LiOH·H2O, Ni(CH3COO)2·4H2O and NH4VO3 were used to synthesize nano-crystalline LiNiVO4 by hydrothermal process in deionized water at 150 °C for 2 h and subsequent calcination at 300-600 °C for 6 h. By using an X-ray diffractometer (XRD), a transmission electron microscope (TEM) and a selected area electron diffraction (SAED) method, nano-crystalline LiNiVO4 with inverse spinel structure was detected. The stretching vibration of VO4 tetrahedrons analyzed by a Fourier transform infrared spectrometer (FTIR) was split into three bands at 661, 746 and 835 cm- 1, and that analyzed by a Raman spectrometer was detected at 823.9 and 787.7 cm- 1. The thermogravimetric and differential thermal analyses (TGA and DTA) show two discrete weight losses at 25-117 °C and 117-600 °C and four endothermic peaks at 84, 145, 202 and 372 °C, corresponding to the evaporation of water and the decomposition of inorganic and organic compounds. © 2006 Elsevier B.V. All rights reserved.