The decomposition of organometallic precursors of AIN thin film on the Ni (100) single crystal surface is examined at temperature between 470 K ~ 1070 K during continuous exposure to single precursors $[Me_2Al(μ-NHR)]_2$ ($R=^iPr,^tBu$) at $5 \times 10^{-7}$ torr. The deposited films are characterized with X-ray photoelectron spectroscopy (XPS) and the gas products are analyzed by mass spectrometry. The optimum temperature for the formation of AIN thin film is found to be about 700 ~ 770 K. Carbon contamination of the films is mainly attributed to the carbon of methyl group. In this thesis it is presented how the substitution of alkyl group(R) in the single precursor affects the decomposition pathway. A special sample doser is designed and constructed.