Fe2(moo4)3 / CoMoo4 double-shell hollow nanospheres hetero-catalyst and preparation method and application thereof
The synthesis of Fe2(MoO4)3/CoMoO4 double-shell hollow nanosphere catalysts by a solvothermal combined with high-temperature solid-state method solves the resource and stability problems of precious metal catalysts, achieves high-efficiency water electrolysis for hydrogen production, and promotes the industrialization of non-precious metal catalysts.
Patent Information
- Application Number
- CN202611402446.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-09-10
- Publication Date
- 2026-11-06
AI Technical Summary
In the existing technology, the oxygen evolution reaction (OER) in the process of hydrogen production by water electrolysis of noble metal oxide catalysts suffers from the problems of scarce resources, high cost and poor stability. In addition, the activity improvement space of existing non-noble metal molybdate catalysts is limited, and the application of heterostructure and double-shell hollow structure in composite metal molybdate catalysts is not yet mature, resulting in performance bottlenecks under actual working conditions.
Fe2(MoO4)3/CoMoO4 double-shell hollow nanosphere catalysts were synthesized by a solvothermal method combined with high-temperature solid-phase oxidation. By constructing heterogeneous interfaces and double-shell structures, the electronic state and active sites of the catalysts were optimized, thereby improving catalytic activity and stability.
The synthesized Fe2(MoO4)3/CoMoO4 catalyst exhibits excellent activity and stability in the OER process, with an overpotential lower than that of the noble metal IrO2/C catalyst. It can operate stably for a long time in water electrolysis to produce hydrogen and has the potential for industrial application.
Smart Images

Figure CN123043572A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of water electrolysis for hydrogen production technology, and particularly relates to a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst, its preparation method and application. Background Technology
[0002] Electrolysis of water to produce hydrogen directly converts electrical energy into chemical energy, boasting advantages such as simple process, high product purity, and environmental friendliness, making it an effective way to address the energy crisis and environmental pollution. The oxygen evolution reaction (OER), as the core half-reaction in water electrolysis for hydrogen production, is also widely involved in metal-air batteries and various energy conversion and storage devices. However, the OER process involves four-electron transfer, resulting in relatively sluggish reaction kinetics, which has become a key bottleneck restricting the overall energy efficiency improvement of these devices.
[0003] Currently, noble metal oxides (such as IrO2 and RuO2) are widely recognized as OER electrocatalysts with excellent overall performance. However, their large-scale application is limited by multiple factors: the scarcity of noble metal resources, high material costs, and shortcomings in durability and resistance to poisoning under actual operating conditions. Therefore, developing non-noble metal-based alternative materials that combine high activity and high stability is of great significance for promoting the industrialization of water electrolysis hydrogen production technology.
[0004] Transition metal molybdates have attracted widespread attention in the field of electrocatalysis due to their rich valence states of metal ions, outstanding redox properties, and the electronic synergistic effect between bimetallic ions. Studies have shown that Mo can effectively lower the energy barrier of the oxidation transformation of 3d metals such as Fe, Co, and Ni, inducing the generation of highly oxidized active species, thereby enhancing OER catalytic activity. Currently, research on single-component molybdates (such as ferric molybdate, cobalt molybdate, and nickel molybdate) as electrode materials has been reported, but compared with noble metal benchmark catalysts, their oxygen evolution overpotential is still relatively high, limiting the potential for activity improvement.
[0005] Theoretical studies have shown that catalytic reaction kinetics are closely related to the electronic state of the catalyst surface, and high-performance OER catalysts need to maintain a suitable adsorption energy with reaction intermediates. Constructing heterojunction structures can optimize the interfacial electronic structure, accelerate charge transfer and reactant adsorption; at the same time, constructing double-shell hollow structures can increase the number of exposed active sites, shorten ion diffusion paths, and improve charge-mass transport efficiency. However, in the current technology, the synergistic application of heterostructure construction and double-shell hollow structures in composite metal molybdate catalysts is still lacking. Specifically, currently reported multi-shell molybdate-based OER catalysts are mostly limited to single components (such as Fe2(MoO4)3, CoMoO4, NiMoO4, etc.), and their synthesis processes generally rely on template methods, which are cumbersome and not conducive to large-scale preparation. As for the synthesis of Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere catalysts with heterojunction interfaces by direct calcination, there are no clear technical inspirations or preparation examples in the current technology.
