Nanocrystalline lithium iron oxide LiFeO<sub>2</sub> was synthesized using sol-gel method. Rietveld analysis was performed to confirm the different phases associated in the formation of LiFeO<sub>2</sub>. Quantitative Rietveld refinement revealed that sample contains: 39.9 wt% of cubic α – LiFeO<sub>2</sub> phase, 58.5 wt% of monoclinic β - LiFeO<sub>2</sub> and tetragonal 1.7 wt%. of γ - LiFeO<sub>2</sub>. The nanocrystalline nature of the prepared samples was confirmed by SEM analysis. The magnetic properties of LiFeO<sub>2</sub> showed ferromagnetic property at room temperature