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Application of X-ray Absorption Near-Edge Spectroscopy at the S K-edge to the Structural Characterisation of Surface Reacted Metallic Alloys

X-ray absorption spectroscopy has been used to study the interaction of H2S at 700°C with a protective oxide layer on a Ni-20Cr alloy. Both fluoresence and electron yield detection modes, applied simultaneously, enabled structural information from 100nm and 5nm respectively to be probed which allowed the processes at the air/oxide and oxide/alloy interfaces to be monitored as a function of corrosion time. The data revealed sulphur to be in a high 6+ oxidation state in the early stages of the corrosion process, changing to 2- with the formation of a thicker sulphide-like surface film.