[0006] Furthermore, existing literature reports that the OER performance of currently developed transition metal molybdate-based catalysts in practical applications such as water electrolysis is generally lower than that of noble metal-based catalysts, leading to performance bottlenecks under real-world conditions. Simultaneously, systematic experimental research and in-depth theoretical analysis are still lacking regarding the structure-activity relationship between the microstructural characteristics of these catalysts (especially double-shell hollow heterocomposite structures) and their water electrolysis OER performance, as well as the corresponding catalytic reaction mechanisms. This restricts further optimization and rational design of catalyst performance. Summary of the Invention
[0007] To address the aforementioned technical problems, this invention proposes a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst, its preparation method, and its applications. This invention synthesizes Fe2(MoO4)3 / CoMoO4 double-shell hollow nanospheres for use as an OER catalyst in water electrolysis using a simple solvothermal combined with high-temperature solid-phase oxidation strategy. Benefiting from its double-shell morphology and the establishment of a heterogeneous interface, it exhibits excellent OER activity, even surpassing that of noble metal IrO2 / C catalysts. Furthermore, it can maintain its activity well for 360 hours without significant degradation. Therefore, the synthesized Fe2(MoO4)3 / CoMoO4 catalyst has potential application prospects in the field of hydrogen production through water electrolysis.
[0008] To achieve the above objectives, the present invention provides the following technical solution: A method for preparing a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst includes the following steps: Iron and cobalt salts were dissolved in a mixed solvent of glycerol and isopropanol and stirred until completely dissolved. Then, a molybdenum source was added and stirring was continued to obtain a mixed solution. The mixed solution was transferred to a reaction vessel for a solvothermal reaction. After the reaction was completed, the solution was cooled, washed, and dried to obtain the Fe-Co-Mo precursor. The Fe-Co-Mo precursor was calcined in air to obtain a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst.
[0009] Furthermore, the iron salt is ferric nitrate nonahydrate, the cobalt salt is cobalt nitrate hexahydrate, and the molybdenum source is molybdenum acetylacetonate; the molar ratio of the iron salt to the cobalt salt is 1:1, and the molar ratio of the total amount of the iron salt and cobalt salt to the molybdenum source is 1:1.
[0010] Furthermore, the temperature of the solvothermal reaction is 180°C, and the reaction time is 12 to 48 hours (e.g., 24 hours).
[0011] Furthermore, the calcination temperature is 400–550°C (e.g., 500°C), and the calcination time is 4–12 hours (e.g., 4 hours).
[0012] Furthermore, the drying is vacuum drying, the drying temperature is 80°C, and the drying time is 12 to 48 hours (e.g., 12 hours).
[0013] The present invention also provides a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst, which is prepared by the above preparation method.
[0014] Furthermore, the Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterogeneous catalyst exhibits a double-shell hollow nanosphere morphology and contains a two-phase heterojunction structure of Fe2(MoO4)3 and CoMoO4.
[0015] Furthermore, the Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst has a particle size of 400 nm.
[0016] This invention also provides the application of Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterogeneous catalyst in the oxygen evolution reaction of water electrolysis.
[0017] Furthermore, the Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst is subjected to a current density of 10 mA·cm⁻¹. -2 and 100mA·cm -2 The oxygen evolution overpotentials were 138 mV and 235 mV, respectively.
