Cross-Sectional Sample Preparation and Analysis of Intergranular Stress Corrosion Cracks in FE-NI-CR Alloys.

Abstract Transmission electron microscopy in its modern high-resolution analytical form has great potential for elucidating mechanisms of environmental cracking in structural alloys and other materials. Apart from a few pioneering efforts, the difficulties of preparing suitable samples with the original corrosion structures preserved in narrow crack tips have limited contributions of TEM in this area. Recent work involving cross-sectional crack preparation has focused on intergranular stress-corrosion cracking of Fe- and Ni-base stainless alloys in high-temperature water. This presentation will illustrate preparation methods that have proven successful, and describe limitations of the analysis. The method for preparing cross-section samples suitable for high-resolution TEM characterization is based on earlier work by Lewis et al. It involves preparing a thin section containing cracks filled with epoxy, dimple grinding selected locations near the crack tip, and ion milling. Figure 1 schematically illustrates this method. The first step is to preserve the crack opening characteristics present under loading and protect the crack surfaces during thinning.