Unleashing OER Potential: Interface-Engineered CoS2/CuxS via Dynamic Surface Reconstruction

Unleashing OER Potential: Interface-Engineered CoS2/CuxS via Dynamic Surface Reconstruction | Authorea try { document.documentElement.classList.add('js'); } catch (e) { } var _gaq = _gaq || []; _gaq.push(['_setAccount', 'G-8VDV14Y67G']); _gaq.push(['_trackPageview']); (function() { var ga = document.createElement('script'); ga.type = 'text/javascript'; ga.async = true; ga.src = ('https:' == document.location.protocol ? 'https://ssl' : 'http://www') + '.google-analytics.com/ga.js'; var s = document.getElementsByTagName('script')[0]; s.parentNode.insertBefore(ga, s); })(); Skip to main content Preprints Collections Wiley Open Research IET Open Research Ecological Society of Japan All Collections About About Authorea FAQs Contact Us Quick Search anywhere Search for preprint articles, keywords, etc. Search Search ADVANCED SEARCH SCROLL This is a preprint and has not been peer reviewed. Data may be preliminary. 24 July 2025 V1 Latest version Share on Unleashing OER Potential: Interface-Engineered CoS2/CuxS via Dynamic Surface Reconstruction Authors : Heyang Liu , Fengli Wei , Linlin Huang , Chenggong Niu , Zuyang Luo , Tayirjan Taylor Isimjan , and Xiulin Yang 0000-0003-2642-4963 [email protected] Authors Info & Affiliations https://doi.org/10.22541/au.175332441.16575068/v1 224 views 143 downloads Contents Abstract Supplementary Material Information & Authors Metrics & Citations View Options References Figures Tables Media Share Abstract Dynamic surface reconstruction offers a promising route to enhance oxygen evolution reaction (OER) activity by optimizing the adsorption of key intermediates. Here, we construct a pearl-thread-like CoS 2 -Cu x S heterostructure on copper foam (CoS 2 -Cu x S/CF) to induce in situ formation of an active CoOOH-CuO-Cu x S interface at low potentials. In situ Raman spectroscopy confirms the dynamic transformation, while operando electrochemical impedance spectroscopy reveals accelerated charge transfer. Density functional theory calculations show that the interface engineering shifts the d-band center, enhances electron density near the Fermi level, and lowers the free energy barrier for *O to *OOH conversion from 1.78 eV (CoOOH) to 1.48 eV (CoOOH-CuO-Cu x S). Benefiting from the reconstructed interface, CoS 2 -Cu x S/CF achieves an overpotential of 239 mV at 10 mA cm −2 and maintains stability over 200 hours in alkaline electrolyte. This work highlights a dynamic interface strategy to promote intrinsic OER kinetics and catalyst durability. Unleashing OER Potential: Interface-Engineered CoS 2 /Cu x S via Dynamic Surface Reconstruction Heyang Liu a , Fengli Wei a , Linlin Huang a , Chenggong Niu a , Zuyang Luo a , Tayirjan Taylor Isimjan b, *, Xiulin Yang a, * a Guangxi Key Laboratory of Low Carbon Energy Materials, School of Chemistry and Pharmaceutical Sciences, Guangxi Normal University, Guilin 541004, China b Saudi Arabia Basic Industries Corporation (SABIC) at King Abdullah University of Science and Technology (KAUST), Thuwal 23955-6900, Saudi Arabia *Corresponding authors (email: [email protected] ; [email protected] ) Abstract Dynamic surface reconstruction offers a promising route to enhance oxygen evolution reaction (OER) activity by optimizing the adsorption of key intermediates. Here, we construct a pearl-thread-like CoS 2 -Cu x S heterostructure on copper foam (CoS 2 -Cu x S/CF) to induce in situ formation of an active CoOOH-CuO-Cu x S interface at low potentials. In situ Raman spectroscopy confirms the dynamic transformation, while operando electrochemical impedance spectroscopy reveals accelerated charge transfer. Density functional theory calculations show that the interface engineering shifts the d-band center, enhances electron density near the Fermi level, and lowers the free energy barrier for *O to *OOH conversion from 1.78 eV (CoOOH) to 1.48 eV (CoOOH-CuO-Cu x S). Benefiting from the reconstructed interface, CoS 2 -Cu x S/CF achieves an overpotential of 239 mV at 10 