In the present study, ZrO2 co-doped with Gd3+/Sm3+ and Gd3+/Er3+ ions have been synthesized using Pechini method. Phase composition, morphology and photoluminescence properties of the synthesized phosphors were investigated by using X-ray powder diffraction (XRD), differential thermal analysis/thermal gravimetry (DTA/TG), scanning electron microscopy (SEM) and photoluminescence spectrofluorometer (PL). After heating at 1200 °C, XRD revealed that the phosphors were crystallized as monoclinic and tetragonal multiphases. SEM images indicated that the phosphors consist of fine and spherical grains with a size around 200 nm to 250 nm. Luminescence studies of these phosphors have been carried out on the emission and excitation, along with lifetime measurements.