Three Dimensional NiS-MoOx/CC Nanosheet Array for Efficient Electrocatalytic Oxygen Evolution Reaction

Three Dimensional NiS-MoOx/CC Nanosheet Array for Efficient Electrocatalytic Oxygen Evolution Reaction | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Three Dimensional NiS-MoOx/CC Nanosheet Array for Efficient Electrocatalytic Oxygen Evolution Reaction Weiwei Zhang, Haidong Yang, Hui Wang This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6326912/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract Developing highly efficient oxygen evolution reaction (OER) electrocatalysts remains critical for advancing large-scale water splitting. Self-supported electrodes, where catalysts are directly grown on conductive substrates, offer a promising strategy to enhance OER performance by improving structural stability and charge transfer. Herein, we fabricate a self-supported electrode via in situ growth of a MoS 2 precursor on carbon cloth (CC) using a facile hydrothermal method, followed by Ni incorporation to optimize catalytic activity. The optimized NiS-MoO x /CC-0.6 electrode exhibits outstanding OER performance with a low overpotential of 340 mV at a current density of 50 mA cm − 2 in alkaline media. This enhanced activity is attributed to the three-dimensional (3D) nanosheet array architecture, which exposes abundant active sites, facilitates electrolyte penetration, and ensures efficient electron transport. Our work provides insights into designing high-performance transition metal-based electrocatalysts for sustainable energy applications. 3D nanosheet array oxygen evolution reaction self-supported catalyst Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 1. Introduction Currently, the excessive consumption of fossil fuels and the associated environmental pollution has become one of the foremost global challenges. Among renewable energy sources, hydrogen has been utilized as a viable alternative fuel due to its environmental friendliness, high energy density and low losses. 1, 2 Currently, hydrogen is primarily produced through the steam-methane reforming process, which is both inefficient and responsible for significant carbon dioxide emissions. 3 Therefore, it is crucial to explore alternative methods for hydrogen production. As one of the most promising strategy, electrolytic water splitting involves two half-reactions: hydrogen evolution reaction (HER) and oxygen evolution reaction (OER). 4-6 The OER involves a complex four-electron transfer process with slow kinetics, requiring a high overpotential to drive the reaction, which presents a bottleneck in hydrogen production through electrolytic water splitting. 7, 8 In recent years, significance progress has been made in developing cost-efficient OER electrocatalysts. Transition metal-based catalysts with high activity toward the OER in alkaline media have been extensively studied, attributed to their unique intrinsic structures and physicochemical properties. 9, 10 For instance, transition metal sulfides, 11, 12 selenides, 13, 14 phosphide, 15-17 nitride, 18, 19 hydroxide, 20, 21 oxides, 22 and metal alloys 23, 24 have shown excellent OER activity under similar conditions, thereby promoting the water splitting efficiency. Transition metal sulfides have been demonstrated as promising OER catalyst due to their abundant active sites and high intrinsic activity. 25 For example, nickel sulfide has been proved as an active OER electrocatalyst in alkaline media, undergoing a transformation from Ni 2+ to Ni 3+ during the OER process, which produces disordered NiOOH as the active site for the catalytic reaction. 26 Additionally, structural regulation of the catalyst is crucial for the high electrocatalytic performance, which not only affects the morphology of catalysts but also accelerates the diffusion and adsorption of the reactant, thereby promoting the whole reaction rate. 27 Generally speaking, there are two effective methods for optimizing the OER performance of catalysts. The first approach involves preparing a composite material to create heterogeneous structure or multicomponent catalyst in which synergistic effect can be observed in enhancing both OER activity and stability. For instance, the NiS/Ni 2 P heterogeneous structure by Xiao et al. prepared demonstrates excellent OER performance due to its low charge transfer resistance, abundant active sites, and the synergistic effect between Ni 2 P and NiS. 28 Another viable method to improve the catalytic performance for OER is the fabrication of self-supported electrode through an in-situ process. Compared to powder electrode materials, self-supported materials exhibit a more ordered structure with fully exposed active sites, and simultaneously facilitate efficient mass and charge transfer during electrocatalysis. For example, Zhang et al. developed a self-supported WO 3 @RuO 2 nanowire on a titanium mesh, which exhibits enhanced OER kinetics due to its three-dimensional structure, leading to a lower interface resistance between active sites and the electrolyte. 29 Therefore, the preparation of electrocatalysts with self-supported structures presents a promising strategy for enhancing electrocatalytic OER performance. 30 Herein, the in situ growth of self-supported NiS-MoO x nanosheet array on carbon cloth (CC) was prepared through a hydrothermal process (denoted as NiS-MoO x /CC). Compared to power electrocatalysts bonded with polymer adhesives, the self-supported NiS-MoO x /CC exhibit enhanced stability and superior OER performance, effectively preventing the loss of active components and improving the conductivity of the catalysts. The NiS-MoO x /CC-0.6 catalysts exhibited a low overpotential of 340 mV at a current density of 50 mA cm -2 for the OER. The self-supported NiS-MoO x /CC electrode as an OER electrocatalyst exhibits excellent catalytic activity, which gives a promising candidate as OER electrocatalysts. 2. Experimental Section 2.1. Materials. Nickel nitrate hexahydrate (Ni(NO 3 ) 2 ·6H 2 O), ammonium fluoride (NH 4 F) and thiourea (CH 4 N 2 S) were purchased from Sinopharm Chemical Reagents Co., Ltd. Sodium molybdate dihydrate (Na 2 MoO 4 ·2H 2 O) was obtained from Shanghai Energy and Chemical Co., Ltd. Nitric acid (HNO 3 ) was obtained from Beijing Chemical Plant. Sulfuric acid (H 2 SO 4 ) was obtained from Chengdu Kelong Chemical Co., Ltd. Ammonium hydroxide (NH 4 OH) was obtained from Tianjin Kemiou Chemical Reagent Co., Ltd. Urea (CO(NH 2 ) 2 ) was obtained from Tianjin Dengfeng chemical reagent factory. Ethanol (C 2 H 6 O) was obtained from Lianlong Bohua Pharmaceutical Chemical Co., Ltd. All chemical reagents used without further purification., and all chemical reagents were used without further purification. 