mA cm −2 and maintains stability over 200 hours in alkaline electrolyte. This work highlights a dynamic interface strategy to promote intrinsic OER kinetics and catalyst durability. Keywords： Dynamic reconstruction, in situ characterization, oxygen evolution reaction, density functional theory 1. Introduction The transition toward a sustainable energy future necessitates the development of efficient clean energy conversion technologies. Electrochemical water splitting has emerged as a promising route for carbon-neutral hydrogen production; however, its practical implementation is severely impeded by the sluggish kinetics of the oxygen evolution reaction (OER) at the anode. [1, 2] The OER involves complex four-electron transfer steps and substantial energy barriers, particularly during the formation of O=O bonds, resulting in high overpotentials and poor energy efficiency. [3-5] Noble metal-based catalysts, such as RuO 2 and IrO 2 , have been widely employed to mitigate these kinetic challenges by optimizing the adsorption energy of oxygenated intermediates. [6] Nevertheless, noble metals’ limited availability and high cost severely restrict their widespread application in large-scale water splitting systems. [7] To address these limitations, substantial efforts have focused on developing non-noble transition metal-based catalysts that are earth-abundant, cost-effective, and possess tunable electronic structures. [8, 9] Among these, copper-based materials have garnered significant attention in OER systems due to their unique electronic configuration and high natural abundance. For instance, Zhu’s group demonstrated that CuNCo 3 nanosheets achieved an overpotential of 260 mV at 10 mA cm −2 . [10] Chen’s group electrodeposit CoS on Cu(OH) 2 nanorods to form three-dimensional hierarchical core-shell electrocatalysts, achieving an overpotential of 296 mV at the same current density. [11] However, Cu-based catalysts face inherent limitations, including high charge transfer resistance and sluggish reaction kinetics, which hinder their practical application. [12] However, intrinsic drawbacks, including sluggish charge transfer kinetics and suboptimal binding energies for key OER intermediates, limit Cu-based materials’ catalytic efficiency. [13, 14] Interface engineering has recently emerged as a powerful strategy to overcome these challenges by modulating the local electronic environment at heterostructured interfaces, thus enhancing electron transfer, tuning the d-band center, and facilitating optimal adsorption/desorption of oxygen species. [15, 16] While significant progress has been made in designing heterostructures for OER, achieving dynamic surface reconstruction at low overpotentials to form catalytically active phases with strong interfacial electronic coupling remains an outstanding challenge. [17-19] Herein, we report a self-supported, pearl-thread-like CoS 2 -Cu x S heterostructure grown on copper foam (CoS 2 -Cu x S/CF) that enables dynamic surface reconstruction under OER conditions. In situ Raman spectroscopy reveals the low-potential formation of a CoOOH-CuO-CuₓS active interface through partial oxidation of CoS 2 and Cu x S. Operando electrochemical impedance spectroscopy confirms enhanced charge transfer kinetics, and density functional theory (DFT) calculations show that the in situ generated interface optimizes the electronic structure, facilitating stronger *OOH adsorption and lowering the free energy barrier of the rate-determining step. Benefiting from the synergistic effects of dynamic reconstruction and interfacial coupling, the CoS 2 -Cu x S/CF catalyst exhibits outstanding OER performance with a low overpotential of 239 mV at 10 mA cm −2 and excellent operational stability over 200 hours in alkaline media. This study highlights the importance of interface design in promoting dynamic surface reconstruction and provides new insights into the rational design of high-performance, non-noble-metal OER catalysts. 