[0018] Compared with the prior art, the present invention has the following advantages and technical effects: This invention utilizes a solvothermal method combined with a high-temperature solid-state method to achieve the controllable synthesis of Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere catalysts, and systematically studies their OER catalytic activity and stability. The prepared Fe2(MoO4)3 / CoMoO4 catalyst exhibits stable OER catalytic activity at 10 mA·cm⁻¹. -2 and 100mA·cm -2 The overpotentials at the current densities were 138 mV and 235 mV, respectively, far lower than those of CoMoO4 (305 mV and 511 mV) and Fe2(MoO4)3 (372 mV and 557 mV) samples alone, and even superior to commercial noble metal IrO2 / C (167 mV, 239 mV) catalysts. Moreover, at 100 mA·cm⁻¹, the overpotentials were... -2 The catalyst can operate stably for 360 hours without significant activity decay at a given current density. The Fe2(MoO4)3 / CoMoO4 catalyst synthesized in this invention has great application potential in the field of water electrolysis for hydrogen production. Attached Figure Description
[0019] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings: Figure 1 XRD patterns of Fe2(MoO4)3 / CoMoO4, Fe2(MoO4)3, and CoMoO4; Figure 2 XRD patterns of Fe2(MoO4)3 / CoMoO4 samples synthesized under different conditions; Figure 3 FE-SEM images of Fe2(MoO4)3 / CoMoO4 (a), Fe2(MoO4)3 (b) and CoMoO4 (c); Figure 4 The TEM (a, b), HAADF-STEM (c), and corresponding elemental mapping (dh) diagrams of Fe2(MoO4)3 / CoMoO4 at different multiples are shown. Figure 5 OER polarization curves (a) for Fe2(MoO4)3 / CoMoO4, Fe2(MoO4)3, CoMoO4 and IrO2 / C catalysts at 10 and 100 mA·cm -2 The overpotential corresponding to the current density (b); Figure 6 The OER stability test curves for the Fe2(MoO4)3 / CoMoO4 catalyst are shown. Detailed Implementation
[0020] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.
[0021] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.
[0022] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.
[0023] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be apparent to those skilled in the art. This specification and embodiments are merely exemplary.
[0024] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.
[0025] The Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere catalyst synthesized in this invention is prepared by a simple solvothermal method combined with a high-temperature solid-state method, which is superior to the traditional template method. Furthermore, it exhibits excellent OER activity and stability, surpassing noble metal IrO2 / C catalysts, and shows potential application prospects in the industrial hydrogen production field of water electrolysis. It provides theoretical guidance and technical support for the design, synthesis, and practical application of other non-noble metal water electrolysis catalysts.
[0026] Unless otherwise specified, "room temperature" in this invention refers to 25±2℃.
[0027] All raw materials used in this invention were purchased from the market.
[0028] The technical solution of the present invention will be further illustrated by the following embodiments.
[0029] Example 1 A method for preparing a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst includes the following steps: 0.125 mmol of ferric nitrate nonahydrate (Fe(NO3)3•9H2O) and 0.125 mmol of cobalt nitrate hexahydrate were dissolved in a mixed solvent of 8 mL glycerol and 48 mL isopropanol. The mixture was stirred for 30 minutes until completely dissolved. Then, 0.25 mmol of molybdenum acetylacetonate was added to the above solution, and stirring was continued at room temperature for 1 hour to obtain a mixed solution. The mixed solution was transferred to a polytetrafluoroethylene reactor and reacted at 180 °C for 24 hours. After naturally cooling to room temperature, it was washed several times with deionized water and ethanol, and finally vacuum dried at 80 °C for 12 hours to obtain the Fe-Co-Mo precursor. The Fe-Co-Mo precursor was placed in a tube furnace and calcined in air at 500 °C for 4 hours to obtain Fe2(MoO4)3 / CoMoO4 double-shell hollow heterojunction nanospheres.
