The formation and crystallization of disordered nanosized ZnO resulting from the thermal decomposition of nanocrystalline hydrozincite [Zn5(CO3)2(OH)6] has been observed and investigated during pulse annealing experiments up to 625 °C in air or vacuum by electron paramagnetic resonance of trace amounts of substitutional Mn2+ impurity ions, in correlation with X-ray diffraction and transmission electron microscopy measurements. The mesoporous structure of the disordered ZnO, which initially forms in air and vacuum at 225 and 175 °C, respectively, further transforms into nanocrystalline ZnO of increasing particle size and improved lattice quality at higher annealing temperatures. The crystallization process, which does not affect the concentration of the substitutional impurity ions, as well as the simultaneous presence of both disordered and crystalline phases, should be considered in further applications of the resulting nanosized ZnO.
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