2. Results and Discussion Figure 1 (a) Schematic illustration of the preparation of CoS 2 -Cu x S/CF. (b) XRD patterns. (c) SEM. (d) TEM. (e) HR-TEM image. (f) corresponding lattice spacing profiles. (g) SAED pattern. (h) HAADF-STEM image and corresponding elemental mappings of CoS 2 -Cu x S/CF. The synthesis pathway of CoS 2 -Cu x S/CF is illustrated in Figure 1a. CoS 2 -Cu x S/CF was successfully synthesized through a straightforward one-step hydrothermal vulcanization method. During the preparation, copper foam (CF) with high electrical conductivity was selected as the substrate and copper source, while cobalt nitrate was the source of the cobalt. [20] Under elevated temperature and pressure, thiourea decomposes to generate hydrogen sulfide, which exhibits moderate reducing properties. [21, 22] The resulting sulfide chemically reacts with metal ions, eventually growing CoS 2 and Cu x S on the CF surface. The crystallographic structure of the obtained catalysts was characterized by X-ray diffraction (XRD). As shown in Figure 1b, the diffraction peaks of Cu x S/CF correspond to the standard cards for Cu (JCPDS: No.85-1326), CuS (JCPDS: No.78-0879), and Cu 2 S (JCPDS: No.84-0207). In addition to the Cu and Cu x S phases, CoS 2 -Cu x S/CF exhibits the peaks at 32.3, 36.2, and 39.8°, corresponding to CoS 2 (JCPDS: No.89-1492). Compared with Cu x S/CF, CoS 2 -Cu x S/CF displays peaks with higher intensity, indicating increased crystallinity upon CoS 2 incorporation. Raman spectroscopy was further employed to probe the vibrational modes of bonding sites on the catalyst surface (Figure S1). [23, 24] The peak at 267 cm −1 is assigned to the stretching vibration of the Cu-S bond, while the peak at 390 cm −1 corresponds to Co−S bond. These results are consistent with XRD analysis, confirming the successful synthesis of CoS 2 -Cu x S/CF. [25] To further investigate the copper substrate’s influence, we replaced CF with carbon cloth and synthesized samples under Cu-free conditions. The diffraction peaks of the resulting CoS 2 -Co 3 S 4 /CC correspond to Co 2 S (JCPDS No. 89-1492) and Co 3 S 4 (JCPDS No. 75-1561). In contrast to CoS 2 -Cu x S/CF, the cobalt species in Co 2 S-Co 3 S 4 /CC show more complex phase composition, which can be attributed to the absence of copper during the reaction process (Figure S2). The morphology of CoS 2 –Cu x S/CF was characterized by scanning electron microscopy (SEM). As shown in Figure S3a, the untreated copper foam (CF) exhibits a smooth surface. After hydrothermal treatment, CoS 2 –Cu x S/CF displays a uniformly distributed pearl-thread-like structure across the CF surface (Figure 1b). Compared to the SEM image of Cu x S/CF (Figure S3b), introducing CoS 2 significantly improves the morphology, transforming it from a fragmented granular structure into an ordered pearly thread-like structure. This architecture provides a larger specific surface area and enhances the contact between the catalyst surface and the electrolyte, thereby promoting OER activity. [26] To further investigate the morphological evolution during synthesis, we monitored the catalyst structure as a function of hydrothermal reaction time (Figure S4). Initially, only a few thread-like features were observed within 2 hours. With prolonged reaction time, these structures gradually developed into more ordered pearl-thread-like formations. However, after 4 hours, excessive growth led to the appearance of aggregated granular structures that covered the underlying framework. These observations suggest that insufficient and excessive hydrothermal durations are detrimental to the formation of the optimal morphology, limiting active site exposure and hindering the adsorption of reactive oxygen species. [27] Transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) were further employed to visualize the structure in greater detail. As shown in Figure 1d, TEM confirms the distinctive pearl-thread morphology observed in SEM. High-resolution TEM (HR-TEM) images reveal dual lattice fringes with spacings of 0.247, 0.306, and 0.404 nm, corresponding to the (210) plane of CoS 2 , the (101) plane