[0030] Comparative Example 1 A method for preparing Fe2(MoO4)3 nanosphere catalyst includes the following steps: 0.25 mmol of ferric nitrate nonahydrate (Fe(NO3)3•9H2O) was dissolved in a mixed solvent of 8 mL glycerol and 48 mL isopropanol. The mixture was stirred for 30 minutes until completely dissolved. Then, 0.25 mmol of molybdenum acetylacetonate was added to the above solution, and stirring was continued at room temperature for 1 hour to obtain a mixed solution. The mixed solution was transferred to a polytetrafluoroethylene reactor and reacted at 180 °C for 24 hours. After naturally cooling to room temperature, it was washed several times with deionized water and ethanol, and finally vacuum dried at 80 °C for 12 hours to obtain the Fe-Mo precursor. The Fe-Mo precursor was placed in a tube furnace and calcined in air at 500 °C for 4 hours to obtain Fe2(MoO4)3 nanospheres.
[0031] Comparative Example 2 A method for preparing a CoMoO4 nanosphere catalyst includes the following steps: 0.25 mmol of cobalt nitrate hexahydrate was dissolved in a mixed solvent of 8 mL glycerol and 48 mL isopropanol, and the mixture was stirred for 30 minutes until completely dissolved. Then, 0.25 mmol of molybdenum acetylacetonate was added to the above solution, and stirring was continued at room temperature for 1 hour to obtain a mixed solution. The mixed solution was transferred to a polytetrafluoroethylene reactor and reacted at 180 °C for 24 hours. After naturally cooling to room temperature, it was washed several times with deionized water and ethanol, and finally vacuum dried at 80 °C for 12 hours to obtain the Co-Mo precursor. The Co-Mo precursor was placed in a tube furnace and calcined in air at 500 °C for 4 hours to obtain CoMoO4 nanospheres.
[0032] Comparative Example 3 0.25 mmol of ferric nitrate nonahydrate (Fe(NO3)3•9H2O) and 0.125 mmol of cobalt nitrate hexahydrate were dissolved in a mixed solvent of 8 mL of glycerol and 48 mL of isopropanol. The mixture was stirred for 30 minutes until completely dissolved. Then, 0.25 mmol of molybdenum acetylacetonate was added to the above solution, and stirring was continued at room temperature for 1 hour to obtain a mixed solution. The mixed solution was transferred to a polytetrafluoroethylene reactor and reacted at 180 °C for 24 hours. After naturally cooling to room temperature, it was washed several times with deionized water and ethanol, and finally vacuum dried at 80 °C for 12 hours to obtain the Fe-Co-Mo- precursor. The Fe-Co-Mo- precursor was placed in a tube furnace and calcined in air at 500 °C for 4 hours to obtain the Fe2(MoO4)3 / CoMoO4 heterojunction.
[0033] Comparative Example 4 0.125 mmol of ferric nitrate nonahydrate (Fe(NO3)3•9H2O) and 0.125 mmol of cobalt nitrate hexahydrate were dissolved in a mixed solvent of 8 mL of glycerol and 48 mL of isopropanol. The mixture was stirred for 30 minutes until completely dissolved. Then, 0.25 mmol of molybdenum acetylacetonate was added to the above solution, and stirring was continued at room temperature for 1 hour to obtain a mixed solution. The mixed solution was transferred to a polytetrafluoroethylene reactor and reacted at 180 °C for 24 hours. After naturally cooling to room temperature, it was washed several times with deionized water and ethanol, and finally vacuum dried at 80 °C for 12 hours to obtain the Fe-Co-Mo- precursor. The Fe-Co-Mo- precursor was placed in a tube furnace and calcined in air at 400 °C for 4 hours to obtain the Fe2(MoO4)3 / CoMoO4 heterojunction.
