Cold-neutron depth profiling as a research tool for the study of surface oxides on metals

Full text: The shiny surface of most metals, with the exceptions of gold and platinum, is actually coated with a thin layer of oxide. Although typically only a few nanometres (nm) thick, the oxide layer is key for the metal's survival in our 02-containing atmosphere. Consequently, there is a continuing need to develop experimental techniques to study oxide layers on metals. The need for a technique that could track the movement of an oxygen-containing layer first came to our attention when we studied the growth of anodic oxide on Ti with neutron reflectometry. As new oxide grew with oxygen ions derived from an aqueous solution, a small amount of hydrogen was found to be incorporated into the oxide layer, and remained adjacent to the oxide/water interface. Whether the H remains attached to its companion 0, i.e., as an OH ion, or if the ion dissociates once inside the oxide layer is unknown. Whether the original air-grown oxide acts as a passive screen during anodization, or if it plays an active in the hopping of ions from site to site is also unknown. These questions could be answered unambiguously only if we can somehow label the original 0 atoms. Isotopic labeling combined with neutron scattering is not an option since the coherent scattering lengths of all three 0 isotopes are very similar. Fortunately, one of the isotopes, 170, is sensitive to neutron depth-profiling via the (n,a) reaction (1). We hereby report encouraging results obtained by a preliminary experiment carried out to assess the potential of this technique.