PbMoO4 and PbWO4 were successfully synthesized by microwave radiation using different lead salts (acetate, chloride, nitrate and sulfate) and Na2MO4 (M = Mo, W) in propylene glycol. The products were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM, TEM), Fourier transform infrared (FT-IR), Raman spectroscopy and photoluminescence (PL) spectroscopy. In this research, morphologies, crystallization and photoluminescence of the products were influenced by the kinetics of anions, including the detection of M–O (M = Mo, W) stretching modes in the (MO4)2 tetrahedrons. Photoluminescence of PbMoO4 synthesized from Pb(NO3)2 and of PbWO4 synthesized from PbCl2 showed the strongest blue emission due to the electronic diffusion in tetrahedrons at room temperature.
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