The anodization of Si in a 1 MHz oxygen plasma is described. In‐situ film thickness measurements were made using a single angle “s” light reflectance technique and this data, coupled with information on the variation of sample voltage with thickness, was used to determine the dependence of ionic current on oxide field strength. The data for a given oxide thickness could be described by an equation of the form given by the theory of ionic conduction by a thermally activated, field‐assisted process. However, the ionic current and, in paticular, the oxide field strength were dependent on oxide thickness. MOS C‐V measurements on oxides of different thickness indicated a change in flatband voltage that could be attributed to a progressive build‐up of positive charge within the oxide. This space charge could be reduced by a low temperature annealing treatment. The oxides were found to be slightly absorbing optically, to have a relative permittivity in the range 3.5–3.9, and to possess good insulation properties as long as the oxide thickness did not exceed about 2500â.