LiNiVO4 nano-crystallites were prepared by the polymerized complex method using Li2CO3, Ni(CH3COO)(2)center dot 4H(2)O and NH4VO3 as starting reagents and malic acid as a complexing agent. With the subsequent calcination at 450 degrees C, the powder analyzed by XRD, FTIR, Raman, electron diffraction, SEM and TEM techniques was found to be inverse spinel LiNiVO4 with similar to 20 nm in diameter. TGA shows continuous weight loss at 40-450 degrees C due to the evaporation and decomposition processes. Above 450 degrees C, weight percent tended to be constant. In addition, formation mechanism of the purified LiNiVO4 was proposed to relate with the experimental results.