[0034] Comparative Example 5 0.125 mmol of ferric nitrate nonahydrate (Fe(NO3)3•9H2O) and 0.125 mmol of cobalt nitrate hexahydrate were dissolved in a mixed solvent of 8 mL of glycerol and 48 mL of isopropanol. The mixture was stirred for 30 minutes until completely dissolved. Then, 0.25 mmol of ammonium molybdate was added to the above solution, and stirring was continued for 1 hour at room temperature to obtain a mixed solution. The mixed solution was transferred to a polytetrafluoroethylene reactor and reacted at 180 °C for 24 hours. After naturally cooling to room temperature, it was washed several times with deionized water and ethanol, and finally vacuum dried at 80 °C for 12 hours to obtain the Fe-Co-Mo- precursor. The Fe-Co-Mo- precursor was placed in a tube furnace and calcined in air at 500 °C for 4 hours to obtain the Fe2(MoO4)3 / CoMoO4 heterojunction.
[0035] Performance testing: 1. The three synthesized samples were characterized by X-ray powder diffraction (XRD).
[0036] Figure 1 The XRD patterns of Fe2(MoO4)3 / CoMoO4, Fe2(MoO4)3, and CoMoO4 are shown. Abundant diffraction peaks are observed. Comparison reveals that the diffraction peaks of the synthesized Fe2(MoO4)3 and CoMoO4 samples are completely consistent with their corresponding standard cards, suggesting the successful synthesis of Fe2(MoO4)3 and CoMoO4 catalysts. Furthermore, the synthesized Fe2(MoO4)3 / CoMoO4 sample contains diffraction peaks from both Fe2(MoO4)3 and CoMoO4, indicating the successful preparation of the Fe2(MoO4)3 / CoMoO4 heterojunction catalyst.
[0037] 2. The Fe2(MoO4)3 / CoMoO4 samples synthesized under different conditions were characterized by X-ray powder diffraction (XRD).
[0038] Figure 2 The XRD patterns of Fe2(MoO4)3 / CoMoO4 synthesized under different conditions are shown. It can be observed that under the conditions of a Fe salt to Co salt molar ratio of 2:1, a calcination temperature of 400℃, and the conversion of molybdenum acetylacetone to ammonium molybdate, the diffraction peaks of the corresponding samples are completely consistent with the standard cards of Fe2(MoO4)3 and CoMoO4 alone. It can be inferred that under the above synthesis conditions, Fe2(MoO4)3 / CoMoO4 heterojunction catalysts can be successfully prepared.
[0039] 3. The morphology of the three synthesized samples was characterized using field emission scanning electron microscopy (FE-SEM).
[0040] Figure 3Figures show the FE-SEM images of Fe2(MoO4)3 / CoMoO4 (a), Fe2(MoO4)3 (b), and CoMoO4 (c). Figure a shows that the synthesized Fe2(MoO4)3 / CoMoO4 exhibits a uniform nanosphere morphology with a smooth surface and a size of approximately 400 nm. The presence of a few broken spheres suggests a core-shell structure. Furthermore, Figures b and c show that both Fe2(MoO4)3 and CoMoO4 have uniform nanosphere morphologies, but their surfaces are rough, with some nanoparticles coating the nanosphere surface.
[0041] 4. The internal structure of the synthesized Fe2(MoO4)3 / CoMoO4 sample was further observed using transmission electron microscopy (TEM).
[0042] Figure 4 Figures a and b show TEM (a, b), HAADF-STEM (c), and corresponding elemental mapping (dh) images of Fe2(MoO4)3 / CoMoO4 at different magnifications. As shown in Figures a and b, Fe2(MoO4)3 / CoMoO4 exhibits a double-shell hollow nanosphere morphology. Furthermore, the high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) image further reveals the double-shell structure of Fe2(MoO4)3 / CoMoO4 (Figure c). Simultaneously, the elemental mapping shows that Fe, Co, Mo, and O elements are uniformly distributed throughout the double-shell hollow nanosphere region (Figures d-h).
