Abstract Nanocrystallines lead molybdate and lead tungstate were successfully prepared by microwave irradiation method. The products were characterized by XRD, Raman spectroscopy, TEM and luminescence spectroscopy. The phase of products were detected by XRD and was in accordance with that of the XRD simulation using CaRIne Version 3.1 program. TEM showed the particle sizes of 15–50 nm for PbMoO 4 and 12–32 nm for PbWO 4. Their photoluminescent spectra were decomposed to four individual Gaussian components in blue and green wavelength range for PbMoO 4 and three individual Gaussian components in blue wavelength range for PbWO 4. These photoluminescent features could be interpreted by Jahn–Teller splitting effect on [MO 4] 2− (M Ma and W) tetrahedrons.