Beschreibung:
<jats:title>Abstract</jats:title><jats:p>The structural evolution with alkali ion insertion, and the subsequent thermal evolution of the alkali‐ion inserted ReO<jats:sub>3</jats:sub> electrodes are shown by employing <jats:italic>in situ</jats:italic> and <jats:italic>ex situ</jats:italic> synchrotron X‐ray diffraction (XRD). During Na and K insertion, there is a combination of intercalation into ReO<jats:sub>3</jats:sub> and a two‐phase reaction. Interestingly in the case of Li insertion, a more complex evolution is noted, which suggests a conversion reaction takes place at deep discharge (insertion). Following these ion insertion studies, extracted electrodes at various states of discharge (kinetically determined) were examined with variable temperature XRD. The thermal evolution of the A<jats:sub>x</jats:sub>ReO<jats:sub>3</jats:sub> phases, where A=Li, Na, or K, are significantly modified from the parent ReO<jats:sub>3</jats:sub> thermal evolution. This shows the impact of alkali‐ion insertion on the thermal properties of ReO<jats:sub>3</jats:sub>.</jats:p>