Preparation method of cobalt-doped nano-zinc sulfide oxygen reduction electrocatalytic material

Abstract

The present application relates to the technical field of electrocatalytic material, disclose a kind of preparation method and device of cobalt-doped nano-zinc sulfide oxygen reduction electrocatalytic material, comprising: amino thiazole, anhydrous zinc acetate and the solution of the preset concentration of cobalt nitrate hexahydrate are placed in grinding mortar and mixed grinding and drying, obtain electrocatalytic precursor, after grinding electrocatalytic precursor is placed in porcelain boat and using tube furnace to the pyrolysis precursor to be pyrolyzed, obtain pyrolysis product, using hydrochloric acid to the pyrolysis product is etched, obtain pyrolysis etching product, to pyrolysis etching product is washed and filtered, obtain initial oxygen reduction electrocatalytic material, the initial electrocatalytic product is dried, obtain target oxygen reduction electrocatalytic material.The present application is mainly aimed at solving the problem of current Pt / C catalyst with high price and low catalytic performance.

Description

Technical Field

[0001] This invention relates to a method and apparatus for preparing cobalt-doped nano-zinc sulfide oxygen reduction electrocatalytic material, belonging to the field of electrocatalytic material technology. Background Technology

[0002] Hydrogen fuel cells possess advantages such as being environmentally friendly, having high energy density, and being highly compatible with renewable energy sources, thus gradually becoming a representative of the next generation of energy. The oxygen reduction reaction (ORR) is a crucial half-reaction in hydrogen fuel cells. Currently, most oxygen reduction catalysts used industrially are platinum (Pt)-based noble metal catalysts.

[0003] Currently, the most widely used commercial oxygen reduction catalyst is platinum nanoparticles (Pt / C) supported on carbon black or activated carbon. This is achieved by mixing carbon black or activated carbon with a chloroplatinic acid solution, followed by drying, reduction, heat treatment, and washing to obtain Pt nanoparticles with a particle size of approximately 3–5 nm distributed on the surface of a carbon support; this is the Pt / C catalyst. However, the use of the precious metal Pt results in high prices for commercially available Pt / C catalysts, limiting their large-scale application. Furthermore, the Pt nanoparticles in Pt / C catalysts are prone to detachment during the catalytic reaction, leading to a decrease in catalytic performance. Therefore, current Pt / C catalysts suffer from both high cost and relatively low catalytic performance. Summary of the Invention

[0004] This invention provides a method, apparatus, and computer-readable storage medium for preparing cobalt-doped nano-zinc sulfide oxygen reduction electrocatalyst material, the main purpose of which is to solve the problems of high cost and low catalytic performance of current Pt / C catalysts.

[0005] To achieve the above objectives, the present invention provides a method for preparing a cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material, comprising:

[0006] Aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution were mixed, ground, and dried in a grinding dish to obtain an electrocatalytic precursor.

[0007] The electrocatalytic precursor was ground and placed in a ceramic boat and then placed in the center of a tube furnace to obtain the precursor to be pyrolyzed.

[0008] According to the preset optimal pyrolysis temperature, optimal pyrolysis time and heating gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain the pyrolysis product.

[0009] The pyrolysis product is etched with hydrochloric acid of a preset concentration to obtain a pyrolysis etched product. The pyrolysis etched product is then washed and filtered with deionized water to obtain an initial oxygen reduction electrocatalytic material.

[0010] The initial electrocatalytic product was dried at a preset drying temperature and time to obtain the target oxygen reduction electrocatalytic material.

[0011] Optionally, the step of mixing and grinding aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish and then drying to obtain an electrocatalytic precursor includes:

[0012] A predetermined mass of aminothiazole, anhydrous zinc acetate, and a predetermined volume of cobalt nitrate hexahydrate with a fixed concentration were placed in a grinding dish to obtain electrocatalytic raw materials.

[0013] The electrocatalytic raw materials are mixed, ground, and dried in the grinding dish to obtain the electrocatalytic precursor.

[0014] Optionally, the step of pyrolyzing the precursor to be pyrolyzed using the tubular furnace according to a preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient to obtain pyrolysis products includes:

[0015] According to the heating gradient, the precursor to be pyrolyzed is heated using the tubular furnace to obtain a heating tubular furnace;

[0016] Monitor the center temperature of the heating tube furnace;

[0017] Determine whether the center temperature of the heating tube furnace has reached the optimal pyrolysis temperature;

[0018] If the center temperature of the heating tube furnace does not reach the optimal pyrolysis temperature, then return to the above steps of heating the precursor to be pyrolyzed using the tube furnace according to the heating gradient.

[0019] If the center temperature of the heating tube furnace reaches the optimal pyrolysis temperature, the heating tube furnace is kept at the optimal pyrolysis temperature and optimal pyrolysis time to obtain pyrolysis products.

[0020] Optionally, before pyrolyzing the precursor to be pyrolyzed using the tubular furnace according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient to obtain the pyrolysis products, the method further includes:

[0021] Based on the preset set of test pyrolysis temperatures or test pyrolysis times, obtain the pyrolysis products at different test pyrolysis temperatures or different test pyrolysis times to obtain the temperature test pyrolysis product set or the time test pyrolysis product set.

[0022] The pyrolysis products to be tested at temperature or the pyrolysis products to be tested at time are extracted sequentially from the set of pyrolysis products tested at temperature or time.

[0023] The pyrolysis product to be tested at temperature or the pyrolysis product to be tested at time are etched using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or the etched product to be tested at time.

[0024] The etching product to be tested for temperature or time is washed and filtered with deionized water to obtain the washing product to be tested for temperature or time.

[0025] The temperature-tested washing product or time-tested washing product is dried at a preset drying temperature and drying time to obtain the temperature-tested target product or time-tested target product.

[0026] The pre-constructed glassy carbon electrode is modified using the target product for temperature testing or the target product for time testing to obtain a rotating disk electrode for temperature testing or a rotating disk electrode for time testing. The rotating disk electrode for temperature testing or the rotating disk electrode for time testing is then used as the working electrode for temperature testing or the working electrode for time testing.

[0027] Obtain the counter electrode and reference electrode, and construct a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, counter electrode and reference electrode;

[0028] The temperature test half-wave potential or the time test half-wave potential of the target product to be tested are obtained according to the temperature test three-electrode system or the time test three-electrode system.

[0029] The half-wave potentials of all pyrolysis products at different temperatures in the temperature test pyrolysis product set are summarized to obtain the temperature test half-wave potential set.

[0030] Extract the target temperature pyrolysis product corresponding to the maximum temperature test half-wave potential from the temperature test half-wave potential set.

