Abstract MMoO4 (M=Ca, Ba) particles were synthesized by a metathetic reaction in ethylene glycol assisted by cyclic microwave irradiation followed by further heat-treatment. The MMoO4 (M=Ca, Ba) particles were well crystallized after heat-treatment at 400–600°C for 3h. The microstructures exhibited fine morphologies with sizes of 0.5–1μm and 1.5–2μm for the CaMoO4 and BaMoO4 particles, respectively. The synthesized MMoO4 (M=Ca, Ba) particles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The optical properties were examined by photoluminescence emission and Raman spectroscopy.