Calcium aluminate, CaAl 2 O 4 is efficient and well known host material for inorganic phosphors. Although this host structure is mostly doped with Eu 2+ , different types of rare earth ions have also been studied. In this study, attention was drawn to CaAl 2 O 4 type phosphors doped with Dy 3+ and Sm 3+ at different concentrations. Ca 1-x Al 2 O 4 : Dy 3+x (x= 0.008, 0.012, 0.02, 0.03) and Ca 1-y Al 2 O 4 : Sm 3+ y (y= 0.008, 0.012, 0.02, 0.03) phosphors were synthesized as powder samples through the solid-state reaction method. After heat treatments, monoclinic CaAl 2 O 4 structure was confirmed for all rare earth doped samples by the XRD analysis. PL characteristics of samples depend on activator ion. The PL emission spectra of Dy 3+ doped powder samples show two strong bands at 484 nm and 577 nm which are attributed to a typical 4 F 9/2 → 6 H 15/2 and 4 F 9/2 → 6 H 13/2 transitions of Dy 3+ ions. Sm 3+ activated phosphors have the emission peaks at 565 nm, 604 nm, 649 nm, and 712 nm which are assigned to Sm 3+ transitions: 4