[0031] Extract the test pyrolysis temperature of the product to be pyrolyzed at the target temperature, and take the test pyrolysis temperature of the product to be pyrolyzed at the target temperature as the optimal pyrolysis temperature.

[0032] The half-wave potentials of all time-tested pyrolysis products in the time-tested pyrolysis product set are summarized to obtain the time-tested half-wave potential set.

[0033] Extract the target time pyrolysis product corresponding to the maximum time test half-wave potential from the set of time test half-wave potentials;

[0034] Extract the test pyrolysis time of the product to be pyrolyzed at the target time, and take the test pyrolysis time of the product to be pyrolyzed at the target time as the optimal pyrolysis time.

[0035] Optionally, obtaining the temperature test half-wave potential or the time test half-wave potential of the target product under test based on the temperature test three-electrode system or the time test three-electrode system includes:

[0036] Linear sweep voltammetry is performed on the temperature testing three-electrode system or the time testing three-electrode system using the temperature testing working electrode or the time testing working electrode to obtain the temperature testing oxygen reduction polarization curve or the time testing oxygen reduction polarization curve.

[0037] Extract the temperature test half-wave potential or the time test half-wave potential of the target product to be tested from the temperature test oxygen reduction polarization curve or the time test oxygen reduction polarization curve.

[0038] Optionally, the step of etching the pyrolysis product to be tested at temperature or time using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or time includes:

[0039] Extract a predetermined mass of the pyrolysis product to be tested at the specified temperature or time from the pyrolysis product to be tested at the specified temperature;

[0040] The predetermined mass of the temperature-tested pyrolysis product or the time-tested pyrolysis product is placed in hydrochloric acid of a preset concentration and etched for a preset etching time to obtain the temperature-tested etched product or the time-tested etched product.

[0041] Optionally, the step of obtaining the counter electrode and reference electrode, and constructing a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, the counter electrode, and the reference electrode, includes:

[0042] The pre-constructed graphite rod was used as the counter electrode, and the pre-constructed Ag / AgCl electrode was used as the reference electrode.

[0043] The temperature testing three-electrode system is constructed based on the counter electrode, reference electrode, temperature testing working electrode, and pre-prepared test solution.

[0044] The time-testing three-electrode system is constructed based on the counter electrode, reference electrode, time-testing working electrode, and test solution.

[0045] Optionally, the step of performing linear sweep voltammetry on the temperature testing three-electrode system or the time testing three-electrode system using the temperature testing working electrode or the time testing working electrode to obtain the temperature-tested oxygen reduction polarization curve or the time-tested oxygen reduction polarization curve includes:

[0046] A preset test sweep speed is applied to the temperature test working electrode or the time test working electrode, and the electrolytic current of the temperature test working electrode or the time test working electrode is recorded.

[0047] Based on the test scan rate and electrolysis current, plot the oxygen reduction polarization curve for temperature test or the oxygen reduction polarization curve for time test.

[0048] Optionally, after drying the initial electrocatalytic product at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material, the method further includes:

[0049] The oxygen reduction electrocatalytic performance curves of the target oxygen reduction electrocatalytic material and the oxygen reduction catalytic performance curves of the commercial platinum-carbon material are obtained according to the preset comparison time.

[0050] The oxygen reduction electrocatalytic performance curves of the target oxygen reduction electrocatalytic material and the commercial platinum-carbon material were plotted on the same oxygen reduction catalytic performance-time coordinate system to obtain a comparison chart of the oxygen reduction electrocatalytic performance of the target oxygen reduction electrocatalytic material and the commercial platinum-carbon material.

[0051] To address the aforementioned problems, the present invention also provides an apparatus for preparing a cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material, the apparatus comprising:

[0052] The electrocatalytic precursor preparation module is used to mix and grind aminothiazole, anhydrous zinc acetate and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish and then dry them to obtain the electrocatalytic precursor.

[0053] The pyrolysis module is used to grind the electrocatalytic precursor, place it in a ceramic boat, and put it in the center of a tube furnace to obtain the precursor to be pyrolyzed; according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain the pyrolysis product.

[0054] The etching and washing module is used to etch the pyrolysis product with hydrochloric acid of a preset concentration to obtain pyrolysis etched product, and to wash and filter the pyrolysis etched product with deionized water to obtain the initial oxygen reduction electrocatalytic material.

[0055] The drying module is used to dry the initial electrocatalytic product at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material.

[0056] To address the above problems, the present invention also provides an electronic device, the electronic device comprising:

[0057] At least one processor; and,

[0058] A memory communicatively connected to the at least one processor; wherein,

[0059] The memory stores instructions that can be executed by the at least one processor to implement the above-described method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material.

[0060] To address the aforementioned problems, the present invention also provides a computer-readable storage medium storing at least one instruction, which is executed by a processor in an electronic device to implement the above-described method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material.

[0061] Compared to the problems described in the background art, the embodiments of the present invention involve pyrolyzing the ground electrocatalytic precursor to obtain pyrolysis products, then etching the pyrolysis products and washing and filtering them with deionized water to obtain the initial oxygen reduction electrocatalytic material. Finally, the initial oxygen reduction electrocatalytic material is dried to obtain the target oxygen reduction electrocatalytic material. Since the electrocatalytic precursor contains all the constituent elements of the target oxygen reduction electrocatalytic material, it is necessary to determine the compounds to be mixed when obtaining the electrocatalytic precursor. After determining that the compounds to be mixed are aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution, they can be placed in a grinding dish for mixing, grinding, and drying to obtain the electrocatalytic precursor. After obtaining the electrocatalytic precursor, it can be... After grinding, the material is placed in a ceramic boat and then in the center of a tube furnace to obtain the precursor to be pyrolyzed. The most crucial step is then the pyrolysis of this precursor. Before pyrolysis, the optimal pyrolysis temperature and time need to be determined experimentally. Using the optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the precursor is pyrolyzed in the tube furnace to obtain the pyrolysis product. This product can then be etched using hydrochloric acid of a preset concentration to obtain the pyrolysis-etched product. The pyrolysis-etched product is then washed and filtered with deionized water to obtain the initial oxygen reduction electrocatalyst material. Finally, the initial electrocatalyst product is dried at a preset drying temperature and time to obtain the target oxygen reduction electrocatalyst material. Therefore, the cobalt-doped nano-zinc sulfide oxygen reduction electrocatalyst material preparation method, apparatus, electronic equipment, and computer-readable storage medium proposed in this invention primarily aim to solve the problems of high cost and low catalytic performance of current Pt / C catalysts. Attached Figure Description

[0062] Figure 1 This is a schematic flowchart of a method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material according to an embodiment of the present invention;

[0063] Figure 2The oxygen reduction polarization curve was obtained by temperature testing.

