Abstract
The effects of citric acid (CA) and ammonium (NH4+) ions on the structural and morphological transformations of olivine LiFePO4 upon hydrothermal treatment are systematically investigated, as a function of reaction time, by using a combination of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), magic-angle-spinning nuclear magnetic resonance (MAS NMR), and Fourier transform infrared absorption spectroscopy (FTIR). In the presence of both CA and NH4+ ions, the structures evolve from amorphous precursors to crystalline (NH4)FePO4·H2O and finally LiFePO4. The initial olivine particles adopt an egglike shape and appear to form from the fusing of (NH4)FePO4·H2O plates. This metastable morphology evolves to form a mixture of cubic and rhombic particles. These particles are then etched, resulting in hollow structures and then ultimately barrel-like particles, after over 120 h of hydrothermal reaction at 180 °C. The final morphology is close to the equili...
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