NaFePO4, which is analogue to LiFePO4, has been expected to show similar properties as LiFePO4 that has a good cycle stability and excellent electrochemical performances. Here we report the synthesis of NaFePO4 via sol-gel method and the structural study of NaFePO4 as a cathode material for sodium-ion battery (SIB). The as-synthesized NaFePO4 samples were calcined under air and argon atmosphere at the constant holding time of 10 hours with the variation of calcined temperature. In this report, we present the successfully synthesized NaFePO4 based on XRD and SEM result. XRD results show the presence of NaFePO4 as a major phase and some amount of secondary phase. SEM result indicates the plate-like particle which tends to agglomerate with the size range 2-5 μm.