[0064] Figure 3 For time-dependent oxygen reduction polarization curves;

[0065] Figure 4 Scanning transmission electron microscope (STEM) image of the target oxygen reduction electrocatalyst material;

[0066] Figure 5 X-ray energy dispersive spectroscopy (EDS) image of the target oxygen reduction electrocatalyst material;

[0067] Figure 6 X-ray diffraction (XRD) peak patterns of the target oxygen reduction electrocatalytic material and the ZnS standard card (PDF#39-1363);

[0068] Figure 7 X-ray photoelectron spectroscopy (XPS) of the target oxygen reduction electrocatalyst material;

[0069] Figure 8 Comparison of ORR electrocatalytic performance between the target oxygen reduction electrocatalytic material (Co-ZnS / NC) and commercial Pt / C;

[0070] Figure 9 This is a functional block diagram of an apparatus for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material according to an embodiment of the present invention;

[0071] Figure 10 This is a schematic diagram of an electronic device for implementing the method of preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material according to an embodiment of the present invention.

[0072] The objectives, features, and advantages of this invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0073] It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

[0074] This application provides a method for preparing a cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst. The execution entity of this method includes, but is not limited to, at least one of the following electronic devices that can be configured to execute the method provided in this application: a server, a terminal, etc. In other words, the method for preparing the cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst can be executed by software or hardware installed on a terminal device or a server device. The server includes, but is not limited to, a single server, a server cluster, a cloud server, or a cloud server cluster.

[0075] Example 1:

[0076] Reference Figure 1 The diagram shown is a schematic flow chart of a method for preparing a cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material according to an embodiment of the present invention. In this embodiment, the method for preparing the cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material includes:

[0077] S1. Place aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish, mix and grind them, and then dry them to obtain an electrocatalytic precursor.

[0078] In this embodiment of the invention, the aminothiazole is an organic compound with the molecular formula C3H4N2S, and can be 2-aminothiazole or 4-aminothiazole. The concentration of the pre-set concentration of the cobalt nitrate hexahydrate solution can be 0.1 mol / L. The electrocatalytic precursor refers to the precursor of the cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material.

[0079] Specifically, the step of mixing, grinding, and drying aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish to obtain an electrocatalytic precursor includes:

[0080] A predetermined mass of aminothiazole, anhydrous zinc acetate, and a predetermined volume of cobalt nitrate hexahydrate with a fixed concentration were placed in a grinding dish to obtain electrocatalytic raw materials.

[0081] The electrocatalytic raw materials are mixed, ground, and dried in the grinding dish to obtain the electrocatalytic precursor.

[0082] Furthermore, the mass of the aminothiazole and anhydrous zinc acetate, and the volume of 0.1 mol / L cobalt nitrate hexahydrate should be configured according to the yield of the cobalt-doped zinc sulfide nano-oxidation electrocatalyst material. However, the ratio of aminothiazole, anhydrous zinc acetate, and a fixed concentration of cobalt nitrate hexahydrate is fixed at 1 g:1 g:1 ml, for example: 1 g aminothiazole, 1 g anhydrous zinc acetate, and 1 ml of a fixed concentration of cobalt nitrate hexahydrate. The fixed concentration of cobalt nitrate hexahydrate can be 0.1 mol / L. The mixing and grinding time can be 30 min, determined according to the specific grinding effect. The drying time after mixing and grinding can be 12 h.

[0083] Understandably, the electrocatalytic raw materials refer to the raw materials used to prepare the cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material. The cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material contains the following elements: Co (cobalt), Zn (zinc), S (sulfur), N (nitrogen) and C (carbon). All of the above five elements are contained in the electrocatalytic raw materials.

[0084] It should be understood that developing non-noble metal catalysts with high oxygen reduction (ORR) activity that can replace Pt is one of the core research directions for current hydrogen fuel cell electrode materials. Transition metals and their sulfides are catalytic materials with high ORR activity. Carbon materials, with their large specific surface area and abundant doping / defect sites, play a crucial role in increasing the loading capacity of transition metal catalysts and enhancing the diffusion and mass transfer of reactants / products. High ORR-active transition metal nanoparticles, if loaded onto carbon materials rich in doping sites, can achieve highly efficient catalysis of the ORR reaction.

[0085] S2. The electrocatalytic precursor is ground and placed in a ceramic boat and then placed in the center of a tube furnace to obtain the precursor to be pyrolyzed.

[0086] Optionally, the preparation of the cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material via electrocatalytic precursor requires pyrolysis, which can be achieved by placing the electrocatalytic precursor in the center of a tube furnace for pyrolysis.

[0087] S3. Based on the preset optimal pyrolysis temperature, optimal pyrolysis time and heating gradient, the precursor to be pyrolyzed is pyrolyzed using the tubular furnace to obtain the pyrolysis product.

[0088] Furthermore, the optimal pyrolysis temperature refers to the highest temperature at which the precursor to be pyrolyzed is pyrolyzed; the optimal pyrolysis time refers to the time required to pyrolyze the precursor at the specified pyrolysis temperature; and the temperature gradient refers to the temperature increase per minute at the center of the tubular furnace as the temperature rises from the initial temperature to the pyrolysis temperature. The initial temperature refers to the temperature at the center of the tubular furnace when the pyrolysis of the precursor begins.

[0089] In this embodiment of the invention, the step of pyrolyzing the precursor to be pyrolyzed using the tubular furnace according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient to obtain pyrolysis products includes:

[0090] According to the heating gradient, the precursor to be pyrolyzed is heated using the tubular furnace to obtain a heating tubular furnace;

[0091] Monitor the center temperature of the heating tube furnace;

[0092] Determine whether the center temperature of the heating tube furnace has reached the optimal pyrolysis temperature;

[0093] If the center temperature of the heating tube furnace does not reach the optimal pyrolysis temperature, then return to the above steps of heating the precursor to be pyrolyzed using the tube furnace according to the heating gradient.

[0094] If the center temperature of the heating tube furnace reaches the optimal pyrolysis temperature, the heating tube furnace is kept at the optimal pyrolysis temperature and optimal pyrolysis time to obtain pyrolysis products.

[0095] Furthermore, the temperature gradient should be 5℃ / min, the optimal pyrolysis temperature should be 900℃, and the optimal pyrolysis time should be 2h.

[0096] Specifically, before pyrolyzing the precursor to be pyrolyzed using the tubular furnace according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient to obtain the pyrolysis products, the method further includes:

[0097] Based on the preset set of test pyrolysis temperatures or test pyrolysis times, obtain the pyrolysis products at different test pyrolysis temperatures or different test pyrolysis times to obtain the temperature test pyrolysis product set or the time test pyrolysis product set.

