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Herein, we suggest a novel chemical precipitation method to prepare different concentrations (0.05–0.25 M) of cobalt doped Bi2O3 nanoparticles. The prepared products exhibit excellent structural and optical properties. The influence of doping on the morphology of Bi2O3 was analyzed by FE-SEM and confirmed by HR-TEM. Furthermore, the photocatalytic activities of the samples were studied in the degradation of methylene blue under visible light irradiation. Compared to bare Bi2O3, 3% of cobalt doped Bi2O3 showed the highest degradation in 135 min of irradiation. Keywords: Cobalt, Bismuth oxide, HR-ETM, Photocatalytic, Methylene blue