Praseodymium-doped ZrO2 photoluminescent (PL) powders have been prepared by a co-precipitation process. Different doping concentrations in the start mixture and annealing temperatures for the precipitated were studied. It is observed that the crystalline structure and the crystallinity of the powders depend on the annealing temperature. For temperatures higher than 750°C, the material presents the monoclinic phase with an average crystalline grain size of 100 nm. Measurements on photoluminescence show excitation and emission spectra. For an excitation wavelength of 294 nm, all the PL emission spectra show the peaks located at 490, 505, 536, 567, 589, 616, 645, 725 and 745 nm associated with 3P0 → 3H4, 3P0 → 3H4, 3P1 → 3H5, 3P0 → 3H5, 3P0 → 3H5, 3P0 → 3H6, 3P0 → 3F2, 3P0 → 3F3 and 3P0 → 3F4 transitions in the Pr3 + ion, respectively.