[0098] The pyrolysis products to be tested at temperature or the pyrolysis products to be tested at time are extracted sequentially from the set of pyrolysis products tested at temperature or time.

[0099] The pyrolysis product to be tested at temperature or the pyrolysis product to be tested at time are etched using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or the etched product to be tested at time.

[0100] The etching product to be tested for temperature or time is washed and filtered with deionized water to obtain the washing product to be tested for temperature or time.

[0101] The temperature-tested washing product or time-tested washing product is dried at a preset drying temperature and drying time to obtain the temperature-tested target product or time-tested target product.

[0102] The pre-constructed glassy carbon electrode is modified using the target product for temperature testing or the target product for time testing to obtain a rotating disk electrode for temperature testing or a rotating disk electrode for time testing. The rotating disk electrode for temperature testing or the rotating disk electrode for time testing is then used as the working electrode for temperature testing or the working electrode for time testing.

[0103] Obtain the counter electrode and reference electrode, and construct a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, counter electrode and reference electrode;

[0104] The temperature test half-wave potential or the time test half-wave potential of the target product to be tested are obtained according to the temperature test three-electrode system or the time test three-electrode system.

[0105] The half-wave potentials of all pyrolysis products at different temperatures in the temperature test pyrolysis product set are summarized to obtain the temperature test half-wave potential set.

[0106] Extract the target temperature pyrolysis product corresponding to the maximum temperature test half-wave potential from the temperature test half-wave potential set.

[0107] Extract the test pyrolysis temperature of the product to be pyrolyzed at the target temperature, and take the test pyrolysis temperature of the product to be pyrolyzed at the target temperature as the optimal pyrolysis temperature.

[0108] The half-wave potentials of all time-tested pyrolysis products in the time-tested pyrolysis product set are summarized to obtain the time-tested half-wave potential set.

[0109] Extract the target time pyrolysis product corresponding to the maximum time test half-wave potential from the set of time test half-wave potentials;

[0110] Extract the test pyrolysis time of the product to be pyrolyzed at the target time, and take the test pyrolysis time of the product to be pyrolyzed at the target time as the optimal pyrolysis time.

[0111] Understandably, the set of test pyrolysis temperatures refers to the set of highest test temperatures for pyrolyzing the precursor to be pyrolyzed, which can be 700℃, 800℃, 900℃, and 950℃. The set of test pyrolysis times refers to the set of times for pyrolyzing the precursor to be pyrolyzed at the highest test temperature, which can be 1h, 2h, and 3h. The preset concentration of hydrochloric acid can be 2mol / L.

[0112] In this embodiment of the invention, obtaining the temperature test half-wave potential of the target product to be tested or the time test half-wave potential of the target product to be tested based on the temperature test three-electrode system or the time test three-electrode system includes:

[0113] Linear sweep voltammetry is performed on the temperature testing three-electrode system or the time testing three-electrode system using the temperature testing working electrode or the time testing working electrode to obtain the temperature testing oxygen reduction polarization curve or the time testing oxygen reduction polarization curve.

[0114] Extract the temperature test half-wave potential or the time test half-wave potential of the target product to be tested from the temperature test oxygen reduction polarization curve or the time test oxygen reduction polarization curve.

[0115] For details, please refer to the oxygen reduction polarization curve obtained from the temperature test. Figure 2 As shown, Figure 2 One curve in the graph represents a temperature-tested oxygen reduction polarization curve. The time-tested oxygen reduction polarization curve can be found in [reference needed]. Figure 3 As shown, Figure 3One of the curves in the graph represents a time-tested oxygen reduction polarization curve.

[0116] In this embodiment of the invention, the step of performing linear sweep voltammetry on the temperature-testing three-electrode system or the time-testing three-electrode system using the temperature-testing working electrode or the time-testing working electrode to obtain the temperature-tested oxygen reduction polarization curve or the time-tested oxygen reduction polarization curve includes:

[0117] A preset test sweep speed is applied to the temperature test working electrode or the time test working electrode, and the electrolytic current of the temperature test working electrode or the time test working electrode is recorded.

[0118] Based on the test scan rate and electrolysis current, plot the oxygen reduction polarization curve for temperature test or the oxygen reduction polarization curve for time test.

[0119] Further, the etching of the pyrolysis product to be tested at temperature or time using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or time includes:

[0120] Extract a predetermined mass of the pyrolysis product to be tested at the specified temperature or time from the pyrolysis product to be tested at the specified temperature;

[0121] The predetermined mass of the temperature-tested pyrolysis product or the time-tested pyrolysis product is placed in hydrochloric acid of a preset concentration and etched for a preset etching time to obtain the temperature-tested etched product or the time-tested etched product.

[0122] Explained, the predetermined mass of the pyrolysis product to be tested at the predetermined temperature or time can be 100 mg. The etching time can be 4 h.

[0123] It should be understood that the drying temperature can be 60℃, and the drying time can be 12 hours. The glassy carbon electrode can be a rotating disk electrode (RDE) with a diameter of 5 mm. When the rotating disk electrode rotates, the solution can undergo laminar flow on the surface of the rotating disk electrode, causing the thickness of the diffusion layer on the electrode surface to change with the rotation speed.

[0124] In detail, the acquisition of the counter electrode and reference electrode, and the construction of a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, the counter electrode, and the reference electrode, includes:

[0125] The pre-constructed graphite rod was used as the counter electrode, and the pre-constructed Ag / AgCl electrode was used as the reference electrode.

[0126] The temperature testing three-electrode system is constructed based on the counter electrode, reference electrode, temperature testing working electrode, and pre-prepared test solution.

[0127] The time-testing three-electrode system is constructed based on the counter electrode, reference electrode, time-testing working electrode, and test solution.

[0128] Furthermore, the test solution can be an O2-saturated 0.1 mol / L KOH solution.

[0129] It should be understood that the linear sweep voltammetry test refers to the test method of applying a linearly changing voltage to the working electrode of the temperature test or the working electrode of the time test in a three-electrode system of temperature test or time test, and recording the electrolytic current on the working electrode of temperature test or time test. The curve of the electrolytic current changing with the electrode potential is called the linear sweep voltammetry graph.

[0130] Furthermore, such as Figure 2 As shown, when the pyrolysis temperatures are tested at 700℃, 800℃, 900℃, and 950℃, the corresponding half-wave potentials are 0.59V vs RHE, 0.76V vs RHE, 0.86V vs RHE, and 0.83V vs RHE, respectively. Figure 3 As shown, when the pyrolysis time is tested at 1h, 2h and 3h, the corresponding half-wave potentials are 0.85V vs RHE, 0.87V vs RHE and 0.84V vs RHE, respectively.

