In this study, we described an atomic layer deposition (ALD) process for the preparation of nanoscale nickel oxide (NiO) films with high growth rate by using a combination of nickel(II) diketonate-diamine (Ni(acac)(2)(TMEDA), TMEDA = N,N,N',N'-tetramethyl-ethylenediamine) and ozone (O-3). Typical self-limiting film growth behavior was observed between 200 and 275 degrees C, and growth saturation with respect to both precursor pulse time was verified. The chemical composition, crystalline phase, and surface morphology of the films were studied using X-ray photoelectron spectroscopy, X-ray diffraction, and atomic force microscopy. All the results confirmed that the ALD process occurred with high growth rate of approximately 2.0 angstrom/cycle and resulted in high-quality, smooth films.