2.2. Synthesis of NiS-MoO x /CC. NiS-MoO x /CC was synthesized by a simple hydrothermal method. Briefly, 0.6 mmol Ni(NO 3 ) 2 ⋅6H 2 O was dissolved in deionized water (52 ml) and stirred for about 10 min to obtain a green solution, then 8 ml NH 4 OH (25 %) was added to provide a weakly alkaline environment, and subsequently put the precursor (MoS 2 /CC) into the solution. The mixture was transferred into a 100 ml Teflon-lined high-pressure reactor and heated at 180 ℃ for 3 h. After cooling down to room temperature, the sample was washed with deionized water and ethanol at least three times and dried at 60 ℃. The obtained sample was denoted as NiS-MoO x /CC. By adjusting content of Ni(NO 3 ) 2 ⋅6H 2 O (0.4 mmol, 0.5 mmol, 0.6 mmol, 1 mmol, 2 mmol), the obtained samples were named as NiS-MoO x /CC-0.4, NiS-MoO x /CC-0.5, NiS-MoO x /CC-0.6, NiS-MoO x /CC-1 and NiS-MoO x /CC-2, respectively. Take a similar preparation approach, the sample by adding only processed CC is denoted as Ni(OH) 2 /CC. 2.3. Synthesis of MoS 2 /CC. 2 mmol Na 2 MoO 4 ⋅2H 2 O and 8 mmol CH 4 N 2 S were dissolved in deionized water (60 mL) and stirred for about 15 min. The treated CC was immersed in the solution, and then transferred to a 100 mL Teflon-lined high pressure reactor for hydrothermal reaction at 200 ℃ for 24 h, and finally washed with deionized water and ethanol at least three times and dried naturally at room temperature. 2.4. Characterizations. The scanning electron microscopy were performed on ULTRA plus. The powder X-ray diffraction (XRD) patterns were performed on a Rigaku Smart Lab X-ray diffractometer operated at 40 kV using 0.154 nm Cu kα radiation at a scanning rate of 6 ◦ /min. The morphology and structure were observed under a Talos F200s High-resolution transmission electron microscope (HRTEM) with an accelerating voltage of 200 kV. X-ray photoelectron spectroscopy (XPS) was collected by a scanning X-ray microprobe (Al Kα hv = 1486.6 eV) to analyze the chemical states of the elements, and the binding energies of all elements were calibrated by using the C 1s peak of adventitious carbon at 284.60 eV. 2.5. Electrochemical Measurements. All potentials mentioned here were measured without iR-correction, and OER performance tests were performed on a CHI660E electrochemical workstation, using a three-electrode system in 1.0 M KOH electrolyte. The KOH was purchased from Energy Chemica purity (Energy chemical, 99.99%). A Hg/Hg 2 Cl 2 electrode was selected as the reference electrode and a graphite rod was selected as the counter electrode. The obtained self-supported electrode directly was used as a working electrode. Linear sweep voltammetry (LSV) polarization curves were measured from 0 to 1V (vs. SCE) with a slow scan rate of 5 mV s -1 . The measured potential can be converted into a reversible hydrogen electrode (RHE) according to the Nernst equation： E RHE = E SCE + 0.0591 × pH + 0.2412 Tafel slopes were obtained by plotting overpotential η against log (j) from LSV curves, the overpotential (η) was calculated according to the following equation: η (V) = E RHE - 1.23 V and different Tafel slopes represent different kinetic properties and mechanisms. Electrochemical impedance spectroscopy (EIS) was carried out at OCV in a frequency range of 100 K Hz to 0.1 Hz. The galvanostatic measurement at a fixed current density (j) of 10 mA⋅cm -2 were taken to investigate the catalyst stability. In a non-Faradaic region, a potential range was selected, the difference in current density and scan rates at a certain potential (generally the middle potential) is plotted, and a straight line is fitted. Half the differences about current density was calculated to obtain the value of C dl for obtaining the related ECSA. Cyclic voltammetry (CV) curves were measured at different scan rates of 20, 40, 60, 80, and 100 mV s -1 . Stability is also an important criterion for a catalyst material. In this work, the stability of the catalyst is tested using chronoamperometry at a voltage of 0.45 V (vs. SCE). 3. Results and Discussion 3.1 Morphology and structure characterization of materials The schematic illustration for the preparation of the NiS-MoO x /CC composite is shown in Fig. 1 . The X-ray powder diffraction (XRD) patterns of all samples are presented in Fig. 2 . The diffraction peak observed at 2θ=25° corresponds to the CC substrate. For the MoS 2 /CC sample ( Fig. 2a ), diffraction peaks at 2θ=14.3°, 35.8°, 39.5°, and 58.3° are assigned to the (002), (100), (103), and (110) crystallographic plane of MoS 2 (JCPDS NO. 37-1492), respectively, confirming the successful synthesis of 2H phase of MoS 2 . The XRD pattern of Ni(OH) 2 /CC ( Fig. 2b ) shows diffraction peaks corresponding to the characteristic peaks of Ni(OH) 2 (JCPDS NO. 14-0117), indicating the successful growth of Ni(OH) 2 on the CC. For the NiS-MoO x /CC sample ( Fig. 2c ), diffraction peaks at 2θ = 18.5°, 32.2°, 35.7°, 37.3°, 40.5°, 48.8°, 52.6°, 56.25°, 57.4°, and 59.7° are attributed to the (110), (300), (021), (220), (211), (131), (401), (321) ,(330), and (012) crystallographic plane of NiS (JCPDS NO. 86-2281), respectively. Additionally, diffraction peaks at 2θ = 21.9°, 22.68° and 48.8° are associated with the (321), (330) and (012) crystal faces of Mo 9 O 26 , respectively. The XRD pattern of NiS/CC ( Fig. 2d ) shows diffraction peaks corresponding to characteristic peaks of NiS (JCPDS NO.86-2281), confirming the successful synthesis of NiS on CC. The presence of all characteristic peaks confirms the successful synthesis for each of the materials. The morphology of the catalysts was characterized using scanning electron microscopy (SEM), as depicted in Fig. 3 . The morphology characteristics of the MoS 2 /CC precursor is illustrated in Fig. 3a-c , revealing that MoS 2 is uniformly distributed on the carbon cloth surface, exhibiting a nanoflower morphology. However, as shown in the Fig. 3d-f , NiS-MoO x /CC is composed of numerous nanosheets grown vertically on carbon cloth with a morphology similar to a three-dimensional nanosheet array. This structure increases the contact area between the catalysts and the electrolyte solution, potentially enhancing the utilization of active sites and improving electrical conductivity of the catalysts, and thereby boosting the electrocatalytic performance. A comparison of the SEM images of MoS 2 /CC reveals a change in the morphology of NiS-MoO x /CC, indicating that the prepared precursor may underwent a phase transformation from MoS 2 to Mo 9 O 26 , which is consistent with the XRD results. Transmission electron microscopy (TEM) was employed to further investigate the microstructures of NiS-MoO x /CC-0.6. As illustrated in Fig. 4a , the material exhibits a nanosheets morphology. The high-resolution transmission electron microscopy (HRTEM) images are given as Fig. 4b and 4c , which clearly display the lattice fringe spacing of 0.30 nm and 0.62 nm corresponding to the (001) crystal face of NiS and the (310) crystal face of Mo 9 O 26 , respectively. Additionally, Fig 4c reveals some lattice structure distortion, which may be the effect of Mo incorporating into the NiS lattice as reported previously in the literature. 31 Furthermore, Fig. 4d-h displays energy-dispersive X-ray spectroscopy (EDS) elemental mapping, which clearly demonstrates the uniform distribution of S, Ni, O and Mo elements within catalyst. Further characterization of the prepared samples was performed using X-ray photoelectron spectroscopy (XPS) to analyze the surface composition and valence state of the elements in the catalysts. As shown in Fig. 5a , spin-orbit double peaks at energies of 233.05 eV and 236.1 eV are observed, corresponding to Mo 3d 5/2 and Mo 3d 2/3 of Mo 6+ , respectively. 