[0131] Understandable, see reference Figure 2 As shown, the maximum temperature test half-wave potential in the temperature test half-wave potential set is 0.86V vs RHE, and the target temperature corresponding to the maximum temperature test half-wave potential is the test pyrolysis temperature of the product to be pyrolyzed, which is 900℃. At this time, the optimal pyrolysis temperature is 900℃.

[0132] Further, see Figure 3 As shown, the maximum time test half-wave potential in the time test half-wave potential concentration is 0.87Vvs RHE, and the target time for the test pyrolysis of the product to be pyrolyzed corresponding to the maximum time test half-wave potential is 2h. At this time, the optimal pyrolysis time is 2h.

[0133] It should be understood that the determination of the optimal pyrolysis temperature and optimal pyrolysis time is also related to the degree of refinement of the test pyrolysis temperature set and the test pyrolysis time set. For example, when the test pyrolysis temperature set is refined to 800℃, 825℃, 850℃, 875℃, 900℃, 925℃ and 950℃, the optimal pyrolysis temperature can be one of 825℃, 850℃, 875℃, 900℃ and 925℃.

[0134] Optionally, when obtaining pyrolysis products at different test pyrolysis temperatures based on the test pyrolysis temperature set, the pyrolysis time can be set to 2 hours, and when obtaining pyrolysis products at different test pyrolysis times based on the test pyrolysis time set, the pyrolysis temperature can be set to 900℃, thereby achieving the effect of controlling a single variable.

[0135] S4. The pyrolysis product is etched with hydrochloric acid of a preset concentration to obtain a pyrolysis etched product. The pyrolysis etched product is then washed and filtered with deionized water to obtain an initial oxygen reduction electrocatalytic material.

[0136] Understandably, the concentration of the hydrochloric acid at the preset concentration can be 2.0 mol / L. The etching method of the pyrolysis etching product is the same as that of the pyrolysis product to be tested at temperature or time, and will not be described again here.

[0137] S5. The initial electrocatalytic product is dried at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material.

[0138] In this embodiment of the invention, the drying temperature can be 60°C, and the drying time can be 12 hours. The target oxygen reduction electrocatalyst material refers to a cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material prepared at the optimal pyrolysis temperature and optimal pyrolysis time, and its chemical formula can be Co-ZnS / NC.

[0139] Understandably, this invention uses cobalt (Co)-doped zinc sulfide (ZnS) nanoparticles dispersed on the surface of nitrogen (N)-doped carbon material (Co-ZnS / NC) to prepare a catalyst with high oxygen reduction (ORR) activity (targeted oxygen reduction electrocatalytic material). Compared with traditional Pt / C catalysts, the targeted oxygen reduction electrocatalytic material has the following advantages: (1) Zinc sulfide (ZnS) is inexpensive, with a significant price advantage over platinum (Pt); (2) The carbon substrate is rich in N doping elements, which can form chemical bonds with Zn, anchoring ZnS nanoparticles and improving catalytic stability.

[0140] For details, please refer to Figure 4 As shown, Figure 4The image shows a scanning transmission electron microscope (STEM) image of the target oxygen reduction electrocatalyst material, revealing that it is carbon-supported ZnS nanoparticles with a diameter of approximately 20 nm. (See also...) Figure 5 As shown, Figure 5 The X-ray energy dispersive spectroscopy (EDS) image of the target oxygen reduction electrocatalyst material shows that the nanoparticles in the target oxygen reduction electrocatalyst material are composed of three elements: zinc (Zn), sulfur (S), and cobalt (Co), and the carbon substrate is rich in doped nitrogen (N) elements.

[0141] Further, see Figure 6 As shown, Figure 6 X-ray diffraction (XRD) peak patterns of the target oxygen reduction electrocatalyst material and the ZnS standard card (PDF#39-1363), from... Figure 6 The X-ray diffraction (XRD) patterns of the target oxygen reduction electrocatalyst material and the ZnS standard card (PDF#39-1363) showed good peak matching, indicating that the target oxygen reduction electrocatalyst material contains ZnS. However, no peaks in the XRD pattern of the target oxygen reduction electrocatalyst material matched those in the XRD pattern of Co, indicating that the Co content was very low and that it was only doped into ZnS. Inductively coupled plasma mass spectrometry (ICP-MS) analysis showed that the Co content in the target oxygen reduction electrocatalyst material was 0.4 wt.%, which explained why the XRD pattern did not show Co peaks.

[0142] Understandable, see reference Figure 7 As shown, Figure 7 X-ray photoelectron spectroscopy (XPS) of the target oxygen reduction electrocatalyst material revealed elemental peaks for C, N, S, and Zn, confirming the presence of these elements. Simultaneously, the XPS also showed the presence of Zn-N, Zn-S, and CN / CS bonds.

[0143] Furthermore, after drying the initial electrocatalytic product at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material, the method further includes:

[0144] The oxygen reduction electrocatalytic performance curves of the target oxygen reduction electrocatalytic material and the oxygen reduction catalytic performance curves of the commercial platinum-carbon material are obtained according to the preset comparison time.

[0145] The oxygen reduction electrocatalytic performance curves of the target oxygen reduction electrocatalytic material and the commercial platinum-carbon material were plotted on a relative current-time coordinate system to obtain a comparison chart of the oxygen reduction electrocatalytic performance of the target oxygen reduction electrocatalytic material and the commercial platinum-carbon material.

[0146] For details, please refer to Figure 8 As shown, the relative current-time coordinate system is a coordinate system with relative current as the vertical axis and test time as the horizontal axis. Figure 8 This is a comparison of the oxygen reduction (ORR) electrocatalytic performance of the target oxygen reduction electrocatalytic material (Co-ZnS / NC) and a commercial platinum-carbon (Pt / C) material. Both were tested using O2-saturated 0.1 mol / L KOH solutions. Figure 8 As can be seen, after 100 hours of continuous testing, the catalytic performance retention rate of Co-ZnS / NC reached 91%, while the performance of commercial Pt / C declined by more than 40%. This proves that Co-ZnS / NC achieved better ORR electrocatalytic performance than Pt / C in alkaline electrolyte.

