Direct Identification of O─O Bond Formation Through Three‐Step Oxidation During Water Splitting by Operando Soft X‐ray Absorption Spectroscopy (Adv. Sci. 40/2024)

Direct Identification of O–O Bond Formation In article number 2401236, Wu-Ching Chou, Shuangyin Wang, Zhiwei Hu, Chung-Li Dong, and co-workers report the first direct observation of O–O bond formation during the oxygen evolution reaction using operando soft-XAS and Raman spectroscopy on layered double hydroxides intercalated with [Cr(C2O4)3]3−. The findings elucidate a stepwise oxidation process culminating in the formation of O–O bond and O2 evolution, highlighting the crucial role of anionic redox in facilitating water splitting efficiency.