32 In the XPS spectrum of Ni 2p, the peaks at binding energies of 855.7 eV and 873.3 eV can be assigned to Ni 2p 3/2 and Ni 2p 1/2 of Ni 2+ in NiS, respectively, and the peaks at 858.8 eV and 877.1 eV correspond to Ni 3+ that arise from surface oxidation of Ni 2+ ( Fig. 5b ). 33 The remaining peaks at 881.2 eV and 862.75 eV are assigned to satellite peaks. As shown in Fig. 5c , the XPS spectrum of S 2p exhibits a peak at 163.25 eV, attributed to S 2- with the low surface coordination, the peak at 162.05 eV is associated with the metal-S bond, while the peak at 163.5 eV is attributed to sulfur oxide, formed by the oxidation of sulfur compounds in the sample. 34 Notably, as the concentration of Ni ions in the sample increase, the M-S peak was shifted to a lower binding energy, indicating an increase in the Ni-S bond strength. 35 The XPS spectrum of O 1s can be deconvoluted into two peaks at binding energy of 531.9 eV and 533.1 eV, as shown in Fig. 5d , labeled as O1 and O2, corresponding to the metal-oxygen bond (Mo-O) and oxygen adsorbed on the sample surface, respectively. 36 3.2 Electrocatalytic OER measurements To investigate the OER performance of prepared electrocatalysts, their catalytic activities were systematically tested in a standard three-electrode system and evaluated using LSV curves and the corresponding Tafel slope. As shown in Fig 6a-c , NiS-MoO x /CC-0.6 exhibits the lowest overpotential (340 mV at 50 mA cm -2 ) and the smallest Tafel slope (225.9 mV dec -1 ). Notably, as depicted in the Fig. 6a and 6b , a prominent oxidation peak appears at 1.36V (vs. RHE), attributed to the oxidation of Ni 2+ to Ni 3+ , as reported for other nickel-based catalysts. 34 Based on this analysis, the appearance of oxidation peaks can serve as an important active intermediate, which effectively accelerates the reaction and enhance the catalytic performance of OER. 37 Additionally, the C dl value of the catalysts was obtained using cyclic voltammetry in a region with no faradaic response at different scan rates to reflect the ECSA ( Fig. 6d and Fig. S1 ). The C dl value of NiS/CC is 38.8 mF cm -2 , which is higher than NiS-MoOx /CC-0.6 (18.1 mF cm -2 ). These results indicated that although NiS/CC provides more reaction active sites, NiS-MoO x /CC-0.6 exhibits the higher kinetic for OER (Tafel slope of 225.9 mV dec -1 ) attributed to the synergistic effect between Ni and Mo on the enhanced OER efficiency. 38 Furthermore, to determine the charge transfer capability of the catalysts during the OER process, electrochemical impedance spectroscopy (EIS) measurements were conducted at open circuit potential in 1.0 M KOH. The Nyquist plots from EIS characterization are shown in Fig. 6e , the diameter of the semicircle in the high-frequency region reflects the charge transfer resistance (R ct ) at the catalyst-electrolyte interface. 39 NiS-MoO x /CC-0.6 exhibits a lower R ct compared to the others, indicating faster charge transfer and superior electrocatalytic performance, confirming that the presence of Mo enhances charge transfer in NiS-MoO x /CC during the OER process. The stability of NiS-MoO x /CC-0.6 was conducted via 32 h chronoamperometric test, Fig. 6f reveals the current density decreased slightly, with overall stability remaining at 73 %. Additionally, a comparison of the optimal catalysts and other reported nickel-based electrocatalysts in Table. S1 suggests that the OER activity of NiS-MoO x /CC-0.6 is comparable or superior to other nickel-based OER electrocatalysts. 4. Conclustions In this study, a series of self-supported 3D nanosheet array composite electrode materials were synthesized by in situ growing a MoS 2 precursor on CC using a hydrothermal method. The optimal catalyst, NiS-MoO x /CC-0.6, demonstrate superior activity towards the OER, with a low overpotential of 340 mV at a current density of 50 mA⋅cm -2 . The remarkable catalytic performance in OER is attributed to three-dimensional nanosheet array structure, which provides abundant surface-exposed active sites and a good electrical conductivity of the catalyst. This study offers useful insights into the development of nickel-based sulfide electrocatalyst and the synthesis of high-performance transition metal-based OER catalysts. Abbreviations OER: Oxygen evolution reaction CC: Carbon cloth 3D: Three-dimensional HER: Hydrogen evolution reaction NiS-MoO x /CC: NiS-MoOx nanosheet array on carbon cloth SEM: Scanning electron microscopy XRD: X-ray diffraction HRTEM: High-resolution transmission electron microscope XPS: X-ray photoelectron spectroscopy LSV: Linear sweep voltammetry SCE: Saturated calomel electrode RHE: Reversible hydrogen electrode EIS: Electrochemical impedance spectroscopy OCV: Open circuit voltage C dl : Double-layer capacitance ECSA: Electrochemically active surface area CV: Cyclic voltammetry Declarations Data Availability Data is provided within the manuscript or supplementary information files. Acknowledgements We thank the funding sources from National Nature Science Foundation of China (22168035), the Youth Science and Technology Program of Gansu Province (20JR10RA102 and 20JR5R514). ■ Funding This work was financially supported by the National Nature Science Foundation of China (22168035), the Youth Science and Technology Program of Gansu Province (20JR10RA102 and 20JR5R514). ■ Author Information Authors and Affiliations: Dongying Haike Ruilin Chemical Co., Ltd, North of Gangchenglu, Dongying Port Economic Development Zone, Dongying, 257000 (P. R. China) Weiwei Zhang, Hui Wang Northwest Normal University College of Chemistry and Chemical Engineering No.967 Anning East Road Lanzhou, 730070 (P. R. China) Haidong Yang Contributions Weiwei Zhang and Haidong Yang: writing, review, editing, supervision, funding acquisition, investigation, date analysis. Hui Wang: investigation, date analysis visualization, conceptualization. Corresponding author Correspondence to Weiwei Zhang, Haidong Yang . ■ Ethics declarations Conflict of Interest The authors declare no competing interests. Ethics and Consent to Participate Not applicable. Consent for Publication Not applicable. ■ Additional information Publisher ’ s Note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations. ■ Electronic Supplementary Material Below is the link to the electronic supplementary material. ■ Rights and permissions Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law. 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ACS Nano. 10.1021/acsnano.8b07700 Wang Y-L, Yang T-H, Yue S, Zheng H-B, Liu X-P, Gao P-Z, Qin H, Xiao H-N (2023) Effects of Alternating Magnetic Fields on the OER of Heterogeneous Core–Shell Structured NiFe 2 O 4 @(Ni, Fe)S/P. ACS Appl Mater Interfaces. 