[0043] 5. Electrocatalytic oxygen evolution reaction (OER) performance tests were conducted on Fe2(MoO4)3 / CoMoO4, Fe2(MoO4)3, CoMoO4 samples and commercial IrO2 / C in 1M KOH solution using a standard three-electrode system.
[0044] Figure 5 OER polarization curves (a) and (b) at 10 mA·cm⁻¹ for Fe₂(MoO₄)₃ / CoMoO₄, Fe₂(MoO₄)₃, CoMoO₄ and IrO₂ / C catalysts. -2 and 100mA·cm -2 The overpotential corresponding to the current density (b) is shown in Figures a and b, at 10 mA·cm⁻¹. -2 100mA·cm -2At current densities of 138 mV and 235 mV, the overpotentials of Fe2(MoO4)3 / CoMoO4 were much lower than those of CoMoO4 (305 mV and 511 mV) and Fe2(MoO4)3 (372 mV and 557 mV) compared to the samples alone, and even better than those of commercial noble metal IrO2 / C (167 mV and 239 mV), indicating that the Fe2(MoO4)3 / CoMoO4 catalyst has excellent performance.
[0045] 6. At 100mA·cm -2 The OER stability of the Fe2(MoO4)3 / CoMoO4 catalyst was tested at a current density of [value missing].
[0046] Figure 6 The OER stability test curves for the Fe2(MoO4)3 / CoMoO4 catalyst are provided by [the relevant data]. Figure 6 The voltage-time curves show that as the catalytic reaction proceeds, the voltage of the Fe2(MoO4)3 / CoMoO4 catalyst remains stable at around 1.47V over the long 360-hour test period without significant fluctuations, indicating its excellent catalytic stability.
[0047] In summary, the Fe2(MoO4)3 / CoMoO4 synthesized in this invention not only exhibits superior OER performance compared to noble metal IrO2 / C catalysts, but also demonstrates excellent OER catalytic stability. This indicates that the Fe2(MoO4)3 / CoMoO4 catalyst has potential application prospects in the field of water electrolysis for hydrogen production.
[0048] The above are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.
Claims
1. A method for preparing a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst, characterized in that, Includes the following steps: Iron and cobalt salts were dissolved in a mixed solvent of glycerol and isopropanol and stirred until completely dissolved. Then, a molybdenum source was added and stirring was continued to obtain a mixed solution. The mixed solution was transferred to a reaction vessel for a solvothermal reaction. After the reaction was completed, the solution was cooled, washed, and dried to obtain the Fe-Co-Mo precursor. The Fe-Co-Mo precursor was calcined in air to obtain a Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst.
2. The preparation method according to claim 1, characterized in that, The iron salt is ferric nitrate nonahydrate, the cobalt salt is cobalt nitrate hexahydrate, and the molybdenum source is molybdenum acetylacetonate; the molar ratio of the iron salt to the cobalt salt is 1:1, and the molar ratio of the total amount of the iron salt and cobalt salt to the molybdenum source is 1:
1.
3. The preparation method according to claim 1, characterized in that, The solvothermal reaction is carried out at a temperature of 180°C for a reaction time of 12–48 hours.
4. The preparation method according to claim 1, characterized in that, The calcination temperature is 400–550°C, and the calcination time is 4–12 hours.
5. The preparation method according to claim 1, characterized in that, The drying process is vacuum drying, with a drying temperature of 80°C and a drying time of 12–48 hours.
6. A Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterogeneous catalyst, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 5.
7. The Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst according to claim 6, characterized in that, It exhibits a double-shell hollow nanosphere morphology and contains a two-phase heterojunction structure of Fe2(MoO4)3 and CoMoO4.
8. The Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterocatalyst according to claim 6, characterized in that, The Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterogeneous catalyst has a particle size of 400 nm.
9. The application of the Fe2(MoO4)3 / CoMoO4 double-shell hollow nanosphere heterogeneous catalyst as described in any one of claims 6 to 8 in the oxygen evolution reaction of water electrolysis.
