ABSTRACT:The crystallization of ZnO microrods by hydrothermal treatment of a suspension formed from reaction of zinc acetate and sodium hydroxide has been examined using scanning and transmission electron microscopy as a function of hydrothermal reaction time. Polycrystalline hexagonal ZnO microrods first appeared after 0.5 h reaction time at 120 °C. These early stage rods were composed of stacks of hexagonal layers, each ~ 50 nm in thickness containing closely aligned assemblies of nanocrystallites < 20 nm in size. A further growth stage involving smaller pseudo-hexagonal columns nucleating and growing along <0001> from the (0001) basal layers of preformed polycrystalline hexagonal microrods was identified. For reaction times > 3h, the microrods were single crystals, as identified by TEM lattice imaging and electron diffraction, and many were in the form of double rods.