ABSTRACTUltrathin silicon oxide/nitride/oxide films on silicon prepared by the usual route -thermal growth of an oxide followed by deposition of a nitride layer by chemical vapor deposition, and finally a reoxidation step - were characterized using isotopic substitution of N and O and depth profiling with sub-nanometric resolution. The redistribution of N and O during the oxide/nitride/oxide film processing was investigated by: i) ¹⁵N and ¹⁸O depth profiling by means of narrow nuclear resonance, and ii) ¹⁶O profiling using step-by-step chemical dissolution associated with areal densities determinations by nuclear reaction analysis. It was observed that the reoxidation step, here performed varying temperature and time, induces atomic transport of O and N thus resulting in oxide/nitride/oxide structures which are not stacked layered ones, but rather silicon oxynitride ultrathin films, in which the N concentration presents a maximum in the bulk and is moderate in the near-surface and near-interface regions.