LAUSR

Transition metal‐doped CeO2 (MCeOx) is of great importance in industrial catalysis. However, current synthetic methods often result in the separation of MOx phases, which significantly decreases their catalytic activity. Toward this end, the chemistry of mechanochemical redox was introduced to prepare Ce1‐xMnxO2‐δ catalyst. The redox behavior between MnO4− and Ce3+ could in situ produces atomically dispersed Ce1‐xMnxO2‐δ solid solution without calcination. Moreover, the mechanochemical synthesis endows Ce1‐xMnxO2‐δ a surface area (302 m2/g) that is much higher than the counterparts prepared by traditional methods, such as co‐precipitation method (66 m2/g) CTAB‐assisted precipitation method (122 m2/g) and sol‐gel method (136 m2/g). Importantly, the well dispersed heteroatoms and high porosity afford doped ceria excellent activity and stability during CO oxidation. The reaction mechanism was finally explored by DFT calculation, which reveals that Mn and Cu dopants facilitate electron transfer and oxygen releasing.