Dual-shell hollow nanospheres NiCo2S4@CoS2/MoS2: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation

doi:10.1016/S1872-2067(25)64727-9

Abstract

Abstract:

Activating both metal and lattice oxygen sites for efficient oxygen evolution reactions (OER) is a critical challenge. This study pioneers a novel approach, employing cobalt-nickel glycerate solid spheres (CoNi-G SSs) as self-sacrificial templates to synthesize yolk-shell structured CoNi-G SSs@ZIF-67 nanospheres. The derived NiCo₂S₄@CoS₂/MoS₂ double-shelled hollow nanospheres integrate the adsorbate evolution mechanism (AEM) and lattice oxygen mechanism (LOM), enabling synergistic dual catalytic pathways. Nickel modulation facilitates active species reconstruction in NiCo₂S₄, enhancing lattice oxygen activity and optimizing the LOM pathway. Characterization results indicate that anode activation triggered the redox processes of metal and lattice oxygen sites, involving the formation and re-filling of oxygen vacancies. Additionally, the CoS₂/MoS₂ heterostructure enhances the AEM pathway, as supported by density functional theory calculations, which demonstrate optimized adsorption of intermediates for both hydrogen evolution reaction and OER. The assembled anion exchange membrane water splitting device can deliver a catalytic current of 500 mA cm^-2 at 1.74 V under commercial catalytic operating conditions (1 mol L^-1 KOH) for 150 h, with negligible degradation. This work provides important insights into the understanding of OER mechanisms and the design of high-performance water-splitting electrocatalysts, while also opening new avenues for developing multifunctional materials with multi-shell structures.

Key words: Adsorbate evolution mechanism, Lattice oxygen mechanism, Water-splitting, ZIF-67, NiCo₂S₄@CoS₂/MoS₂, Dual-shell hollow nanospheres

Yang Chen, Yu Tang, Leiyun Han, Jiayan Liu, Yingjie Hua, Xudong Zhao, Xiaoyang Liu. Dual-shell hollow nanospheres NiCo₂S₄@CoS₂/MoS₂: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation[J]. Chinese Journal of Catalysis, 2025, 74: 394-410.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64727-9

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Figures/Tables 11

Fig. 1. Schematic illustration of formation mechanism for NiCo2S4@CoS2/MoS2 DSHSs and NiCo2S4@CoS2 DSHSs.

Fig. 2. (a) XRD patterns of CoNi-G SSs (A) and CoNi-G SSs@ZIF-67 YSSs (B). (b) XRD patterns of NiCo2S4@CoS2/MoS2 DSHSs (A), NiCo2S4@CoS2 DSHSs (B), and NiCo2S4 YSSs (C).

Fig. 3. SEM (a-c) and TEM (d-f) images of CoNi-G SSs (a,d), CoNi-G SSs@ZIF-67 YSSs (b,e), and NiCo2S4@CoS2/MoSx -2/1 DSHSs (c,f).

Fig. 4. (a-c) SEM images of S-NiCoMo-2. (d,e) TEM images of S-NiCoMo-2. (f) HRTEM image of S-NiCoMo-2. (g) elemental mapping images of S-NiCoMo-2.

Fig. 5. (a) The XPS patterns of S-NiCoMo-2. High-resolution XPS spectra of Co 2p (b), Ni 2p (c); Mo 3d (d), and S 2p (e) of S-NiCoMo-2. (f) N2 adsorption-desorption isotherm measurements.

Fig. 6. Polarization curves (a), histograms of overpotentials at different current densities (b), and corresponding Tafel slopes (c) of S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs towards HER. Polarization curves (d), histograms of overpotentials at different current densities (e) and corresponding Tafel slopes (f) of S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs towards OER. (g, h) Cdl values of S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs towards HER and OER were obtained from current density versus scan rates. (i) Nyquist plots and equivalent circuit for S-NiCoMo-2, S-NiCoMo-4, S-NiCoMo-0, and NiCo2S4 YSSs.

