Er3+doped SrMoO4(SrMoO4:Er3+) and Er3+/Yb3+co-doped SrMoO4(SrMoO4:Er3+/Yb3+) particles were successfully synthesized by a cyclic microwave-assisted metathetic (MAM) route followed by heat treatment. The microstructures exhibited well-defined and homogeneous morphology with particles sizes of 100500 nm. With excitation at 980 nm, SrMoO4:Er3+and SrMoO4:Er3+/Yb3+particles exhibited a strong 525-nm emission band and a weak 550-nm emission band in the green region and a weak 655-nm emission band in the red region. The Raman spectra of SrMoO4:Er3+and SrMoO4:Er3+/Yb3+particles indicated the detection of additional strong peaks at both higher frequencies (564, 524, 456, and 403 cm-1) and lower frequencies (294, 251, and 220 cm-1).