electrode, an Ag / AgCl electrode as the reference electrode, and a 0.5M H2SO4 solution as the electrolyte.
[0166] Linear scanning voltammetry was performed on a CHI660E electrochemical workstation, with a potential scanning range of 0 to -1.2 V relative to the reversible hydrogen electrode and a scanning rate of 5 mV / s.
[0167] Figure 7a The polarization curves obtained from the scan are shown. Figure 7b for Figure 7a A magnified view of a local area (x(-0.6~0.1)y(-100~10)) at 10mA / cm 2The overpotential at the given current density is 212 mV, meaning that the prepared MoS2 (Mo:S = 1:2.5) / TaS2 composite material has an overpotential of 212 mV as a catalyst for the hydrogen evolution reaction.
[0168] In the description of this specification, the references to terms such as "one embodiment / mode," "some embodiments / modes," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment / mode or example is included in at least one embodiment / mode or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment / mode or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments / modes or examples. Furthermore, without contradiction, those skilled in the art can combine and integrate the different embodiments / modes or examples described in this specification, as well as the features of different embodiments / modes or examples.
[0169] Those skilled in the art should understand that the above embodiments are merely for illustrating the present disclosure and are not intended to limit the scope of the disclosure. Those skilled in the art can make other changes or modifications based on the above disclosure, and these changes or modifications still fall within the scope of the present disclosure.
Claims
1. A method for synthesizing a MoS2 / TaS2 composite material, characterized in that, include: Step S1: Dissolve the molybdenum source and sulfur source in deionized water to form a solution; Step S2: Add TaS2 nanosheets to the solution and mix by ultrasonication to obtain a mixture; Step S3: Add a carbon cloth electrode to the mixture, immersing the carbon cloth electrode in the mixture; Step S4: Transfer the mixture and carbon cloth electrode to the reaction vessel; Step S5: Place the sealed reactor into a forced-air drying oven to carry out the hydrothermal reaction; Step S6: After the reactor is cooled, the carbon cloth electrode is removed to obtain a carbon cloth electrode with MoS2 / TaS2 composite material grown on it.
2. The synthesis method according to claim 1, characterized in that, The molybdenum source is sodium molybdate or ammonium molybdate, and the sulfur source is thiourea.
3. The synthesis method according to claim 1, characterized in that, In step S1, the molar ratio of molybdenum to sulfur is 1:0.5-2.
5.
4. The synthesis method according to claim 1, characterized in that, In step S2, the molar ratio of molybdenum to tantalum is 5 to 20:
1.
5. The synthesis method according to claim 1, characterized in that, Also includes: Before step S2, TaS2 powder is ultrasonically treated in deionized water to obtain TaS2 nanosheets.
6. The synthesis method according to claim 1, characterized in that, Also includes: Before step S3, the carbon cloth electrode is pretreated; The preprocessing includes: A 10% nitric acid solution and a 10% sulfuric acid solution are mixed at a volume ratio of 3:1 to obtain a mixed acid solution. After immersing the carbon cloth electrode in the mixed acid solution, it is removed after soaking at room temperature for a certain period of time. The removed carbon cloth electrode is placed in a container filled with deionized water and ultrasonically vibrated to remove residual sulfuric acid and nitric acid from the carbon cloth electrode.
7. The synthesis method according to claim 1, characterized in that, In step S4, the mixture and the carbon cloth electrode are transferred to a stainless steel reactor; in step S5, the sealed reactor is placed in a 180℃~220℃ forced-air drying oven and kept at that temperature for 20h~24h to carry out a hydrothermal reaction.
8. The synthesis method according to claim 1, characterized in that, It also includes the following steps after step S6: Step S7: Clean the carbon cloth electrode sequentially with deionized water and ethanol; Step S8: Place the cleaned carbon cloth electrode into a vacuum drying oven for heat preservation and drying; Step S9: After the carbon cloth electrode has cooled to room temperature, add Nafion solution to the surface of the carbon cloth electrode and allow it to air dry naturally.
9. The synthesis method according to claim 1, characterized in that, It also includes the following steps after step S6: Step S10: Centrifuge the remaining solution in the reactor to obtain a black precipitate; Step S11: The black precipitate is washed sequentially with deionized water and ethanol; Step S12: Place the cleaned black precipitate into a vacuum drying oven and keep it warm to dry; Step S13: Collect the dried black precipitate and grind it in a mortar until it is evenly mixed to obtain the MoS2 / TaS2 composite material.
Citation Information
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