Optimizing site-specific specimen preparation for atom probe tomography by using hydrogen for visualizing radiation-induced damage

Atom probe tomography (APT) is extensively used to measure the local chemistry of materials. Site-specific preparation via a focused ion beam (FIB) is routinely implemented to fabricate needle-shaped specimens with an end radius in the range of 50 nm. This preparation route is sometimes supplemented by transmission Kikuchi diffraction (TKD) to facilitate the positioning of a region of interest sufficiently close to the apex. Irradiating the specimen with energetic electrons and ions can lead to the generation of vacancies and even amorphization of the specimen. These extrinsically created vacancies become crucial for probing the hydrogen or deuterium distribution since they act as a strong trap. Here, we investigated the feasibility of site-specific preparation of a two-phase medium-Mn steel containing austenite (fcc) and ferrite (bcc). Following gaseous charging of APT specimens in deuterium (D2), clusters enriched by up to 35 at.% D, are imaged after Pt deposition, conventional Ga-FIB preparation, and TKD conducted separately. These D-rich clusters are assumed to arise from the agglomeration of vacancies acting as strong traps. By systematically eliminating these preparation-induced damages, we finally introduce a workflow allowing for studying intrinsic traps for H/D inherent to the material.(c) 2023 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.