Single mode microwave assisted synthesis of Lithium iron phosphate using iron carbonyl complex [Fe2(CO)9], as source of iron is reported in this paper. The suitable synthesis method for the LiFePO4 was designed based on FT-IR and TG-DTA studies of precursors. As prepared samples were characterized using different techniques such as X-ray diffraction, scanning electron microscope, field emission scanning electron microscope, transmission electron microscope, thermo gravimetric analysis, Raman spectroscope and electrochemical measurements. X-ray diffraction revealed that a single phase LiFePO4 powder can be synthesized quickly and easily by microwave processing. The surface analysis of the as prepared samples reveal that, it consist of nano-size particles with porous agglomeration, where the pores serve as channel for lithium supply and assist for augmentation of the electrochemical character of the product. The initial discharge capacities are 154.2, 132.2 and 121mAhg−1 at 0.1C, 0.5C and1C rate respectively. The obtained LiFePO4 has a high electrochemical capacity and good cyclic ability even after 50 cycles, which is attributed to the smaller particle size, porous agglomeration and graphitic carbon content.