High‐Resolution X‐ray Absorption and Emission Spectroscopy for Detailed Analysis of New CO2 Methanation Catalysts <jats:title>Abstract</jats:title><jats:p>A new approach for the characterization of CO<jats:sub>2</jats:sub> methanation catalysts prepared by thermal decomposition of a nickel MOF by hard X‐ray photon‐in/photon‐out spectroscopy in form of high energy resolution fluorescence detected X‐ray absorption near edge structure spectroscopy (HERFD‐XANES) and valence‐to‐core X‐ray emission (VtC‐XES) is presented. In contrast to conventional X‐ray absorption spectroscopy, the increased resolution of both methods allows a more precise phase determination of the final catalyst, which is influenced by the conditions during MOF decomposition.</jats:p> Wiley