[0147] Compared to the problems described in the background art, the embodiments of the present invention involve pyrolyzing the ground electrocatalytic precursor to obtain pyrolysis products, then etching the pyrolysis products and washing and filtering them with deionized water to obtain the initial oxygen reduction electrocatalytic material. Finally, the initial oxygen reduction electrocatalytic material is dried to obtain the target oxygen reduction electrocatalytic material. Since the electrocatalytic precursor contains all the constituent elements of the target oxygen reduction electrocatalytic material, it is necessary to determine the compounds to be mixed when obtaining the electrocatalytic precursor. After determining that the compounds to be mixed are aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution, they can be placed in a grinding dish for mixing, grinding, and drying to obtain the electrocatalytic precursor. After obtaining the electrocatalytic precursor, it can be... After grinding, the material is placed in a ceramic boat and then in the center of a tube furnace to obtain the precursor to be pyrolyzed. The most crucial step is then the pyrolysis of this precursor. Before pyrolysis, the optimal pyrolysis temperature and time need to be determined experimentally. Using the optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the precursor is pyrolyzed in the tube furnace to obtain the pyrolysis product. This product can then be etched using hydrochloric acid of a preset concentration to obtain the pyrolysis-etched product. The pyrolysis-etched product is then washed and filtered with deionized water to obtain the initial oxygen reduction electrocatalyst material. Finally, the initial electrocatalyst product is dried at a preset drying temperature and time to obtain the target oxygen reduction electrocatalyst material. Therefore, the cobalt-doped nano-zinc sulfide oxygen reduction electrocatalyst material preparation method, apparatus, electronic equipment, and computer-readable storage medium proposed in this invention primarily aim to solve the problems of high cost and low catalytic performance of current Pt / C catalysts.

[0148] Example 2:

[0149] like Figure 9The diagram shown is a functional block diagram of an apparatus for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material according to an embodiment of the present invention.

[0150] The apparatus 100 for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material according to the present invention can be installed in an electronic device. Depending on the functions to be performed, the apparatus 100 may include an electrocatalytic precursor preparation module 101, a pyrolysis module 102, an etching and washing module 103, and a drying module 104. The module described in this invention can also be referred to as a unit, which refers to a series of computer program segments that can be executed by the processor of an electronic device and can perform a fixed function, and which are stored in the memory of the electronic device.

[0151] The electrocatalytic precursor preparation module 101 is used to mix and grind aminothiazole, anhydrous zinc acetate and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish and then dry them to obtain an electrocatalytic precursor.

[0152] The pyrolysis module 102 is used to grind the electrocatalytic precursor, place it in a ceramic boat, and place it in the center of a tube furnace to obtain a precursor to be pyrolyzed; according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain pyrolysis products.

[0153] The etching and washing module 103 is used to etch the pyrolysis product with hydrochloric acid of a preset concentration to obtain pyrolysis etching product, and to wash and filter the pyrolysis etching product with deionized water to obtain the initial oxygen reduction electrocatalytic material.

[0154] The drying module 104 is used to dry the initial electrocatalytic product at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material.

[0155] In detail, the modules in the cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material preparation apparatus 100 described in this embodiment of the invention employ the same methods as described above during use. Figure 1 The preparation method of the cobalt-doped nano-zinc sulfide oxygen reduction electrocatalyst material described in the article uses the same technical means and can produce the same technical effect, so it will not be repeated here.

[0156] Example 3:

[0157] like Figure 10 The diagram shown is a schematic diagram of an electronic device for preparing a method for cobalt-doped nano-zinc sulfide oxygen reduction electrocatalytic material according to an embodiment of the present invention.

[0158] The electronic device 1 may include a processor 10, a memory 11, a bus 12 and a communication interface 13, and may also include a computer program stored in the memory 11 and capable of running on the processor 10, such as a program for preparing cobalt-doped nano-zinc sulfide oxygen reduction electrocatalytic material.

[0159] The memory 11 includes at least one type of readable storage medium, such as flash memory, portable hard drive, multimedia card, card-type memory (e.g., SD or DX memory), magnetic memory, disk, optical disk, etc. In some embodiments, the memory 11 can be an internal storage unit of the electronic device 1, such as a portable hard drive. In other embodiments, the memory 11 can be an external storage device of the electronic device 1, such as a plug-in portable hard drive, SmartMediaCard (SMC), SecureDigital (SD) card, or FlashCard. Furthermore, the memory 11 can include both internal and external storage units of the electronic device 1. The memory 11 can be used not only to store application software and various types of data installed on the electronic device 1, such as the code for preparing cobalt-doped nano-zinc sulfide oxygen reduction electrocatalyst materials, but also to temporarily store data that has been output or will be output.

[0160] In some embodiments, the processor 10 may be composed of integrated circuits, such as a single packaged integrated circuit or multiple integrated circuits with the same or different functions, including combinations of one or more central processing units (CPUs), microprocessors, digital processing chips, graphics processors, and various control chips. The processor 10 is the control unit of the electronic device, connecting various components of the entire electronic device through various interfaces and lines. It executes programs or modules stored in the memory 11 (e.g., a program for preparing oxygen reduction electrocatalyst materials of cobalt-doped zinc sulfide nanoparticles) and calls data stored in the memory 11 to perform various functions of the electronic device 1 and process data.

[0161] The bus can be a Peripheral Component Interconnect (PCI) bus or an Extended Industry Standard Architecture (EISA) bus, etc. This bus can be divided into an address bus, a data bus, a control bus, etc. The bus is configured to enable communication between the memory 11 and at least one processor 10, etc.

[0162] Figure 10 Only electronic devices with components are shown; those skilled in the art will understand that... Figure 10 The structure shown does not constitute a limitation on the electronic device 1, and may include fewer or more components than shown, or combine certain components, or have different component arrangements.

[0163] For example, although not shown, the electronic device 1 may also include a power supply (such as a battery) to power various components. Preferably, the power supply can be logically connected to the at least one processor 10 through a power management device, thereby enabling functions such as charging management, discharging management, and power consumption management. The power supply may also include one or more DC or AC power supplies, recharging devices, power fault detection circuits, power converters or inverters, power status indicators, and other arbitrary components. The electronic device 1 may also include various sensors, Bluetooth modules, Wi-Fi modules, etc., which will not be described in detail here.

[0164] Furthermore, the electronic device 1 may also include a network interface. Optionally, the network interface may include a wired interface and / or a wireless interface (such as a Wi-Fi interface, a Bluetooth interface, etc.), which is typically used to establish communication connections between the electronic device 1 and other electronic devices.

[0165] Optionally, the electronic device 1 may further include a user interface, which may be a display, an input unit (such as a keyboard), or a standard wired or wireless interface. Optionally, in some embodiments, the display may be an LED display, a liquid crystal display, a touch-sensitive liquid crystal display, or an OLED (Organic Light-Emitting Diode) touchscreen. The display may also be appropriately referred to as a screen or display unit, used to display information processed in the electronic device 1 and to display a visual user interface.

[0166] It should be understood that the embodiments described are for illustrative purposes only and are not limited to this structure in the scope of the patent application.

[0167] The preparation program for the oxygen reduction electrocatalyst material of cobalt-doped zinc sulfide nanoparticles stored in the memory 11 of the electronic device 1 is a combination of multiple instructions, which, when run in the processor 10, can achieve the following:

[0168] Aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution were mixed, ground, and dried in a grinding dish to obtain an electrocatalytic precursor.