of Cu 2 S, and the (004) plane of CuS, respectively (Figure 1e and Figure 1f). Selected area electron diffraction (SAED) patterns (Figure 1g) further corroborate these assignments, indicating a polycrystalline structure. Elemental analysis through energy-dispersive X-ray spectroscopy (EDX) (Figure S5) and energy-dispersive spectrometer (EDS) elemental mapping reveals a homogeneous distribution of Co, Cu, and S throughout the structure. Together, these comprehensive characterizations confirm the successful construction of the CoS 2 –Cu x S/CF catalyst. Figure 2 High-resolution XPS spectra of (a) Cu 2p (the inset shows Cu LMM Auger spectra) and (b) S 2p regions in CoS 2 -Cu x S/CF and Cu x S/CF. (c) Co 2p of CoS 2 -Cu x S/CF (d) Contact angle images of CoS 2 -Cu x S/CF and Cu x S/CF. The surface elemental composition and valence states analysis are explored by X-ray photoelectron spectroscopy (XPS). The high-resolution C 1s spectrum of the CoS 2 -Cu x S/CF is employed as a calibration standard for other elements (Figure S6). The peaks at around 284, 284.8, 286, 288.4 eV are designated as C=C, C−C, C−O, and C=O respectively. [28] The high-resolution Cu 2p spectrum demonstrated two peaks centered at 932.6 eV and 933.6 eV, assigned to Cu + and Cu 2+ in CoS 2 -Cu x S/CF (Figure 2a). [29] Compared with Cu x S/CF, the Cu + peak in CoS 2 –Cu x S/CF shifts 0.5 eV to lower binding energy, accompanied by an increased Cu + /Cu 2+ ratio. This indicates that CoS 2 alters the local electronic environment of Cu x S, facilitating the conversion of Cu + to Cu 2+ and accelerating the generation of active intermediates. Given the close binding energies of Cu 0 and Cu + , Cu LMM Auger spectra were also collected (inset of Figure 2a). [30] A peak at 569.2 eV corresponds to Cu + , while a peak at 566.5 eV is attributed to Cu 0 , confirming the oxidation states. [31] Within the S 2p spectral range for CoS 2 -Cu x S/CF (Figure 2b), the characteristic peaks of 161.6 and 162.3 eV are assigned to S 2p 3/2 and S 2p 1/2 , with essentially free of changes in the electronic environment. [32] For the spectra of Co 2p, the peak at 778.4 eV corresponds to Co-S, while 781.5 and 784.2 eV are ascribed to Co 2+ and satellite peak, demonstrating that the cobalt is mainly present in the form of Co 2+ for CoS 2 -Cu x S/CF (Figure 2c). [33, 34] Based on the comprehensive analysis of XPS results, valence shifts of Cu and valence retention of S represent the electron transfer effect exists between CoS 2 and Cu x S, which improves metal coordination environment, thus enhancing catalytic efficiency. Besides, we performed contact angle tests to investigate the impact of interfacial interactions on water adhesion. As shown in Figure 2d, the CoS 2 -Cu x S/CF exhibits a contact angle of 29.2°, much smaller than 56.4° of Cu x S/CF, meaning more intimate contact between catalytic surface and electrolyte for CoS 2 -Cu x S heterostructure, which modifies the catalyst surface wettability, promoting the transportation of catalyst to the electrolyte. [35] Figure 3 (a) LSV curves. (b) Tafel plots. (c) Comparison of overpotential at 10 mA cm −2 and Tafel slopes for previously reported catalysts. (d) C dl plots. (e) ECSA-normalized LSV curves (the insert shows the comparison of ECSA for different catalysts) (f) TOF curves. (g) Faradaic efficiency measurement for OER. (h) Stability test at 100 mA cm −2 (the insert shows stability test at 10 mA cm −2 ) The OER performance of CoS 2 -Cu x S/CF was evaluated in 1.0 M KOH using a standard three-electrode system. As shown in Figure 3a, CoS 2 -Cu x S/CF exhibits outstanding activity, requiring an overpotential of only 239 mV at 10 mA cm −2 and 315 mV at 100 mA cm −2 . Compared with CoS 2 -Co 3 S 4 /CC and Cu x S/CF, CoS 2 -Cu x S/CF demonstrates superior catalytic performance, surpassing even RuO 2 /CF (η = 259 mV at 10 mA cm −2 ) under alkaline conditions. Notably, a high current density of 500 mA cm −2 is achieved with a relatively low overpotential of 390 mV, demonstrating the potential of CoS 2 -Cu x S/CF for