In this study, the structure, morphology and electrochemical properties of olivine LiNixFel_xP04 (0.05 <= x <= 0.25) have been investigated by using XRD, SEM, and Raman spectroscopy techniques. The XRD results showed that the obtained NixFel_xP04 are pure and the x values are exactly 0.05; 0.10 and 0.15. The electrochemical properties of LiNixFel_xP04 (with x = 0.05; 0.10 and 0.15) from cyclic voltammetry in LiPF6/EC: DMC (1:1) showed the reversible oxydo-recdtuction peaks which prove that the intercalation of u'. The Randle-Sevcik equations showed better diffusion coefficients of Ni-doped materials in comparison with LiFeP04.