This paper presents Photoluminescence studies of Lanthanum, Terbium, doped Calcium Aluminate nanophosphors (CaAl2O4: La, Tb) prepared by sol-gel method. These phosphors has been characterized by powder X-ray diffraction, scanning electron microscope, Diffuse reflectance spectrometer. Optical properties were studied by photoluminescence spectra. XRD analysis confirmed, the monoclinic structure, the particle size was found to be 27 nm and 31 nm and is determined by (Williamson and Hall plot) W-H plot method. PL emission is obtained at 395nm, 535 nm corresponds to blue, green region of the spectrum for 800 nm excitation. Photoluminescence studies of the prepared phosphors showed near band edge emission and green emission.