10.1021/acsami.2c16656 Additional Declarations No competing interests reported. Supplementary Files SupportingInformation.docx Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6326912","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":436830952,"identity":"a4cf7deb-cb4d-4a60-aac8-b677c4ae002f","order_by":0,"name":"Weiwei Zhang","email":"","orcid":"","institution":"Dongying Haike Ruilin Chemical Co., Ltd, North of Gangchenglu, Dongying Port Economic Development Zone","correspondingAuthor":false,"prefix":"","firstName":"Weiwei","middleName":"","lastName":"Zhang","suffix":""},{"id":436830953,"identity":"49a3f059-8f36-41b2-8aa4-f1b06d11dcd3","order_by":1,"name":"Haidong Yang","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA6klEQVRIiWNgGAWjYDACCQaDAx8q/smxMfN/fJBQUUOUFsODM84cMOZnbzA2eHDmGFFajA/zth1InNlzwEzyYQszYR0Gt5s3HOY5c4dxw42EtIrEBjYG/vbuBPxa7hwrODin4hmzwY2EYzcSd8gwSJw5uwG/lhs5BgfenGFmM7iR2HYj8Qwbg4FELhFaeNuYeQxuJLMVJLYxE6flIG/bYQnJnmNsDERpkbyRVgAM5DQDfvYeZomEM8d4CPqF70by5g8fKmzqgW5j/PijokaOv70XvxaFA2gCPHiVg4B8A0Elo2AUjIJRMOIBACe7V12PvtwvAAAAAElFTkSuQmCC","orcid":"","institution":"Northwest Normal University College of Chemistry and Chemical Engineering","correspondingAuthor":true,"prefix":"","firstName":"Haidong","middleName":"","lastName":"Yang","suffix":""},{"id":436830954,"identity":"8849a0d5-23f7-4f86-a938-9d085c362ea0","order_by":2,"name":"Hui Wang","email":"","orcid":"","institution":"Dongying Haike Ruilin Chemical Co., Ltd, North of Gangchenglu, Dongying Port Economic Development Zone","correspondingAuthor":false,"prefix":"","firstName":"Hui","middleName":"","lastName":"Wang","suffix":""}],"badges":[],"createdAt":"2025-03-28 09:38:25","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6326912/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6326912/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":79865799,"identity":"f1fff2e3-8af5-459f-afdc-a54affe5dfcc","added_by":"auto","created_at":"2025-04-03 18:57:54","extension":"jpeg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":249657,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic diagram of preparation of electrocatalyst of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC.\u003c/p\u003e","description":"","filename":"floatimage1.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/54494cfa01bbd82bac04ddc9.jpeg"},{"id":79866169,"identity":"977c023a-4d2e-4d06-a3e4-615b6ea78ec2","added_by":"auto","created_at":"2025-04-03 19:05:54","extension":"jpeg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":341342,"visible":true,"origin":"","legend":"\u003cp\u003eXRD pattern of the catalysts; (a) MoS\u003csub\u003e2\u003c/sub\u003e/CC; (b) Ni(OH)\u003csub\u003e2\u003c/sub\u003e/CC; (c) NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6; (d) NiS/CC.\u003c/p\u003e","description":"","filename":"floatimage2.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/f0c145c5ea98fa775f8c5eb6.jpeg"},{"id":79865806,"identity":"ccf968bd-2d9f-4e2e-8b27-e11e5feb3ab2","added_by":"auto","created_at":"2025-04-03 18:57:54","extension":"jpeg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":1283501,"visible":true,"origin":"","legend":"\u003cp\u003e(a-c) SEM images of MoS\u003csub\u003e2\u003c/sub\u003e/CC at different magnifications; (d-f) SEM images of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 at different magnifications.\u003c/p\u003e","description":"","filename":"floatimage3.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/09fdf05ee34a19f8a41d1337.jpeg"},{"id":79865800,"identity":"237bed38-f9c8-4306-a03a-730699f564eb","added_by":"auto","created_at":"2025-04-03 18:57:54","extension":"jpeg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":771243,"visible":true,"origin":"","legend":"\u003cp\u003e(a) TEM image of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6; (b) and (c) HRTEM image of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6; (d-h) elemental distribution of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6.\u003c/p\u003e","description":"","filename":"floatimage4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/4aa05a81b02b8da525d6567f.jpeg"},{"id":79866172,"identity":"e73f61f6-9bd7-410c-99ea-da7ca4b10ce7","added_by":"auto","created_at":"2025-04-03 19:05:54","extension":"jpeg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":687679,"visible":true,"origin":"","legend":"\u003cp\u003eXPS spectra of the NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC; (a) Mo 3d; (b) Ni 2p; (c) Co 2p; (d) O 1s.\u003c/p\u003e","description":"","filename":"floatimage5.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/adcf7fbd7b64236236336c4c.jpeg"},{"id":79865819,"identity":"ef50b01c-4405-4be4-bc83-ec7b18937092","added_by":"auto","created_at":"2025-04-03 18:57:55","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":271971,"visible":true,"origin":"","legend":"\u003cp\u003eOER performance: (a) and (b) LSV curves; (c) Tafel plots; (d) Electrochemical double-layer capacitance; (e) EIS result; (f) i-t curve of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 in 1 M KOH.\u003c/p\u003e","description":"","filename":"6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/fc17626fce26d05f503d7140.jpg"},{"id":80042931,"identity":"ec85518d-e8e7-4807-a40c-ad6e7ec7c037","added_by":"auto","created_at":"2025-04-07 09:32:06","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":4336472,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/3cc0eae7-434d-464f-ac3e-1cd77063901e.pdf"},{"id":79865808,"identity":"715d6db2-318d-4be7-a484-0d00cbf1b04e","added_by":"auto","created_at":"2025-04-03 18:57:54","extension":"docx","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":763400,"visible":true,"origin":"","legend":"","description":"","filename":"SupportingInformation.docx","url":"https://assets-eu.researchsquare.com/files/rs-6326912/v1/959400eab47ffac65be4093c.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Three Dimensional NiS-MoOx/CC Nanosheet Array for Efficient Electrocatalytic Oxygen Evolution Reaction","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eCurrently, the excessive consumption of fossil fuels and the associated environmental pollution has become one of the foremost global challenges. Among renewable energy sources, hydrogen has been utilized as a viable alternative fuel due to its environmental friendliness, high energy density and low losses.\u003csup\u003e1, 2\u003c/sup\u003e Currently, hydrogen is primarily produced through the steam-methane reforming process, which is both inefficient and responsible for significant carbon dioxide emissions.\u003csup\u003e3\u003c/sup\u003e Therefore, it is crucial to explore alternative methods for hydrogen production. As one of the most promising strategy, electrolytic water splitting involves two half-reactions: hydrogen evolution reaction (HER) and oxygen evolution reaction (OER).\u003csup\u003e4-6\u003c/sup\u003e The OER involves a complex four-electron transfer process with slow kinetics, requiring a high overpotential to drive the reaction, which presents a bottleneck in hydrogen production through electrolytic water splitting.\u003csup\u003e7, 8\u003c/sup\u003e\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eIn recent years, significance progress has been made in developing cost-efficient OER electrocatalysts. Transition metal-based catalysts with high activity toward the OER in alkaline media have been extensively studied, attributed to their unique intrinsic structures and physicochemical properties.