Considering energy-related technologies including rechargeable batteries and water electrolysis, effective catalytic materials play a crucial role in the rise and unceasing development. Metal-organic frameworks (MOFs) have drawn attention due to their abundant and identical catalytic sites along the periodic network with tunable catalytic functionality and stability. Herein, structural information, catalytic sites, and their corresponding mechanistic pathways have been investigated by employing synchrotron-based X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS). The framework stability, the accessible active sites related to pre-designed metal clusters, the alteration of oxidation state of, and the coordination geometry around the active metal centers evolving along the electrochemical oxygen evolution reaction (OER) are thoroughly revealed. In addition, aqueous zinc-ion batteries (AZIBs) are promising energy storage systems due to their cost-effectiveness and eco-friendliness. However, there are some limitations restricting their practical utilizations such as the high activity of water leading to Zn corrosion and hydrogen evolution, along with the formation of dendrites on the Zn surface during repeated charge–discharge cycles. To limit parasitic side reactions, an artificial solid electrolyte interphase (ASEI) protective layer made of a covalent organic framework (COFs) is an effective strategy. Herein, grazing-incidence XAS was employed to specifically characterize the Zn speciation on the electrode surface. According to XAS results, the protective COF-ASEI layer can retard the coordination of water at the electrolyte–Zn interface, improve Zn plating/stripping kinetics, and increase the stability of the Zn anode. This presentation highlights the significance of synchrotron characterizations in energy-related technologies.
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