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Using citric acid (C6H8O7·H2O), samarium nitrate (Sm(NO3)3·6H2O) and cobalt nitrate (Co(NO3)3·6H2O) as main raw materials, the SmCoO3 samples were successfully prepared by sol-gel method. The prepared samples were characterized by thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray diffractometer (XRD), scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FT-IR). Using azo dye methyl orange solution as the simulated sewage, the photocatalytic activity of SmCoO3 samples was explored at different synthesis temperatures and illumination times. The experimental results show that pure SmCoO3 samples can be prepared at a calcination temperature of 600 °C to 1000 °C. Under ultraviolet light conditions, the sample of SmCoO3 calcined at 800 °C has the best photocatalytic activity. When illumination times is 120 min, the degradation rate of methyl orange of 10 mg/L can reach more than 97%, and SmCoO3 shows good photocatalytic performance. [ABSTRACT FROM AUTHOR]