This manuscript describes an effective and facile synthesis route of AlN microspheres via combining sol-gel technique and gas-reduction-nitridation method. Monodisperse AlN microspheres have been synthesized by heat treatment of amorphous precursors at 1200°C under the flow of NH 3 . Compared to AlN particles reported in the previous literatures, the monodisperse AlN microspheres prepared in this work exhibit high degree of crystallinity, regular spherical morphology, controllable particle size, and narrow particle size distribution. In combination with the lower heat-treated temperature and simple synthesis equipment, this synthesis route will decrease significantly the preparation costs of AlN microspheres with regular spherical morphology and is sure of potential commercial value. Graphical Abstract
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