\u003csup\u003e9, 10\u003c/sup\u003e For instance, transition metal sulfides,\u003csup\u003e11, 12\u003c/sup\u003e selenides,\u003csup\u003e13, 14\u003c/sup\u003e phosphide,\u003csup\u003e15-17\u003c/sup\u003e nitride,\u003csup\u003e18, 19\u003c/sup\u003e hydroxide,\u003csup\u003e20, 21\u003c/sup\u003e oxides,\u003csup\u003e22\u003c/sup\u003e and metal alloys \u003csup\u003e23, 24\u003c/sup\u003e have shown excellent OER activity under similar conditions, thereby promoting the water splitting efficiency. Transition metal sulfides have been demonstrated as promising OER catalyst due to their abundant active sites and high intrinsic activity.\u003csup\u003e25\u003c/sup\u003e For example, nickel sulfide has been proved as an active OER electrocatalyst in alkaline media, undergoing a transformation from Ni\u003csup\u003e2+\u003c/sup\u003e to Ni\u003csup\u003e3+\u003c/sup\u003e during the OER process, which produces disordered NiOOH as the active site for the catalytic reaction.\u003csup\u003e26\u003c/sup\u003e Additionally, structural regulation of the catalyst is crucial for the high electrocatalytic performance, which not only affects the morphology of catalysts but also accelerates the diffusion and adsorption of the reactant, thereby promoting the whole reaction rate.\u003csup\u003e27\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eGenerally speaking, there are two effective methods for optimizing the OER performance of catalysts. The first approach involves preparing a composite material to create heterogeneous structure or multicomponent catalyst in which synergistic effect can be observed in enhancing both OER activity and stability. For instance, the NiS/Ni\u003csub\u003e2\u003c/sub\u003eP heterogeneous structure by Xiao et al. prepared demonstrates excellent OER performance due to its low charge transfer resistance, abundant active sites, and the synergistic effect between Ni\u003csub\u003e2\u003c/sub\u003eP and NiS.\u003csup\u003e28\u003c/sup\u003e Another viable method to improve the catalytic performance for OER is the fabrication of self-supported electrode through an in-situ process. Compared to powder electrode materials, self-supported materials exhibit a more ordered structure with fully exposed active sites, and simultaneously facilitate efficient mass and charge transfer during electrocatalysis. For example, Zhang et al. developed a self-supported WO\u003csub\u003e3\u003c/sub\u003e@RuO\u003csub\u003e2\u003c/sub\u003e nanowire on a titanium mesh, which exhibits enhanced OER kinetics due to its three-dimensional structure, leading to a lower interface resistance between active sites and the electrolyte.\u003csup\u003e29\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eTherefore, the preparation of electrocatalysts with self-supported structures presents a promising strategy for enhancing electrocatalytic OER performance.\u003csup\u003e30\u003c/sup\u003e Herein, the in situ growth of self-supported NiS-MoO\u003csub\u003ex\u003c/sub\u003e nanosheet array on carbon cloth (CC) was prepared through a hydrothermal process (denoted as NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC). Compared to power electrocatalysts bonded with polymer adhesives, the self-supported NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC exhibit enhanced stability and superior OER performance, effectively preventing the loss of active components and improving the conductivity of the catalysts. The NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 catalysts exhibited a low overpotential of 340 mV at a current density of 50 mA cm\u003csup\u003e-2\u003c/sup\u003e for the OER. The self-supported NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC electrode as an OER electrocatalyst exhibits excellent catalytic activity, which gives a promising candidate as OER electrocatalysts.\u003c/p\u003e"},{"header":"2. Experimental Section","content":"\u003cp\u003e\u003cstrong\u003e2.1. Materials.\u003c/strong\u003e Nickel nitrate hexahydrate (Ni(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e·6H\u003csub\u003e2\u003c/sub\u003eO), ammonium fluoride (NH\u003csub\u003e4\u003c/sub\u003eF) and thiourea (CH\u003csub\u003e4\u003c/sub\u003eN\u003csub\u003e2\u003c/sub\u003eS) were purchased from Sinopharm Chemical Reagents Co., Ltd. Sodium molybdate dihydrate (Na\u003csub\u003e2\u003c/sub\u003eMoO\u003csub\u003e4\u003c/sub\u003e·2H\u003csub\u003e2\u003c/sub\u003eO) was obtained from Shanghai Energy and Chemical Co., Ltd. Nitric acid (HNO\u003csub\u003e3\u003c/sub\u003e) was obtained from Beijing Chemical Plant. Sulfuric acid (H\u003csub\u003e2\u003c/sub\u003eSO\u003csub\u003e4\u003c/sub\u003e) was obtained from Chengdu Kelong Chemical Co., Ltd. Ammonium hydroxide (NH\u003csub\u003e4\u003c/sub\u003eOH) was obtained from Tianjin Kemiou Chemical Reagent Co., Ltd. Urea (CO(NH\u003csub\u003e2\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e) was obtained from Tianjin Dengfeng chemical reagent factory. Ethanol (C\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e6\u003c/sub\u003eO) was obtained from Lianlong Bohua Pharmaceutical Chemical Co., Ltd. All chemical reagents used without further purification., and all chemical reagents were used without further purification.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.2. Synthesis of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC.\u0026nbsp;\u003c/strong\u003eNiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC was synthesized by a simple hydrothermal method. Briefly, 0.6 mmol Ni(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e⋅6H\u003csub\u003e2\u003c/sub\u003eO was dissolved in deionized water (52 ml) and stirred for about 10 min to obtain a green solution, then 8 ml NH\u003csub\u003e4\u003c/sub\u003eOH (25 %) was added to provide a weakly alkaline environment, and subsequently put the precursor (MoS\u003csub\u003e2\u003c/sub\u003e/CC) into the solution. The mixture was transferred into a 100 ml Teflon-lined high-pressure reactor and heated at 180 ℃ for 3 h. After cooling down to room temperature, the sample was washed with deionized water and ethanol at least three times and dried at 60 ℃. The obtained sample was denoted as NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC. By adjusting content of Ni(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e⋅6H\u003csub\u003e2\u003c/sub\u003eO (0.4 mmol, 0.5 mmol, 0.6 mmol, 1 mmol, 2 mmol), the obtained samples were named as NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.4, NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.5, NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6, NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-1 and NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-2, respectively. Take a similar preparation approach, the sample by adding only processed CC is denoted as Ni(OH)\u003csub\u003e2\u003c/sub\u003e/CC.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.3. Synthesis of MoS\u003csub\u003e2\u003c/sub\u003e/CC.\u003c/strong\u003e 2 mmol Na\u003csub\u003e2\u003c/sub\u003eMoO\u003csub\u003e4\u003c/sub\u003e⋅2H\u003csub\u003e2\u003c/sub\u003eO and 8 mmol CH\u003csub\u003e4\u003c/sub\u003eN\u003csub\u003e2\u003c/sub\u003eS were dissolved in deionized water (60 mL) and stirred for about 15 min. The treated CC was immersed in the solution, and then transferred to a 100 mL Teflon-lined high pressure reactor for hydrothermal reaction at 200 ℃ for 24 h, and finally washed with deionized water and ethanol at least three times and dried naturally at room temperature.