The photoluminescence (PL) phenomena of two kinds of zirconia powders prepared with industrial-grade reagents and analytical-grade reagents, respectively, have been studied through fluorescence spectrophotometry. The PL intensity increases with the elevation of heat-treatment temperature T, The visibility of the former is higher than that of the latter. Under the same excitation condition the emission peaks exhibit an obvious "blue shift" as treatment temperature decreases, especially between 400 and 600 degreesC. The shift of the latter is larger than that of the former. TEM, SAXS, XRD and chemical analysis were used to determine particle size, phase and chemical composition of the samples, respectively. In conclusion, the PL phenomena of zirconia nanometer powders are always accompanied by the monoclinic microstructure" the increase of PL intensity with elevation of treatment temperature is related to their crystallinity, the PL intensity difference of both kinds of powders arises from CaO and MgO rather than Cl content; the "blue shift" of emission peaks as T, decreased should be related to "equivalent particle size". (C) 2003 Elsevier B.V. All rights reserved.