Abstract. Recently, Na2/3[Fe1/2Mn1/2]O2 has received attention as a potential candidate material for cathode sodium-ion batteries. However, this material was synthesized by a solid-state process, resulting in larger particle size and nonuniform morphology. The larger particle size will sluggish the Na ion diffusion. Here we report the synthesis of Na2/3[Fe1/2Mn1/2]O2 using a simple sol-gel process. The X-ray diffraction revealed that the sample was identified as Na2/3[Fe1/2Mn1/2]O2 with a hexagonal crystal structure. However, the impurities are formed at diffraction angles of 36.28°, 45.03°, and 51.23°. Calcination temperature affects the formation of the crystal phase, grain growth, morphology, and particle size. Our findings provide valuable insight into the development of Na2/3[Fe1/2Mn1/2]O2  material with desirable properties. Keywords:Sol-Gel, Solid State, Grain Growth, Calcination, Na2/3[Fe1/2Mn1/2]O2 
                        
                        
                        
                        
                            
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