LiFePO 4 nanoparticles were synthesized via polyol process. The temperature of the solution was rapidly increased up to 320 °C to obtain larger particles and the temperature was maintained for 16 h in a round-bottomed flask attached to a refluxing condenser. The X-ray diffractrion (XRD), pattern was indexed on the basis of orthorhombic olivine structure. The LiFePO 4 compound prepared through polyol process exhibited a high crystallinity. The particles show the various shapes with size ranging from 100 to 300 nm. The initial discharge curve of LiFePO 4 capacity shows 168 mA h/g at the 0.1 C rate in the voltage range of 2.5–4 V with well-formed plateau.
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