: Ultrafine M 5 (PO 4 ) 3 F:Dy 3+ (M = Ca, Ba) phosphors were prepared via combustion process using metal nitrates as precursors. The formation of crystalline phosphate was confirmed by X-ray diffraction pattern. The PL excitation spectra show the excitation peaks observed at 250 to 400 nm due to f → f transition of Dy 3+ ion, which are useful for solid-state lighting purpose (mercury free excitation). The PL emission of Dy 3+ ion by 348 nm excitation gave an emission at 489 nm (blue), 582 nm (yellow) and 675 nm (red). All the characteristics of BYR emissions like BGR indicate that Dy doped Ca 5 (PO 4 ) 3 F and Ba 5 (PO 4 ) 3 F phosphors are good candidates that can be applied in solid-state lighting phosphor (mercury free excited lamp phosphor) and white light LED.