Specimen preparation for correlating transmission electron microscopy and atom probe tomography of mesoscale features.

Atom-probe tomography (APT) provides atomic-scale spatial and compositional resolution that is ideally suited for the analysis of grain boundaries. The small sample volume analyzed in APT presents, however, a challenge for capturing mesoscale features, such as grain boundaries. A new site-specific method utilizing transmission electron microscopy (TEM) for the precise selection and isolation of mesoscale microstructural features in a focused-ion-beam (FIB) microscope lift-out sample, from below the original surface of the bulk sample, for targeted preparation of an APT microtip by FIB-SEM microscopy is presented. This methodology is demonstrated for the targeted extraction of a prior austenite grain boundary in a martensitic steel alloy; it can, however, be easily applied to other mesoscale features, such as heterophase interfaces, precipitates, and the tips of cracks.