high-current-density applications. Tafel plots (Figure 3b) highlight the favorable reaction kinetics of CoS 2 -Cu x S/CF, with a Tafel slope of 60.3 mV dec −1 , significantly lower than those of CoS 2 -Co 3 S 4 /CC (71.7 mV dec −1 ) and Cu x S/CF (96.7 mV dec −1 ), indicating accelerated charge transfer and reduced energy loss during OER. [36, 37] The catalytic performance of CoS 2 -Cu x S/CF is influenced by synthetic parameters such as the amount of Co(NO 3 ) 2 , hydrothermal time, and temperature. Optimization studies (Figure S7) reveal that using 1.5 mmol Co(NO 3 ) 2 achieves the best performance, with faster reaction kinetics and improved charge transfer (Figure S7b, S7c). Further investigations (Figure S8, S9) show that a hydrothermal time of 4 h and a temperature of 150 ℃ yield the optimal morphology and catalytic activity. The enhanced performance is attributed to the synergistic effects between CoS 2 and Cu x S, which improve interfacial electron transfer and facilitate dynamic surface reconstruction by reducing charge transfer resistance ( R ct ). Additional cyclic voltammetry (CV) analyses supporting these observations are shown in Figures S10-S12. As summarized in Figure 3c and Table S2, CoS 2 -Cu x S/CF ranks among the best-performing sulfide and copper-based OER catalysts reported. The double-layer capacitance ( C dl ) obtained from CV measurements (Figure 3d) indicates electrochemical surface area. [38] The C dl for CoS 2 -Cu x S/CF is 93.2 mF cm −2 , surpassing the comparison samples by several times, such as Cu x S/CF (28.6 mF cm −2 ), CoS 2 -Co 3 S 4 /CC (20.4 mF cm −2 ), and CF (19.7 mF cm −2 ). The electrochemical surface area (ECSA) is determined using C dl (Figure 3e). A specific capacitance of 1 cm 2 surface area is selected as 40 mF cm −2 under normal circumstances. [39] The electrochemical surface area (ECSA) is calculated to be 1560 cm 2 for CoS 2 -Cu x S/CF, nearly five times larger than that of Cu x S/CF (340 cm 2 ) (Figure 3e). The pearl-thread-like morphology is responsible for the expanded surface area, increasing active site exposure and enhancing catalyst-electrolyte interactions. [40] The larger specific surface increases the exposure of the interface in solution, which achieves higher density interfaces and facilitates the bonding of the active site. In order to demonstrate the intrinsic activity of CoS 2 -Cu x S/CF more efficiently, ECSA-normalized LSV curves are displayed in Figure 3e as well, which proves that CoS 2 -Cu x S/CF has the highest electrocatalytic performance and intrinsic activity for OER in alkaline environment. The turnover frequency (TOF) is derived from the results of inductively coupled plasma mass spectrometry (ICP−MS), invariably correlating with the intrinsic activity of electrocatalysts (Table S1). [41] As depicted in the Figure 3f, the TOF of CoS 2 -Cu x S/CF exhibits the most rapid increasing trend with applied voltage rises. When the applied voltage attains 259 mV, the TOF value of CoS 2 -Cu x S/CF is 0.03 s −1 , further demonstrating that the formation of CoS 2 -Cu x S interface improves the intrinsic activity. The Faradaic efficiency (FE) of the OER process is further calculated, representing the ratio of actual gas evolved to the theoretically (Figure 3g). [42] As a result, actual oxygen production and theoretical oxygen production exhibit an extremely high degree of fit. More than 10 mL O 2 are generated by 1 cm 2 of CoS 2 -Cu x S/CF within 30 min, which is close to the theoretical oxygen production. In particular, the high activity of CoS 2 -Cu x S/CF can be maintained for over 200 h at a current density of 100 mA cm −2 (Figure 3h), implying the extraordinary cycling stability of CoS 2 -Cu x S/CF. Figure 4 (a-b) TEM image of CoS 2 -Cu x S/CF after reaction. High-resolution XPS spectra of (c) Cu 2p (the inset shows Cu LMM Auger spectra) and (d) S 2p regions in CoS 2 -Cu x S/CF and Cu x S/CF after reaction. (e) Potential-dependent in situ Raman spectra of CoS 2 -Cu x S/CF at different potentials (vs. RHE). Nyquist plots for (f) CoS 2 -Cu x