| Summary: | Defect-rich photocatalytic materials with excellent charge transfer properties are very popular. Herein, Sm-doped CeO<sub>2</sub> nanorods were annealed in a N<sub>2</sub> atmosphere to obtain the defective Sm-doped CeO<sub>2</sub> photocatalysts (Vo–Sm–CeO<sub>2</sub>). The morphology and structure of Vo–Sm–CeO<sub>2</sub> were systematically characterized. The Vo–Sm–CeO<sub>2</sub> nanorods demonstrated an excellent photodegradation performance of methyl blue under visible light irradiation compared to CeO<sub>2</sub> nanorods and Sm–CeO<sub>2</sub>. Reactive oxygen species including OH, ·O<sub>2</sub><sup>−</sup>, and h<sup>+</sup> were confirmed to play a pivotal role in the removal of pollutants via electron spin resonance spectroscopy. Doping Sm enhances the conductivity of CeO<sub>2</sub> nanorods, benefiting photogenerated electrons being removed from the surface reactive sites, resulting in the superior performance.
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