Fig. 7. (a) OER polarization curves of S-NiCoMo-4 and S-NiCoMo-2 in 1 mol L-1 KOH and 1 mol L-1 TMAOH, respectively. In situ Raman spectra of S-NiCoMo-4 (b) and S-CoMo-4 (c) during the applied potential range from OCP to 1.7 V vs. RHE. (d, e) show the DEMS measurements of the 32O2, 34O2, and 36O2 signals from the reaction products of 18O-labeled S-NiCoMo-4 and S-CoMo-4, respectively. (f) in situ Raman spectroscopy of HER on S-NiCoMo-4 at different potentials immediately after OER tests. (g) mechanism diagram of synergistic catalysis under AEM and LOM pathways.

Fig. 8. (a) Chronopotentiometry curves recorded at 10 mA cm-2 of S-NiCoMo-2 towards HER and S-NiCoMo-4 towards OER in 1.0 mol L-1 KOH solution. (b) Polarization curves at 10 mA cm-2 of S-NiCoMo-4||S-NiCoMo-2 and Pt/C||RuO2 couples towards overall water electrolysis. (c) Experimental and theoretical values of gas production for S-NiCoMo-4||S-NiCoMo-2. Electrolyte 1 mol L-1 KOH. (d) a drainage device fabricated using an H-type electrolytic cell. (e) Chronopotentiometry curves at 10 mA cm-2 of S-NiCoMo-2||S-NiCoMo-4 and Pt/C||RuO2 couples towards overall water electrolysis. (f) Comparison of the water electrolysis voltage obtained at a current density of 10 mA cm-2 from previous research and that achieved using our NiCo2S4@CoS2/MoS2 DSHSs catalyst in an alkaline medium. Optical image of the AEM water splitting device (g) and schematic diagram (h). (i) Stability testing of the S-NiCoMo-4|| S-NiCoMo-2 electrode pairs in EWS using the AEM water splitting device (constant current charging, current density = 0.5 A cm-2) in 1 mol L-1 KOH.

Fig. 9. (a) DFT calculated PDOS of isolated (002) MoS2 nanoparticles, (112) CoS2 surface and CoS2/MoS2 heterointerface. (b) Charge density difference at the CoS2/MoS2 heterointerface. (c) Band diagrams of semiconductor MoS2 and metallic CoS2 before and after the formation of Mott-Schottky interactions. (d) Schematic of the CoS2/MoS2 heterointerface illustrating electron transfer at the heterojunction.

Fig. 10. (a) Optimized crystal structures of (002) MoS2 nanoparticle, (112) CoS2 and CoS2/MoS2 heterointerface. (b-d) Gibbs free energy diagrams for HER at different H adsorption sites on the surfaces of MoS2, CoS2, and CoS2/MoS2, respectively. Insets in (b-d) represent the considered H adsorption sites on MoS2, CoS2, and CoS2/MoS2, respectively.

Fig. 11. (a) Water adsorption sites for MoS2, CoS2, and CoS2/MoS2. (b) Water adsorption energy on the MoS2, CoS2, and CoS2/MoS2 systems (Adsorption sites: Mo-top (MoS2); Mo-edge (MoS2); Co (CoS2); Co (CoS2/MoS2); and Mo (CoS2/MoS2)). Four proton transfer mechanisms of OER on the Co binding site on the surface of CoS2 under alkaline conditions (c) and the corresponding Gibbs free energy diagrams (e) for OER. Four proton transfer mechanisms of the proposed OER on the surface Co binding site of CoS2/MoS2 under alkaline conditions (d) and the corresponding Gibbs free energy diagrams for OER (f).

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Dual-shell hollow nanospheres NiCo₂S₄@CoS₂/MoS₂: Enhancing catalytic activity for oxygen evolution reaction and achieving water splitting via the unique synergistic effects of mechanisms of adsorption-desorption and lattice oxygen oxidation

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