S/CF and (g) Cu x S/CF at different applied potentials (vs. RHE). (h) Variation trend of R ct under different potential for CoS 2 -Cu x S/CF and Cu x S/CF. The surface evolution of CoS 2 -Cu x S/CF during the OER process was investigated using transmission electron microscopy (TEM) after long-term stability testing. As shown in Figure S12, the reaction process induced significant alterations in the microscopic morphology of the catalyst surface. Elemental mapping (Figure S15) reveals a uniform distribution of Cu, Co, O, and S, while energy-dispersive X-ray (EDX) spectra (Figure S16) quantitatively confirm the elemental composition. Notably, the oxygen content increases significantly after the OER process, accompanied by a corresponding decrease in sulfur content, implying the partial transformation of sulfides into oxides. TEM analysis reveals lattice fringe spacings of 0.186 nm, corresponding to the (202) plane of CuO, confirming the formation of CuO. Additionally, spacings of 0.438 nm and 0.242 nm are assigned to the (003) and (101) planes of CoOOH, respectively, indicating the generation of CoOOH during OER. These findings are consistent with post-reaction XPS analysis (Figure 4c), where an increase in the Cu 2+ signal corroborates the formation of CuO. Importantly, residual sulfur signals were still detected by XPS (Figure 4d), suggesting incomplete transformation of Cu x S, consistent with the elemental mapping results. [43] In situ Raman spectroscopy was further employed to monitor structural evolution during OER. Compared to the dry state, Raman scattering peaks at 390 cm −1 weakened after immersion in alkaline electrolyte due to environmental changes. In addition, copper foam (CF) oxidizes readily upon exposure to water, leading to observable Cu-O vibrations at open-circuit potential (OCP). As shown in Figure 4e, characteristic Raman peaks at 270 cm −1 , 348 cm −1 , and 550 cm −1 correspond to Cu-O, Cu-S, and CoOOH, respectively. [23, 24, 44] With increasing applied potential, the intensity of the Cu-S peak gradually decreases, while the Cu-O peak intensifies, indicating progressive oxidation of Cu x S. Importantly, CoOOH formation becomes significant only after substantial CuO generation, suggesting that the disruption of the Cu-S bond and the formation of Cu-O bonds redistribute the local charge density, thereby facilitating the activation of Co sites into highly active CoOOH species. Combined analysis of these results confirms that a CoOOH-CuO-Cu x S heterointerface forms during OER process. CoS 2 and Cu x S are partially transformed into CoOOH and CuO, respectively, while unreacted Cu x S remains inside the catalyst. This hybrid structure benefits from the high conductivity of residual sulfides, lowering charge transfer resistance and enhancing reaction kinetics. In summary, the in situ generated CoOOH-CuO-Cu x S interface replaces the original sulfide phase, significantly boosting catalytic activity. [45] Electrochemical impedance spectroscopy (EIS) was performed to further investigate the dynamic evolution of active species on the catalyst surface. [46] In-situ EIS measurements are conducted at various potentials to further elucidate the role of Co sites in promoting the adsorption and desorption of oxygen-containing reactants. [47] Figure 4f and 5g present the Nyquist plots of CoS 2 -Cu x S/CF and Cu x S/CF at different potentials. As the potential increased, the charge transfer resistance ( R ct ) decreased significantly, indicating a notable acceleration in reaction kinetics. [48] Moreover, the charge transfer rate of CoS 2 -Cu x S/CF is consistently higher than that of Cu x S/CF, which can be attributed to the dynamic evolution of Co sites at the interfaces of the Cu x S and CoS 2 species. Figure 4h illustrates the decreasing trend of R ct between CoS 2 -Cu x S/CF and Cu x S/CF. Under low-potential conditions, the Co active sites exhibit enhanced adsorption of oxygen-containing intermediates. These intermediates are rapidly accumulated through introducing the Co sites, exciting the