X-RAY PHOTOELECTRON SPECTROSCOPIC STUDIES OF THIN-FILM OXIDES OF COBALT AND MOLYBDENUM

Surface oxidation reactions of cobalt, molybdenum and mixed cobalt–molybdenum metals have been investigated using x‐ray photoelectron spectroscopy (XPS). The oxide stoichiometries have been determined from XPS intensity measurements. Such quantification has been important in identifying oxide compositions with characteristic XPS spectra. A number of discrete binary molybdenum oxides have been characterized after reactions at 200°C and pressures ranging from 1 atm to 10−6 Pa. At the lowest pressure, the Mo 3d spectra and O/Mo ratios suggest the formation of a molybdenum–oxygen structure with a stoichiometry near unity. By contrast, at higher pressures, oxides that are predominantly MoO2 and MoO3 appear, but other intermediate oxide structures are also identified. Well‐defined binary oxides of cobalt can be prepared from cobalt metal after heating in oxygen at different pressures. New binary oxides of cobalt and molybdenum have been generated by the reaction on MoO3 or Co3O4 substrates. Oxidation of a thin film of molybdenum on a Co3O4 substrate has been shown to produce a nearly stoichiometric surface layer of CoMoO4. The procedure could be useful for the production of other ternary oxides of possible interest for use as XPS reference materials. Copyright © 1990 John Wiley & Sons Ltd.