The effects of various interface preparations on atomic layer chemical vapor deposition (ALCVD) deposited Al2O3 and ZrO2 dielectrics properties were investigated by X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), medium energy ion scattering (MEIS) and transmission electron microscopy (TEM). H-terminated Si, SiO2 and SiOxNy, surfaces were used as substrates upon which the dielectric was deposited. Thermal annealing of SiO2 in NH3 forms an oxynitride; subsequent deposition of a ZrO2 /Al2O3 bi-layer stack resulted in a capacitor structure with an equivalent oxide thickness (EOT) of similar to 0.8 nm and a leakage current of 3 X 10(-4) A/cm(2) at - 1 + V-fb. This is in contrast to capacitor structures grown on H-terminated Si where high leakage was found. The growth of additional interfacial SiO2 during processing, a critical problem in nano-electronic device applications, is temperature dependent with ZrO2 exhibiting a higher oxygen permeability than Al2O3. Use of a polysilicon cap was shown to be effective at blocking oxygen absorption and transport through the high-k dielectrics, with stability up to 1100 C. (C) 2002 Elsevier Science B.V. All rights reserved.