OER property of catalysts at a low potential. [49] Figure 5 (a) Optimized model configuration. (b) Charge density difference of CoOOH-CuO-Cu x S. (c) Cross-sectional diagram. (d) DOS for CoOOH-CuO-Cu x S and CoOOH. (e) Schematic representation of the d-band center as well as electronic interaction governing bond formation between the catalyst surface and adsorbate. (f) OER mechanism illustration of CoOOH-CuO-Cu x S (g) Gibbs free energy diagrams of CoOOH-CuO-Cu x S and CoOOH. To elucidate electronic interactions of key reaction intermediates at the interface, we modeled the system using density functional theory (DFT). [50] To align with system characterization, CoOOH-CuO-Cu x S is selected as the computational model, with CoOOH serving as the contrast sample. Figure 5a is introduced for the optimized model configuration. The differential charge density is analyzed in Figure 5b, with yellow region indicating the electron accumulation and green region representing the electron depletion. This suggests that there is localized charge accumulation near CoOOH and CuO regions. Significantly, charge aggregation at Cu sites is markedly weaker than that of Co sites, implying CuO regulates interfacial electron transfer. [51] This electronic coupling is further clarified in the two-dimensional charge density projection (Figure 5c), where blue region represents the electron accumulation, and the red region indicates the electron depletion. Density of states (DOS) calculations (Figure 5d) reveal enhanced electron density near the Fermi level for CoOOH-CuO-Cu x S compared to CoOOH, demonstrating that CoOOH-CuO interactions promote interfacial electron mobility and improve material conductivity. [52] The d-band center shifts from −1.27 eV (CoOOH) to −1.17 eV (CoOOH-CuO-Cu x S), indicating higher antibonding orbital occupancy above Fermi level and reduced bonding orbital occupancy below Fermi level (Figure 5e), which is consistent with weakened Co-O bonds that favor oxygen species desorption. [53] Figure 5f illustrates the four-electron OER pathway on CoOOH-CuO-Cu x S, where Co sites remain the primary adsorption centers. Hydroxide adsorption forms *OH intermediates on Co sites, followed by sequential deprotonation to *O and *OOH species, culminating in O 2 release. [54] Gibbs free energy (ΔG) analysis (Figure 5h) identifies the transition from *O to *OOH (ΔG 3 ) as the rate-determining step. CoOOH-CuO-Cu x S exhibits a significantly lower ΔG 3 (1.48 eV) compared to CoOOH (1.78 eV), which reduces energy barriers of *O to *OOH, further facilitating the formation of CoOOH. In summary, compared to single CoOOH, the in suit generated active CoOOH-CuO-Cu x S interfaces optimizes electronic structure and facilitates the desorption of oxygen-containing intermediates *O during the OER process, resulting in excellent OER performance. The excellent OER performance motivates us to apply the catalyst in overall water splitting. Electrochemical analyses revealed that the CoS 2 -Cu x S/CF (+) ||Pt/C (−) system demonstrated superior overall water splitting performance relative to the control in 1.0 M KOH. As shown in the polarization curve (Figure S17b), CoS 2 -Cu x S/CF (+) ||Pt/C (−) electrolyzer required only 1.62 V to achieve a current density of 100 mA cm −2 , substantially lower than the 1.82 V required for the RuO 2 (+) ||Pt/C (−) . Furthermore, the CoS 2 -Cu x S/CF (+) ||Pt/C (−) system exhibited competitive performance at 100 mA cm −2 compared with numerous reported electrocatalysts (Figure S17c, Table S3). As demonstrated in Figure S17d, CoS 2 -Cu x S/CF (+) ||Pt/C (−) system exhibits outstanding stability at a current density of 100 mA cm −2 for over 60 h, indicating that its certain potential for industrial applications. 