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The low-temperature hydrothermal synthesis method has been drawing ever-growing attention due to the fact that it has many advantages over conventional methods for preparing promising cathode material LiFePO(4). However; the mechanism for hydrothermal synthesis of LiFePO(4) remains unclear. Here, the hydrothermal reaction mechanism of LiFePO(4) is systematically studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), trail mission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and specific surface analysis. As evidenced by apparent precursor dissolution, fast hydrothermal formation, and significant decrease in particle size with adding alcohols and/or carbon black in the reaction system, a dissolution-precipitation mechanism accounts for the hydrothermal synthesis of LiFePO(4). Moreover, we identified tetraphosphate in the LiFePO(4) precursor. This compound undergoes hydrolysis upon heating during the hydrothermal process, resulting in a remarkable decline of pH value.

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