Analytical electron microscopy of a crack tip extracted from a stressed Alloy 800 sample exposed to an acid sulfate environment

Alloy 800 (Fe-21Cr-33Ni) has been found susceptible to cracking in acid sulfate environments, but the mechanism is not well understood. Alloy 800 C-ring samples were exposed to an acid sulfate environment at 315 °C and cracks were found with depths in excess of 300 μm after 60 h. Preparation of a TEM sample containing crack tips is challenging, but the ability to perform high-resolution microscopy at the crack tip would lend insight to the mechanism of acid sulfate stress corrosion cracking (AcSCC). The lift-out technique combined with a focused ion beam sample preparation was used to extract a crack tip along the cross-section of an acid sulfate crack in an Alloy 800 C-ring. TEM elemental analysis was done using EDS and EELS which identified a duplex oxide within the crack; an inner oxide consisting of a thin 3-4 nm Cr-rich oxide and an outer oxide enriched in Fe and Cr. Preliminary conclusions and hypotheses resulted with respect to the mechanism of AcSCC in Alloy 800.