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.4. Characterizations.\u003c/strong\u003e The scanning electron microscopy were performed on ULTRA plus. The powder X-ray diffraction (XRD) patterns were performed on a Rigaku Smart Lab X-ray diffractometer operated at 40 kV using 0.154 nm Cu kα radiation at a scanning rate of 6\u003csup\u003e◦\u003c/sup\u003e/min. The morphology and structure were observed under a Talos F200s High-resolution transmission electron microscope (HRTEM) with an accelerating voltage of 200 kV. X-ray photoelectron spectroscopy (XPS) was collected by a scanning X-ray microprobe (Al Kα\u0026nbsp;hv = 1486.6 eV) to analyze the chemical states of the elements, and the binding energies of all elements were calibrated by using the C 1s peak of adventitious carbon at 284.60 eV.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.5. Electrochemical Measurements.\u003c/strong\u003e All potentials mentioned here were measured without iR-correction, and OER performance tests were performed on a CHI660E electrochemical workstation, using a three-electrode system in 1.0 M KOH electrolyte. The KOH was purchased from Energy Chemica purity (Energy chemical, 99.99%). A Hg/Hg\u003csub\u003e2\u003c/sub\u003eCl\u003csub\u003e2\u003c/sub\u003e electrode was selected as the reference electrode and a graphite rod was selected as the counter electrode. The obtained self-supported electrode directly was used as a working electrode. Linear sweep voltammetry (LSV) polarization curves were measured from 0 to 1V (vs. SCE) with a slow scan rate of 5 mV s\u003csup\u003e-1\u003c/sup\u003e. The measured potential can be converted into a reversible hydrogen electrode (RHE) according to the Nernst equation：\u003c/p\u003e\n\u003cp\u003eE\u003csub\u003eRHE\u003c/sub\u003e = E\u003csub\u003eSCE\u003c/sub\u003e + 0.0591 × pH + 0.2412\u003c/p\u003e\n\u003cp\u003eTafel slopes were obtained by plotting overpotential η against log (j) from LSV curves, the overpotential (η) was calculated according to the following equation:\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eη (V) = E\u003csub\u003eRHE\u003c/sub\u003e - 1.23 V\u003c/p\u003e\n\u003cp\u003eand different Tafel slopes represent different kinetic properties and mechanisms. Electrochemical impedance spectroscopy (EIS) was carried out at OCV in a frequency range of 100 K Hz to 0.1 Hz. The galvanostatic measurement at a fixed current density (j) of 10 mA⋅cm\u003csup\u003e-2\u0026nbsp;\u003c/sup\u003ewere taken to investigate the catalyst stability. In a non-Faradaic region, a potential range was selected, the difference in current density and scan rates at a certain potential (generally the middle potential) is plotted, and a straight line is fitted. Half the differences about current density was calculated to obtain the value of C\u003csub\u003edl\u003c/sub\u003e for obtaining the related ECSA. Cyclic voltammetry (CV) curves were measured at different scan rates of 20, 40, 60, 80, and 100 mV s\u003csup\u003e-1\u003c/sup\u003e.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eStability is also an important criterion for a catalyst material. In this work, the stability of the catalyst is tested using chronoamperometry at a voltage of 0.45 V (vs. SCE).\u003c/p\u003e"},{"header":"3. Results and Discussion","content":"\u003cp\u003e3.1 Morphology and structure characterization of materials\u003c/p\u003e\n\u003cp\u003eThe schematic illustration for the preparation of the NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC composite is shown in \u003cstrong\u003eFig. 1\u003c/strong\u003e. The X-ray powder diffraction (XRD) patterns of all samples are presented in \u003cstrong\u003eFig. 2\u003c/strong\u003e. The diffraction peak observed at 2\u0026theta;=25\u0026deg; corresponds to the CC substrate. For the MoS\u003csub\u003e2\u003c/sub\u003e/CC sample (\u003cstrong\u003eFig. 2a\u003c/strong\u003e), diffraction peaks at 2\u0026theta;=14.3\u0026deg;, 35.8\u0026deg;, 39.5\u0026deg;, and 58.3\u0026deg; are assigned to the (002), (100), (103), and (110) crystallographic plane of MoS\u003csub\u003e2\u003c/sub\u003e (JCPDS NO. 37-1492), respectively, confirming the successful synthesis of 2H phase of MoS\u003csub\u003e2\u003c/sub\u003e. The XRD pattern of Ni(OH)\u003csub\u003e2\u003c/sub\u003e/CC (\u003cstrong\u003eFig. 2b\u003c/strong\u003e) shows diffraction peaks corresponding to the characteristic peaks of Ni(OH)\u003csub\u003e2\u003c/sub\u003e (JCPDS NO. 14-0117), indicating the successful growth of Ni(OH)\u003csub\u003e2\u003c/sub\u003e on the CC. For the NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC sample (\u003cstrong\u003eFig. 2c\u003c/strong\u003e), diffraction peaks at 2\u0026theta; = 18.5\u0026deg;, 32.2\u0026deg;, 35.7\u0026deg;, 37.3\u0026deg;, 40.5\u0026deg;, 48.8\u0026deg;, 52.6\u0026deg;, 56.25\u0026deg;, 57.4\u0026deg;, and 59.7\u0026deg; are attributed to the (110), (300), (021), (220), (211), (131), (401), (321) ,(330), and (012) crystallographic plane of NiS (JCPDS NO. 86-2281), respectively. Additionally, diffraction peaks at 2\u0026theta; = 21.9\u0026deg;, 22.68\u0026deg; and 48.8\u0026deg; are associated with the (321), (330) and (012) crystal faces of Mo\u003csub\u003e9\u003c/sub\u003eO\u003csub\u003e26\u003c/sub\u003e, respectively. The XRD pattern of NiS/CC (\u003cstrong\u003eFig. 2d\u003c/strong\u003e) shows diffraction peaks corresponding to characteristic peaks of NiS (JCPDS NO.86-2281), confirming the successful synthesis of NiS on CC. The presence of all characteristic peaks confirms the successful synthesis for each of the materials.\u003c/p\u003e\n\u003cp\u003eThe morphology of the catalysts was characterized using scanning electron microscopy (SEM), as depicted in \u003cstrong\u003eFig. 3\u003c/strong\u003e. The morphology characteristics of the MoS\u003csub\u003e2\u003c/sub\u003e/CC precursor is illustrated in \u003cstrong\u003eFig. 3a-c\u003c/strong\u003e, revealing that MoS\u003csub\u003e2\u003c/sub\u003e is uniformly distributed on the carbon cloth surface, exhibiting a nanoflower morphology. However, as shown in the \u003cstrong\u003eFig. 3d-f\u003c/strong\u003e, NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC is composed of numerous nanosheets grown vertically on carbon cloth with a morphology similar to a three-dimensional nanosheet array. This structure increases the contact area between the catalysts and the electrolyte solution, potentially enhancing the utilization of active sites and improving electrical conductivity of the catalysts, and thereby boosting the electrocatalytic performance. A comparison of the SEM images of MoS\u003csub\u003e2\u003c/sub\u003e/CC reveals a change in the morphology of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC, indicating that the prepared precursor may underwent a phase transformation from MoS\u003csub\u003e2\u003c/sub\u003e to Mo\u003csub\u003e9\u003c/sub\u003eO\u003csub\u003e26\u003c/sub\u003e, which is consistent with the XRD results.