An in situ generated template method has been developed via the simple reaction of AlCl3 with NH3 for the synthesis of AlN hollow nanospheres with diameters of 80—400 ran and shell thickness of ~15 nm. On the basis of the detailed characterization on the intermediate compounds, the preparation process has been elucidated which includes the first formation of the AlCl3·xNH3@AlN core-shell nanostructures followed by the decomposition of the inner compound around 1100 °C. This reaction route successfully extended the traditional CVD reaction of AlCl3 with NH3 from producing solid AlN powder to preparing AlN hollow nanospheres.
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