Zr0.99Gd0.01O2, Zr0.98Gd0.01Dy0.01O2 and Zr0.98Gd0.01Yb0.1O2 phosphors were synthesized by Pechini method at 1200 °C for 12 h in air. The phosphors were characterized by using X-ray powder diffraction (XRD), differential thermal analysis/thermal gravimetry (DTA/TG), scanning electron microscopy (SEM) and photoluminescence spectrofluorometer (PL). X-ray powder diffraction studies showed that the phosphors were crystallized as monoclinic and tetragonal multiphases. The particle size of the phosphors after heat treatment at 1200 °C was found to be of 200 nm to 250 nm. Luminescence studies on these phosphors have been carried out on the emission and excitation, along with lifetime measurements. The results of emission analysis indicate that the phosphors are expected to find potential applications as new optical materials.