Abstract: In the present work, Synthesis, characterization and electrochemical properties of NaFePO4 and NaCoPO4 have been presented. The materials were synthesized through a solid state reaction by reacting stoichiometric amounts of reaction precursors in the presence of flowing argon. The results of X-ray diffraction confirm that the synthesized phases are well crystalline and pure. The X-ray diffraction spectra of the both materials were refined considering Pnma space group by using Full Proof soft ware. SEM images show that NaFePO4 has relatively smaller particle size (250 nm) as compared to NaCoPO4 (2.5 關m).The results of electrochemical tests indicate that both the material are nearly inactive at room temperature because of slow sodium diffusion kinetics which can be attributed to obstructed occupancy M1 and M2 sites by Na and Fe/Co unlike olivine LiFePO4/ LiCoPO4.