YVO4 micro-rods were synthesized using a high-energy ball milling (HEB) method without other chemicals or solvents. The powder samples were sintered in air at 350, 400, 450, 500, 550 and 600 degrees C for 5 h to form the polycrystalline YVO4 micro-rods. The effects of the processing parameters on the crystallinity, morphology and structure were examined by X-ray diffraction, field emission-scanning electron microscopy and TEM. The rate of YVO4 rod formation from NaYV2O7 increased with increasing sintering temperature. The luminescent properties were determined from their excitation and emission spectra. Overall, high-energy ball milling (HEB) is a promising method for preparing YVO4 with a rod-like morphology. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.104206jes] All rights reserved.