Publication date: 22nd July 2026
Electrochemical Water Splitting (EWS) is currently one of the most suitable processes for “green” H2 production since it can be performed with the surplus of electricity coming from renewable sources. The limiting step of the overall EWS process is the Oxygen Evolution Reaction (OER), which involves a complex transfer of four electrons leading to a sluggish kinetics [1]. Nowadays, the most efficient catalysts for OER are based on rare and expensive metals, like iridium and ruthenium. Materials containing less expensive and more earth-abundant 3d-metals are currently emerging as an alternative for OER catalysis in alkaline media [2].
We focused our research on a low crystalline nickel(II)-based coordination polymer (Ni-C) synthesized using NiBr2·6H2O and a benzenedicarboxylate ligand (C2-) functionalized with a chiral side chain (H2C = 2-[(2S)-2-methylbutoxy]benzene-1,4-dicarboxylic acid). The electrochemical behavior of Ni-C was studied by long-term CV cycling while its structural evolution during OER catalysis was followed by X-ray absorption spectroscopy (XAS) in-operando experiments. Here, the bulk sensitive Ni K-edge, and the surface sensitive Ni L-edge and O K-edge spectra were collected. The in-operando experiments, supported also by UV-Vis, FT-IR, and PXRD ex-situ measurements, suggest that Ni-C undergoes a significant structural reconstruction during OER catalysis in 0.1 M KOH. In particular, the leaching of the organic ligand from the framework begins when Ni-C comes in contact with the alkaline medium and reconstructs into β-Ni(OH)2-like phases. At OER catalytic potentials it is possible to see the reversible formation of γ-NiOOH-like phases. Interestingly, even if Ni-C undergoes an almost fully reconstruction into these inorganic phases during the experiments, the catalytic current is enhanced with respect to that measured starting from synthetic β-Ni(OH)2, confirming that the organic ligand has a pivotal role in OER catalysis.
This project has been funded under: the National Recovery and Resilience Plan (NRRP), Mission 4 Component 2, Investment 1.5 – NextGenerationEU, Call for tender n. 3277 dated 30/12/2021, Award Number: 0001052 dated 23/06/2022; Progetto P20227P7WZ – CUP E53D23015850001 - NRRP Mission 4 Component 2, Investment 1.1 – NextGenerationEU e PRIN – NextGenerationEU - rif. D.D. N. 1409 MUR 14/09/2022; Fondazione di Modena under the grant FAR Mission Oriented 2022 – FOMO line, CUP: E93C22000800007; M.C. and R.B. acknowledge Regione Emilia-Romagna, “Territorio: transizione tecnologica, culturale, economica e sociale verso la sostenibilità” - PR FSE+ 2021/2027 – CUP: E83C24000320002.
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