[0169] The electrocatalytic precursor was ground and placed in a ceramic boat and then placed in the center of a tube furnace to obtain the precursor to be pyrolyzed.

[0170] According to the preset optimal pyrolysis temperature, optimal pyrolysis time and heating gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain the pyrolysis product.

[0171] The pyrolysis product is etched with hydrochloric acid of a preset concentration to obtain a pyrolysis etched product. The pyrolysis etched product is then washed and filtered with deionized water to obtain an initial oxygen reduction electrocatalytic material.

[0172] The initial electrocatalytic product was dried at a preset drying temperature and time to obtain the target oxygen reduction electrocatalytic material.

[0173] Specifically, the processor 10's implementation method for the above instructions can be found in [reference needed]. Figure 1 The descriptions of the relevant steps in the corresponding embodiments are not repeated here.

[0174] Furthermore, if the modules / units integrated in the electronic device 1 are implemented as software functional units and sold or used as independent products, they can be stored in a computer-readable storage medium. The computer-readable storage medium can be volatile or non-volatile. For example, the computer-readable medium may include: any entity or device capable of carrying the computer program code, a recording medium, a USB flash drive, a portable hard drive, a magnetic disk, an optical disk, a computer memory, or a read-only memory (ROM).

[0175] The present invention also provides a computer-readable storage medium storing a computer program, which, when executed by a processor of an electronic device, can perform the following:

[0176] Aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution were mixed, ground, and dried in a grinding dish to obtain an electrocatalytic precursor.

[0177] The electrocatalytic precursor was ground and placed in a ceramic boat and then placed in the center of a tube furnace to obtain the precursor to be pyrolyzed.

[0178] According to the preset optimal pyrolysis temperature, optimal pyrolysis time and heating gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain the pyrolysis product.

[0179] The pyrolysis product is etched with hydrochloric acid of a preset concentration to obtain a pyrolysis etched product. The pyrolysis etched product is then washed and filtered with deionized water to obtain an initial oxygen reduction electrocatalytic material.

[0180] The initial electrocatalytic product was dried at a preset drying temperature and time to obtain the target oxygen reduction electrocatalytic material.

[0181] The modules described as separate components may or may not be physically separate. The components shown as modules may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the modules can be selected to achieve the purpose of this embodiment according to actual needs.

[0182] Furthermore, the functional modules in the various embodiments of the present invention can be integrated into one processing unit, or each unit can exist physically separately, or two or more units can be integrated into one unit. The integrated unit can be implemented in hardware or in the form of hardware plus software functional modules.

[0183] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention.

[0184] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a cobalt-doped zinc sulfide nano-oxidation electrocatalytic material, characterized in that, The method includes: Aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution were mixed, ground, and dried in a grinding dish to obtain an electrocatalytic precursor. The electrocatalytic precursor was ground and placed in a ceramic boat and then placed in the center of a tube furnace to obtain the precursor to be pyrolyzed. According to the preset optimal pyrolysis temperature, optimal pyrolysis time and heating gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain the pyrolysis product. Before obtaining the pyrolysis products by pyrolyzing the precursor to be pyrolyzed using the tubular furnace according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the method further includes: Based on the preset set of test pyrolysis temperatures or test pyrolysis times, obtain the pyrolysis products at different test pyrolysis temperatures or different test pyrolysis times to obtain the temperature test pyrolysis product set or the time test pyrolysis product set. The pyrolysis products to be tested at temperature or the pyrolysis products to be tested at time are extracted sequentially from the set of pyrolysis products tested at temperature or time. The pyrolysis product to be tested at temperature or the pyrolysis product to be tested at time are etched using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or the etched product to be tested at time. The etching product to be tested for temperature or time is washed and filtered with deionized water to obtain the washing product to be tested for temperature or time. The temperature-tested washing product or time-tested washing product is dried at a preset drying temperature and drying time to obtain the temperature-tested target product or time-tested target product. The pre-constructed glassy carbon electrode is modified using the target product for temperature testing or the target product for time testing to obtain a rotating disk electrode for temperature testing or a rotating disk electrode for time testing. The rotating disk electrode for temperature testing or the rotating disk electrode for time testing is then used as the working electrode for temperature testing or the working electrode for time testing. Obtain the counter electrode and reference electrode, and construct a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, counter electrode and reference electrode; The temperature test half-wave potential or the time test half-wave potential of the target product to be tested are obtained according to the temperature test three-electrode system or the time test three-electrode system. The half-wave potentials of all pyrolysis products at different temperatures in the temperature test pyrolysis product set are summarized to obtain the temperature test half-wave potential set. Extract the target temperature pyrolysis product corresponding to the maximum temperature test half-wave potential from the temperature test half-wave potential set. Extract the test pyrolysis temperature of the product to be pyrolyzed at the target temperature, and take the test pyrolysis temperature of the product to be pyrolyzed at the target temperature as the optimal pyrolysis temperature. The half-wave potentials of all time-tested pyrolysis products in the time-tested pyrolysis product set are summarized to obtain the time-tested half-wave potential set. Extract the target time pyrolysis product corresponding to the maximum time test half-wave potential from the set of time test half-wave potentials; Extract the test pyrolysis time of the product to be pyrolyzed at the target time, and take the test pyrolysis time of the product to be pyrolyzed at the target time as the optimal pyrolysis time. The pyrolysis product is etched with hydrochloric acid of a preset concentration to obtain a pyrolysis etched product. The pyrolysis etched product is then washed and filtered with deionized water to obtain an initial oxygen reduction electrocatalytic material. The initial oxygen reduction electrocatalytic material was dried at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material.

2. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 1, characterized in that, The process involves mixing and grinding aminothiazole, anhydrous zinc acetate, and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish, followed by drying to obtain an electrocatalytic precursor, comprising: A predetermined mass of aminothiazole, anhydrous zinc acetate, and a predetermined volume of cobalt nitrate hexahydrate with a fixed concentration were placed in a grinding dish to obtain electrocatalytic raw materials. The electrocatalytic raw materials are mixed, ground, and dried in the grinding dish to obtain the electrocatalytic precursor.

3. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 1, characterized in that, The process involves pyrolyzing the precursor to be pyrolyzed using a tubular furnace according to a preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient to obtain pyrolysis products, including: According to the heating gradient, the precursor to be pyrolyzed is heated using the tubular furnace to obtain a heating tubular furnace; Monitor the center temperature of the heating tube furnace; Determine whether the center temperature of the heating tube furnace has reached the optimal pyrolysis temperature; If the center temperature of the heating tube furnace does not reach the optimal pyrolysis temperature, then return to the above steps of heating the precursor to be pyrolyzed using the tube furnace according to the heating gradient. If the center temperature of the heating tube furnace reaches the optimal pyrolysis temperature, the heating tube furnace is kept at the optimal pyrolysis temperature and optimal pyrolysis time to obtain pyrolysis products.

4. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 3, characterized in that, The step of obtaining the temperature test half-wave potential or the time test half-wave potential of the target product under test based on the temperature test three-electrode system or the time test three-electrode system includes: Linear sweep voltammetry is performed on the temperature testing three-electrode system or the time testing three-electrode system using the temperature testing working electrode or the time testing working electrode to obtain the temperature testing oxygen reduction polarization curve or the time testing oxygen reduction polarization curve. Extract the temperature test half-wave potential or the time test half-wave potential of the target product to be tested from the temperature test oxygen reduction polarization curve or the time test oxygen reduction polarization curve.

5. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 1, characterized in that, The process of etching the pyrolysis product to be tested at temperature or time using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or time includes: Extract a predetermined mass of the pyrolysis product to be tested at the specified temperature or time from the pyrolysis product to be tested at the specified temperature; The predetermined mass of the temperature-tested pyrolysis product or the time-tested pyrolysis product is placed in hydrochloric acid of a preset concentration and etched for a preset etching time to obtain the temperature-tested etched product or the time-tested etched product.

6. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 1, characterized in that, The process of obtaining the counter electrode and reference electrode, and constructing a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, the counter electrode, and the reference electrode, includes: The pre-constructed graphite rod was used as the counter electrode, and the pre-constructed Ag / AgCl electrode was used as the reference electrode. The temperature testing three-electrode system is constructed based on the counter electrode, reference electrode, temperature testing working electrode, and pre-prepared test solution. The time-testing three-electrode system is constructed based on the counter electrode, reference electrode, time-testing working electrode, and test solution.

7. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 5, characterized in that, The step of performing linear sweep voltammetry on the temperature-testing three-electrode system or the time-testing three-electrode system using the temperature-testing working electrode or the time-testing working electrode to obtain the temperature-tested oxygen reduction polarization curve or the time-tested oxygen reduction polarization curve includes: A preset test sweep speed is applied to the temperature test working electrode or the time test working electrode, and the electrolytic current of the temperature test working electrode or the time test working electrode is recorded. Based on the test scan rate and electrolysis current, plot the oxygen reduction polarization curve for temperature test or the oxygen reduction polarization curve for time test.

8. The method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalytic material as described in claim 1, characterized in that, After drying the initial oxygen reduction electrocatalytic material at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material, the method further includes: The oxygen reduction electrocatalytic performance curves of the target oxygen reduction electrocatalytic material and the oxygen reduction catalytic performance curves of the commercial platinum-carbon material are obtained according to the preset comparison time. The oxygen reduction electrocatalytic performance curves of the target oxygen reduction electrocatalytic material and the commercial platinum-carbon material were plotted on the same oxygen reduction catalytic performance-time coordinate system to obtain a comparison chart of the oxygen reduction electrocatalytic performance of the target oxygen reduction electrocatalytic material and the commercial platinum-carbon material.

9. An apparatus for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material based on the method for preparing cobalt-doped zinc sulfide nano-oxygen reduction electrocatalyst material according to any one of claims 1 to 8, characterized in that, The device includes: The electrocatalytic precursor preparation module is used to mix and grind aminothiazole, anhydrous zinc acetate and a pre-concentrated cobalt nitrate hexahydrate solution in a grinding dish and then dry them to obtain the electrocatalytic precursor. The pyrolysis module is used to grind the electrocatalytic precursor, place it in a ceramic boat, and put it in the center of a tube furnace to obtain the precursor to be pyrolyzed; according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the tube furnace is used to pyrolyze the precursor to be pyrolyzed to obtain the pyrolysis product. Before obtaining the pyrolysis products by pyrolyzing the precursor to be pyrolyzed using the tubular furnace according to the preset optimal pyrolysis temperature, optimal pyrolysis time, and temperature gradient, the method further includes: Based on the preset set of test pyrolysis temperatures or test pyrolysis times, obtain the pyrolysis products at different test pyrolysis temperatures or different test pyrolysis times to obtain the temperature test pyrolysis product set or the time test pyrolysis product set. The pyrolysis products to be tested at temperature or the pyrolysis products to be tested at time are extracted sequentially from the set of pyrolysis products tested at temperature or time. The pyrolysis product to be tested at temperature or the pyrolysis product to be tested at time are etched using hydrochloric acid of a preset concentration to obtain the etched product to be tested at temperature or the etched product to be tested at time. The etching product to be tested for temperature or time is washed and filtered with deionized water to obtain the washing product to be tested for temperature or time. The temperature-tested washing product or time-tested washing product is dried at a preset drying temperature and drying time to obtain the temperature-tested target product or time-tested target product. The pre-constructed glassy carbon electrode is modified using the target product for temperature testing or the target product for time testing to obtain a rotating disk electrode for temperature testing or a rotating disk electrode for time testing. The rotating disk electrode for temperature testing or the rotating disk electrode for time testing is then used as the working electrode for temperature testing or the working electrode for time testing. Obtain the counter electrode and reference electrode, and construct a temperature testing three-electrode system or a time testing three-electrode system based on the temperature testing working electrode or time testing working electrode, counter electrode and reference electrode; The temperature test half-wave potential or the time test half-wave potential of the target product to be tested are obtained according to the temperature test three-electrode system or the time test three-electrode system. The half-wave potentials of all pyrolysis products at different temperatures in the temperature test pyrolysis product set are summarized to obtain the temperature test half-wave potential set. Extract the target temperature pyrolysis product corresponding to the maximum temperature test half-wave potential from the temperature test half-wave potential set. Extract the test pyrolysis temperature of the product to be pyrolyzed at the target temperature, and take the test pyrolysis temperature of the product to be pyrolyzed at the target temperature as the optimal pyrolysis temperature. The half-wave potentials of all time-tested pyrolysis products in the time-tested pyrolysis product set are summarized to obtain the time-tested half-wave potential set. Extract the target time pyrolysis product corresponding to the maximum time test half-wave potential from the set of time test half-wave potentials; Extract the test pyrolysis time of the product to be pyrolyzed at the target time, and take the test pyrolysis time of the product to be pyrolyzed at the target time as the optimal pyrolysis time. The etching and washing module is used to etch the pyrolysis product with hydrochloric acid of a preset concentration to obtain pyrolysis etched product, and to wash and filter the pyrolysis etched product with deionized water to obtain the initial oxygen reduction electrocatalytic material. The drying module is used to dry the initial oxygen reduction electrocatalytic material at a preset drying temperature and drying time to obtain the target oxygen reduction electrocatalytic material.

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