LiCoO2 concaved cuboctahedra with a size of about 1.0 μm were hydrothermally prepared from CoCO3 and LiOH·H2O at 150 °C. Field-emitting scanning electron microscope (FESEM) images show that the cuboctahedra consisted of four hexagonal plates, with angles of 70.5° in neighboring plates. Electron diffraction (ED) patterns of the hexagonal plates show 1 0 0 diffraction of LiCoO2 in rhombohedral phase and 2 2 0 diffraction in spinel phase, which means LiCoO2 concaved cuboctahedra are comprised of two intergrown phases. The electrochemical performance of these concaved cuboctahedra of LiCoO2 at a rate of 0.5 C demonstrated first run charge/discharge capacities of 155 and 141 mAh g−1 and a stable discharge capacity of 114 mAh g−1 after 100 cycles. After that, FESEM images show the LiCoO2 concaved cuboctahedra have undergone no significant change. At a temperature of 120 °C and under the same conditions, only a small amount of LiCoO2 concaved cuboctahedron appeared. As the temperature rose to 180 °C, flower-like LiCoO2 microstructures with a size of about 1.0 μm were formed, constructed of irregular plates. The electrochemical performance of the products prepared at 120 °C and 180 °C indicates lower stability than that of LiCoO2 concaved cuboctahedra.
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