A versatile low-temperature chemical approach utilizing an alkoxide-based hydrazide process was developed for the synthesis of nanometer-size aluminum nitride, oxynitride, and composite powders. The process consists of reacting aluminum tri-sec-butoxide and anhydrous hydrazine in acetonitrile at 80 degrees C to yield solid precipitates, which, when dried and heated in argon, nitrogen, or ammonia, yielded nanosize powders of the desired chemistry. The precursors and products of the reactions were identified by gas chromatography (GC), chemical analyses, and X-ray diffraction (XRD), while the morphology and particle size of the powders were determined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). GC revealed the release of butyl alcohol due to the reaction of the alkoxide with anhydrous hydrazine, suggesting the partial replacement (56.5%) of alkoxy groups by hydrazide groups (i.e., formation of Al-NHNH2 species). Fourier transform infrared (FTIR) and Al-27 magic-angle-spinning-nuclear-magnetic-resonance (MAS-NMR) spectroscopy provided structural insights regarding the changes in molecular linkages during heating of the precursor and the role of hydrazine in the subsequent nitridation reaction. Hydrazine's critical function as a nitride former in the initial stages of formation of the precursor, as well as during heat treatment, was further confirmed by studying its reaction with the alkoxide in the presence of controlled amounts of deionized (DI) water. Hydrolysis of the alkoxide while limiting the hydrazide reaction was found to promote the formation of versatile precursors that lead to oxide, oxynitride, or composite powders containing nanoparticles of the nitride phase in an oxynitride matrix.