Using Y2O3, Mn(CH3COO)2·4H2O as raw materials and glacial acetic acid as solvents, YMnxFe1-xO3 precursors (x= 0, 0.05, 0.1, 0.3, 0.5) have been prepared under 80°C water bath conditions. Perovskite YMnxFe1-xO3 samples were achieved after calcination over 900 °C for 4 h. Structure of the samples was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Ultraviolet obvious diffuse reflection(UV-vis DRS), and Field-emission scanning electron microscopy (FESEM). Photocatalytic activity of the samples was also investigated. Results showed that all the samples with stable perovskite structure had high light absorption in visible-light region, suggesting good visible light harvesting. SEM image showed that the samples were sponge-like and porous agglomerates. Photodecoloration activity of 100 mL Rhodamine B (10 mg/L) was 16~56 % under illumination for 150 min. Oxygen vacancies of the perovskite may explain the high activity of x = 0.1 sample.