\u003c/p\u003e\n\u003cp\u003eTransmission electron microscopy (TEM) was employed to further investigate the microstructures of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6. As illustrated in \u003cstrong\u003eFig. 4a\u003c/strong\u003e, the material exhibits a nanosheets morphology. The high-resolution transmission electron microscopy (HRTEM) images are given as \u003cstrong\u003eFig. 4b and 4c\u003c/strong\u003e, which clearly display the lattice fringe spacing of 0.30 nm and 0.62 nm corresponding to the (001) crystal face of NiS and the (310) crystal face of Mo\u003csub\u003e9\u003c/sub\u003eO\u003csub\u003e26\u003c/sub\u003e, respectively. Additionally,\u003cstrong\u003e\u0026nbsp;Fig 4c\u003c/strong\u003e reveals some lattice structure distortion, which may be the effect of Mo incorporating into the NiS lattice as reported previously in the literature.\u003csup\u003e31\u003c/sup\u003e Furthermore, \u003cstrong\u003eFig. 4d-h\u003c/strong\u003e displays energy-dispersive X-ray spectroscopy (EDS) elemental mapping, which clearly demonstrates the uniform distribution of S, Ni, O and Mo elements within catalyst.\u003c/p\u003e\n\u003cp\u003eFurther characterization of the prepared samples was performed using X-ray photoelectron spectroscopy (XPS) to analyze the surface composition and valence state of the elements in the catalysts. As shown in \u003cstrong\u003eFig. 5a\u003c/strong\u003e, spin-orbit double peaks at energies of 233.05 eV and 236.1 eV are observed, corresponding to Mo 3d\u003csub\u003e5/2\u003c/sub\u003e and Mo 3d\u003csub\u003e2/3\u003c/sub\u003e of Mo\u003csup\u003e6+\u003c/sup\u003e, respectively.\u003csup\u003e32\u003c/sup\u003e In the XPS spectrum of Ni 2p, the peaks at binding energies of 855.7 eV and 873.3 eV can be assigned to Ni 2p\u003csub\u003e3/2\u003c/sub\u003e and Ni 2p\u003csub\u003e1/2\u003c/sub\u003e of Ni\u003csup\u003e2+\u003c/sup\u003e in NiS, respectively, and the peaks at 858.8 eV and 877.1 eV correspond to Ni\u003csup\u003e3+\u003c/sup\u003e that arise from surface oxidation of Ni\u003csup\u003e2+\u003c/sup\u003e (\u003cstrong\u003eFig. 5b\u003c/strong\u003e).\u003csup\u003e33\u003c/sup\u003e The remaining peaks at 881.2 eV and 862.75 eV are assigned to satellite peaks. As shown in \u003cstrong\u003eFig. 5c\u003c/strong\u003e, the XPS spectrum of S 2p exhibits a peak at 163.25 eV, attributed to S\u003csup\u003e2-\u003c/sup\u003e with the low surface coordination, the peak at 162.05 eV is associated with the metal-S bond, while the peak at 163.5 eV is attributed to sulfur oxide, formed by the oxidation of sulfur compounds in the sample.\u003csup\u003e34\u003c/sup\u003e Notably, as the concentration of Ni ions in the sample increase, the M-S peak was shifted to a lower binding energy, indicating an increase in the Ni-S bond strength.\u003csup\u003e35\u003c/sup\u003e The XPS spectrum of O 1s can be deconvoluted into two peaks at binding energy of 531.9 eV and 533.1 eV, as shown in \u003cstrong\u003eFig. 5d\u003c/strong\u003e, labeled as O1 and O2, corresponding to the metal-oxygen bond (Mo-O) and oxygen adsorbed on the sample surface, respectively.\u003csup\u003e36\u003c/sup\u003e\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e3.2 Electrocatalytic OER measurements\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eTo investigate the OER performance of prepared electrocatalysts, their catalytic activities were systematically tested in a standard three-electrode system and evaluated using LSV curves and the corresponding Tafel slope. As shown in\u003cstrong\u003e\u0026nbsp;Fig 6a-c\u003c/strong\u003e, NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 exhibits the lowest overpotential (340 mV at 50 mA cm\u003csup\u003e-2\u003c/sup\u003e) and the smallest Tafel slope (225.9 mV dec\u003csup\u003e-1\u003c/sup\u003e). Notably, as depicted in the \u003cstrong\u003eFig. 6a and 6b\u003c/strong\u003e, a prominent oxidation peak appears at 1.36V (vs. RHE), attributed to the oxidation of Ni\u003csup\u003e2+\u003c/sup\u003e to Ni\u003csup\u003e3+\u003c/sup\u003e, as reported for other nickel-based catalysts.\u003csup\u003e34\u003c/sup\u003e Based on this analysis, the appearance of oxidation peaks can serve as an important active intermediate, which effectively accelerates the reaction and enhance the catalytic performance of OER.\u003csup\u003e37\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eAdditionally, the C\u003csub\u003edl\u003c/sub\u003e value of the catalysts was obtained using cyclic voltammetry in a region with no faradaic response at different scan rates to reflect the ECSA (\u003cstrong\u003eFig. 6d and Fig. S1\u003c/strong\u003e). The C\u003csub\u003edl\u003c/sub\u003e value of NiS/CC is 38.8 mF cm\u003csup\u003e-2\u003c/sup\u003e, which is higher than NiS-MoOx /CC-0.6 (18.1 mF cm\u003csup\u003e-2\u003c/sup\u003e). These results indicated that although NiS/CC provides more reaction active sites, NiS-MoO\u003csub\u003ex\u003c/sub\u003e /CC-0.6 exhibits the higher kinetic for OER (Tafel slope of 225.9 mV dec\u003csup\u003e-1\u003c/sup\u003e) attributed to the synergistic effect between Ni and Mo on the enhanced OER efficiency.\u003csup\u003e38\u003c/sup\u003e Furthermore, to determine the charge transfer capability of the catalysts during the OER process, electrochemical impedance spectroscopy (EIS) measurements were conducted at open circuit potential in 1.0 M KOH. The Nyquist plots from EIS characterization are shown in \u003cstrong\u003eFig. 6e\u003c/strong\u003e, the diameter of the semicircle in the high-frequency region reflects the charge transfer resistance (R\u003csub\u003ect\u003c/sub\u003e) at the catalyst-electrolyte interface.\u003csup\u003e39\u003c/sup\u003e NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 exhibits a lower R\u003csub\u003ect\u003c/sub\u003e compared to the others, indicating faster charge transfer and superior electrocatalytic performance, confirming that the presence of Mo enhances charge transfer in NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC during the OER process.\u0026nbsp;The stability of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 was conducted via 32 h chronoamperometric test, \u003cstrong\u003eFig. 6f\u003c/strong\u003e reveals the current density decreased slightly, with overall stability remaining at 73 %. Additionally, a comparison of the optimal catalysts and other reported nickel-based electrocatalysts in Table. S1 suggests that the OER activity of NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 is comparable or superior to other nickel-based OER electrocatalysts.\u003c/p\u003e"},{"header":"4. Conclustions","content":"\u003cp\u003eIn this study, a series of self-supported 3D nanosheet array composite electrode materials were synthesized by in situ growing a MoS\u003csub\u003e2\u003c/sub\u003e precursor on CC using a hydrothermal method. The optimal catalyst, NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6, demonstrate superior activity towards the OER, with a low overpotential of 340 mV at a current density of 50 mA⋅cm\u003csup\u003e-2\u003c/sup\u003e. The remarkable catalytic performance in OER is attributed to three-dimensional nanosheet array structure, which provides abundant surface-exposed active sites and a good electrical conductivity of the catalyst. This study offers useful insights into the development of nickel-based sulfide electrocatalyst and the synthesis of high-performance transition metal-based OER catalysts.