A newly-developed hydrothermal process has been used to prepare LiNiVO4 by reacting nickel acetate, LiOH . H2O, and NH4VO3 in isopropanol. LiNiVO4 powders with particle size ranging from 0.2 to 0.3 mu m were successfully prepared at as low as 200 degrees C in 2 h. Compared to the solid state reaction processes, the hydrothermal process greatly reduced the temperature for preparing LiNiVO4. The subsequent calcination at above 500 degrees C significantly enhanced the crystallinity of LiNiVO4 powder.