Olivine-type LiNiPO 4 has been considered as a most competitive positive electrode active material for lithium-ion batteries. In the present paper, the LiNiPO 4 and Co-doped LiNi 0.5 Co 0.5 PO 4 are synthesized by solid-state reaction method under air atmosphere. All the X-ray diffraction peaks of both the compounds are indexed and it is found that the samples are well crystallized in orthorhombic olivine structure belonging to the space group Pnma. The crystallite size is calculated from the Scherrer formula and it is found to be 6.918 and 4.818 nm for pure and doped samples, respectively. The surface morphology and grain sizes of the materials are investigated through scanning electron microscope. Presence of preferred local cation environment is understood from Fourier transform infrared spectroscopy (FTIR) studies. The conductivity and dielectric analysis of the samples are carried out at different temperatures and frequencies using the complex impedance spectroscopy technique. The electrical conductivity of LiNi 0.5 Co 0.5 PO 4 is higher than that of pure LiNiPO 4 .
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