The surface composition of the polycrystalline Co50Ni50 alloy is determined as a function of temperature by Auger electron spectroscopy (AES) and the influence of the segregation of sulphur on this composition is investigated. The quantitative method of Auger spectrometry based on lowenergy M23 VV transitions is described and the necessity of the use of such transitions in the investigation of segregation is shown. A clean surface of the Co50Ni50 alloy contains 52% Ni in the temperature range 600 to 800 K, while in the range of 800 to 1100 K the surface is enriched in cobalt (66.1% Co at 1100 K). At not too high surface concentrations of sulphur (≦ 15%) the atoms of sulphur compete with those of cobalt for sites in the surface region.
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