High voltage cathode composite LiNiVO4 was synthesized in a very pure state by a new inorganic synthetic procedure. The structural properties of this compound were characterized by X-ray diffraction and vibrational spectroscopies, Its suitability was tested by fabricating a lithium cell in non-aqueous media and the electrochemical parameters (i.e., cyclability, chemical diffusion coefficient of Li ions and enhancement factor) were studied.