Using narrow nuclear reaction resonance profiling, aluminum profiles are obtained in ∼3.5 nm Al2O3 films deposited by low temperature (≪400 °C) chemical vapor deposition on Si(100). Narrow nuclear resonance and Auger depth profiles show similar Al profiles for thicker (∼18 nm) films. The Al profile obtained on the thin film is consistent with a thin aluminum silicate layer, consisting of Al–O–Si bond units, between the silicon and Al2O3 layer. Transmission electron microscopy shows evidence for a two-layer structure in Si/Al2O3/Al stacks, and x-ray photoelectron spectroscopy shows a peak in the Si 2p region near 102 eV, consistent with Al–O–Si units. The silicate layer is speculated to result from reactions between silicon and hydroxyl groups formed on the surface during oxidation of the adsorbed precursor. © 1999 American Institute of Physics.