Harnessing oxygen redox reactions is an intriguing route to increasing capacity in Li-ion batteries (LIBs). Despite numerous experimental and theoretical attempts to unravel the mechanism of oxygen redox behavior, the electronic origin of oxygen activities in energy storage of Li-rich LIB materials remains under intense debate. In this work, the onset of oxygen activity was examined using a Li-rich material that has been reported to exhibit oxygen redox, namely, LiFeO. By comparing experimental measurements and first-principles Bethe-Salpeter equation calculations of oxygen K-edge X-ray absorption spectra (XAS), it was found that experimentally-observed changes in XAS originate from the nonbonding oxygen states in cation-disordered delithiated LiFeO, and the spectral features of oxygen dimers were also determined. This combined experimental and theoretical study offers an effective approach to disentangle the intertwined signals in XAS and can be further utilized in broader contexts for characterizing other energy storage and conversion materials.
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