3. Conclusion We developed a self-supported CoS 2 -Cu x S/CF electrocatalyst that undergoes dynamic surface reconstruction to form an active CoOOH-CuO-Cu x S interface under OER conditions. In situ and operando characterizations, supported by DFT calculations, reveal that the engineered interface enhances electronic coupling, optimizes *OOH adsorption, and reduces the rate-determining step barrier by 0.30 eV compared to pristine CoOOH. As a result, CoS 2 -Cu x S/CF delivers a low overpotential of 239 mV at 10 mA cm −2 , a high current density of 500 mA cm −2 at 390 mV, and long-term stability exceeding 200 hours. These findings underscore the significance of dynamic interface design in advancing non-noble-metal OER catalysts for sustainable water splitting applications. CRediT authorship contribution statement Heyang Liu: Writing – original draft, Methodology. Fengli Wei: Validation, Investigation. Linlin Huang: Methodology. Chenggong Niu: Validation. Zuyang Luo: Investigation. Tayirjan Taylor Isimjan: Writing – review & editing. Xiulin Yang: Writing – review & editing, Supervision. Conflict of Interest The authors declare no conflict of interest. Acknowledgements This work has been supported by the National Natural Science Foundation of China (no. 52363028, 21965005), Natural Science Foundation of Guangxi Province (2021GXNSFAA076001, 2018GXNSFAA294077), Guangxi Training Program of Innovation and Entrepreneurship for Undergraduates, (S202410602138). Appendix A. Supporting information Supplementary data associated with this article can be found in the online version at https://doi.org/10.1002/cjoc.2025.XXXX. References [1] Li, Q.; Luo, W.; Cui, X.; Shi, J., Rapid and In Situ Active Sites Regeneration for OER Activity Recovery and Greatly Prolonged Water-Splitting Performance. Angew. Chem. Int. 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Graphical Abstract A self-supported CoS 2 -Cu x S/CF electrocatalyst was developed, which undergoes dynamic surface reconstruction to form an active CoOOH-CuO-Cu x S interface under oxygen evolution reaction (OER) conditions. This electrocatalyst exhibits remarkable activity and long-term stability exceeding 200 hours, outperforming even RuO 2 /CF in alkaline conditions. In situ and operando characterizations, supported by density functional theory (DFT) calculations, reveal that the engineered interface enhances electronic coupling and optimizes *OOH adsorption, thereby facilitating superior OER performance. Supplementary Material File (image5.emf) Download 14.86 MB Information & Authors Information Version history V1 Version 1 24 July 2025 Copyright This work is licensed under a Non Exclusive No Reuse License. Keywords ： dynamic reconstruction density functional theory in situ characterization oxygen evolution reaction Authors Affiliations Heyang Liu Guangxi Normal University School of Chemistry and Pharmaceutical Sciences View all articles by this author Fengli Wei Guangxi Normal University School of Chemistry and Pharmaceutical Sciences View all articles by this author Linlin Huang Guangxi Normal University School of Chemistry and Pharmaceutical Sciences View all articles by this author Chenggong Niu Guangxi Normal University School of Chemistry and Pharmaceutical Sciences View all articles by this author Zuyang Luo Guangxi Normal University School of Chemistry and Pharmaceutical Sciences View all articles by this author Tayirjan Taylor Isimjan Saudi Basic Industries Corporation View all articles by this author Xiulin Yang 0000-0003-2642-4963 [email protected] Guangxi Normal University School of Chemistry and Pharmaceutical Sciences View all articles by this author Metrics & Citations Metrics Article Usage 224 views 143 downloads .FvxKWukQNSOunydq8rnd { width: 100px; } Citations Download citation Heyang Liu, Fengli Wei, Linlin Huang, et al. Unleashing OER Potential: Interface-Engineered CoS2/CuxS via Dynamic Surface Reconstruction. Authorea . 24 July 2025. DOI: https://doi.org/10.22541/au.175332441.16575068/v1 If you have the appropriate software installed, you can download article citation data to the citation manager of your choice. Simply select your manager software from the list below and click Download. For more information or tips please see 'Downloading to a citation manager' in the Help menu . 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