“…X-ray photoelectron spectroscopy (XPS) measurements were carried out to investigate the elemental states in FeO x /NF before and after electrochemical conversion reaction. The Li 1s and Na 1s signals located at ≈55.5 eV and ≈1069.7 eV, respectively, confirm the intercalation of Li and Na ions into FeO x /NF-Li and FeO x /NF-Na during electrochemical conversion reaction (Figure a,b). − As shown in Figure c, the Fe 2p 3/2 and Fe 2p 1/2 peaks located at ≈724.6 eV and ≈711.3 eV could be deconvoluted into two components assigned to Fe 3+ and Fe 2+ . , Notably, the molar ratio of Fe 2+ /Fe 3+ for FeO x /NF-Li (FeO x /NF-Na) is higher than that for FeO x /NF, which is probably attributed to the electron donation from the created oxygen vacancies (Vo) during electrochemical conversion reaction . As observed in the XPS O 1s spectrum of FeO x /NF (Figure d), the peaks with binding energies at 530.1, 531.4, 532.9, and 534.2 eV are attributed to the metal–oxygen (M–O), metal-hydroxyls (M–OH), Vo, and physically adsorbed water, respectively. − One will note that the content of Vo increases in the order of FeO x /NF < FeO x /NF-Na < FeO x /NF-Li, indicating that more Vo are introduced into FeO x /NF by Li intercalation than by Na intercalation.…”