Well-crystallized zinc vanadium oxide Zn 3 (VO 4 ) 2 micro-particles were successfully synthesized by annealing Zn 3 (OH) 2 V 2 O 7 ·nH 2 O at 600°C for 10h in N 2 atmosphere. X-ray diffraction pattern of the sample is in agreement with the standard pattern of orthorhombic Zn 3 (VO 4 ) 2 . Scanning electron microscopy (SEM) image reveals that the as-synthesized particles are about 2μm in mean diameter. The structure and composition of the as-synthesized sample were further characterized by Fourier transform infrared spectra (FTIR), Raman spectrum, and X-ray photoelectron spectroscopy (XPS). Furthermore, the photoluminescence properties of the as-synthesized Zn 3 (VO 4 ) 2 were characterized via room temperature photoluminescence (PL) measurement, which exhibit excellent visible light emission ranging from 500 to 700nm.