\u003c/p\u003e"},{"header":"Abbreviations","content":"\u003cp\u003eOER: Oxygen evolution reaction\u003c/p\u003e\n\u003cp\u003eCC: Carbon cloth\u003c/p\u003e\n\u003cp\u003e3D: Three-dimensional\u003c/p\u003e\n\u003cp\u003eHER: Hydrogen evolution reaction\u003c/p\u003e\n\u003cp\u003eNiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC: NiS-MoOx nanosheet array on carbon cloth\u003c/p\u003e\n\u003cp\u003eSEM: Scanning electron microscopy\u003c/p\u003e\n\u003cp\u003eXRD: X-ray diffraction\u003c/p\u003e\n\u003cp\u003eHRTEM: High-resolution transmission electron microscope\u003c/p\u003e\n\u003cp\u003eXPS: X-ray photoelectron spectroscopy\u003c/p\u003e\n\u003cp\u003eLSV: Linear sweep voltammetry\u003c/p\u003e\n\u003cp\u003eSCE: Saturated calomel electrode\u003c/p\u003e\n\u003cp\u003eRHE: Reversible hydrogen electrode\u003c/p\u003e\n\u003cp\u003eEIS: Electrochemical impedance spectroscopy\u003c/p\u003e\n\u003cp\u003eOCV: Open circuit voltage\u003c/p\u003e\n\u003cp\u003eC\u003csub\u003edl\u003c/sub\u003e: Double-layer capacitance\u003c/p\u003e\n\u003cp\u003eECSA: Electrochemically active surface area\u003c/p\u003e\n\u003cp\u003eCV: Cyclic voltammetry\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eData Availability\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eData is provided within the manuscript or supplementary information files.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAcknowledgements\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eWe thank the funding sources from National Nature Science Foundation of China (22168035), the Youth Science and Technology Program of Gansu Province (20JR10RA102 and 20JR5R514).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e■ Funding\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis work was financially supported by the National Nature Science Foundation of China (22168035), the Youth Science and Technology Program of Gansu Province (20JR10RA102 and 20JR5R514).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e■ Author Information\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthors and Affiliations:\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eDongying Haike Ruilin Chemical Co., Ltd, North of Gangchenglu, Dongying Port Economic Development Zone, Dongying, 257000 (P. R. China)\u003c/p\u003e\n\u003cp\u003eWeiwei Zhang, Hui Wang\u003c/p\u003e\n\u003cp\u003eNorthwest Normal University College of Chemistry and Chemical Engineering No.967 Anning East Road Lanzhou, 730070 (P. R. China)\u003c/p\u003e\n\u003cp\u003eHaidong Yang\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eContributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eWeiwei Zhang and Haidong Yang: writing, review, editing, supervision, funding acquisition, investigation, date analysis. Hui Wang: investigation, date analysis visualization, conceptualization.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCorresponding author\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eCorrespondence to \u003cstrong\u003eWeiwei Zhang, Haidong Yang\u003c/strong\u003e.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e■ Ethics declarations\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflict of Interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare no competing interests.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eEthics and Consent to Participate\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNot applicable.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConsent for Publication\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNot applicable.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e■ Additional information\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ePublisher\u003c/strong\u003e\u003cstrong\u003e’\u003c/strong\u003e\u003cstrong\u003es Note\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eSpringer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e■ Electronic Supplementary Material\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eBelow is the link to the electronic supplementary material.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e■ Rights and permissions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eSpringer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eHuang HW, Jia HH, Liu Z, Gao PF, Zhao JT, Luo ZL, Yang JL, Zeng J (2017) Understanding of Strain Effects in the Electrochemical Reduction of CO\u003csub\u003e2\u003c/sub\u003e: Using Pd Nanostructures as an Ideal Platform. 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ACS Appl Mater Interfaces. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003e10.1021/acsami.2c16656\u003c/span\u003e\u003cspan address=\"10.1021/acsami.2c16656\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"3D nanosheet array, oxygen evolution reaction, self-supported, catalyst","lastPublishedDoi":"10.21203/rs.3.rs-6326912/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6326912/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eDeveloping highly efficient oxygen evolution reaction (OER) electrocatalysts remains critical for advancing large-scale water splitting. Self-supported electrodes, where catalysts are directly grown on conductive substrates, offer a promising strategy to enhance OER performance by improving structural stability and charge transfer. Herein, we fabricate a self-supported electrode via in situ growth of a MoS\u003csub\u003e2\u003c/sub\u003e precursor on carbon cloth (CC) using a facile hydrothermal method, followed by Ni incorporation to optimize catalytic activity. The optimized NiS-MoO\u003csub\u003ex\u003c/sub\u003e/CC-0.6 electrode exhibits outstanding OER performance with a low overpotential of 340 mV at a current density of 50 mA cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e in alkaline media. This enhanced activity is attributed to the three-dimensional (3D) nanosheet array architecture, which exposes abundant active sites, facilitates electrolyte penetration, and ensures efficient electron transport. Our work provides insights into designing high-performance transition metal-based electrocatalysts for sustainable energy applications.\u003c/p\u003e","manuscriptTitle":"Three Dimensional NiS-MoOx/CC Nanosheet Array for Efficient Electrocatalytic Oxygen Evolution Reaction","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-04-03 18:57:49","doi":"10.21203/rs.3.rs-6326912/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"bdaf20f8-991a-4935-a9be-557698ed836f","owner":[],"postedDate":"April 3rd, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2025-04-07T09:23:55+00:00","versionOfRecord":[],"versionCreatedAt":"2025-04-03 18:57:49","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-6326912","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6326912","identity":"rs-6326912","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}