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LiFePO₄ is a promising cathode material for secondary lithium batteries due to its high energy density, low cost and safety. LiFePO₄ was synthesized by the citrate process under reductive, neutral, and oxidative, atmospheres and the crystal structure was analyzed by X-ray powder diffraction. The samples synthesized under N₂ and H₂ atmosphere showed a single phase of a olivine structure, where the samples synthesized under O₂ atmosphere exhibited second phase of Fe2O₃. All the samples synthesized at 400, 600 and 800℃ under N₂ atmosphere presented a single phase of olivine. Residual organic material was observed for the sample synthesized at 400℃. There was nearly no intensity difference between the samples synthesized at 600℃ and 800℃. The electrochemical characteristic of the LiFePO₄ synthesized at 600℃ in the N₂ atmosphere was analyzed. The result exhibited an high discharge capacity of 160 mAh/g at the first cycle, and 155-160 mAh/g after 45 cycles.

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