ESCA [electron spectroscopy for chemical analysis] examination of metal oxides and electronic ceramic materials: The effect of a low-energy argon-ion beam

Electronic ceramic materials are increasingly of interest to chemists because there is a growing interest in preparing high purity ceramics by chemical means and because the properties of the ceramics often depend on the chemical state of the elements in the ceramic. The chemical species, e.g. the oxidation state, of a metal in a ceramic can be identified by the analytical technique known as ESCA (electron spectroscopy for chemical analysis). In this work, the application of ESCA to ceramic materials begins with studies of metal oxide powders and examines the effect of a low energy argon ion beam. Two problems that occur with oxide powders and ceramics are surface charging and the formation of carbonates on the surface. Surface charging is generally compensated for by referencing to the carbon contaminant or by flooding the surface with electrons. Referencing to the contaminant peak meets with limited success when compared to the literature. Flooding the surface of oxide powders and ceramics causes peak distortion. Surface carbonates are identified in the carbon region by their separation of -4.5 eV from the contaminant carbon. To examine the effect of a low energy ion beam on metal oxide powders and ceramic powders, both the X-ray photoelectron (XPS) and X-ray induced Auger electron spectra (XAES) of SC2O3, V2O5, Cu2 O, ZnO and SnO2 are examined before and after ion beam exposure. Limited reduction of the metal is noted in the XPS spectra of V2O5. XAES indicates the Sc2O3, Cu2O and SnO2 are also reduced. XAES is especially useful for determining that reduction by the ion beam has occurred. A comparison of ion beam exposed oxide powders and heavily oxidized metal foils (Ti, Zr and Nb) shows that while the powders undergo limited reduction, the oxidized foils are reduced much more significantly with the same sputtering parameters