A new type of precursor, AlCl 3 : t BuNH 2 adduct, has been designed. The synthesis, preparation, and characterization of AlN thin films have been carried out. The AlCl 3 : t BuNH 2 adduct was a stable solid material with high vapor pressure (2.5 torr at 65 C) which was purified by sublimation. The structure of the precursor was fully identified by an X-ray single crystal analysis, elemental analysis, and nuclear magnetic resonance (NMR). The CVD process was performed using hydrogen under atmospheric pressure as the carrier gas. The film was characterized by Rutherford backscattering spectroscopy (RBS), Auger electron spectroscopy (AES), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The quality of the film prepared from the precursor was excellent, with a preferential c-axis orientation, exceptionally low carbon contamination, and an ideal N/Al atomic ratio.