Metal-organic frameworks (MOFs) derived materials are extensively utilized in wastewater treatment owing to their remarkable catalytic efficacy and durability. This study exploited iron-cerium-based bimetallic metal-organic framework (FeCe-MOF) as a sacrificial template, which was subsequently calcined at 700 °C to produce an iron-cerium-based bimetallic carbon nanospheres (FeCe@C). The FeCe@C has active sites of bimetallic Fe and Ce derivatives, demonstrating exceptional activation efficiency for persulfate, resulting in approximately 98.2 % elimination of tetracycline hydrochloride (TCH) within 120 min. This removal rate markedly exceeds that of the individual iron-based carbon nanospheres (Fe@C) (53.6 %) and cerium-based carbon nanospheres (Ce@C) (78.3 %). Characterization results, including X-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR), demonstrate that the Fe and Ce composite induces coordination unsaturation at the metal centers, leading to the formation of oxygen vacancies and an increase in active reaction sites. Additionally, radical quenching, EPR and electrochemical experiments demonstrate that radical (OH, O