The PbYO composites were prepared through a precipitation method and used for the degradation of methyl orange under visible-light irradiation. The PbYO complex photocatalysts were characterized by X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, N 2 adsorption–desorption, and terephthalic acid photoluminescence (TA-PL) probing technique. The results indicated that the photodegradation of methyl orange was significantly enhanced in the presence of PbYO complex oxide when compared with BiYO 3 . The calcination temperature was found to have a significant effect on the photocatalytic activity of PbYO composites. Specifically, PbYO calcined at 800°C had a considerably larger surface area, lower reflectance intensity, higher formation rate of free ·OH radicals and showed higher photocatalytic activity.