Comparing Xe⁺pFIB and Ga⁺FIB for TEM sample preparation of Al alloys: Minimising FIB‐induced artefacts

Recently, the dual beam Xe⁺ plasma focused ion beam (Xe⁺ pFIB) instrument has attracted increasing interest for site-specific transmission electron microscopy (TEM) sample preparation for a local region of interest as it shows several potential benefits compared to conventional Ga⁺ FIB milling. Nevertheless, challenges and questions remain especially in terms of FIB-induced artefacts, which hinder reliable S/TEM microstructural and compositional analysis. Here we examine the efficacy of using Xe⁺ pFIB as compared with conventional Ga⁺ FIB for TEM sample preparation of Al alloys. Three potential source of specimen preparation artefacts were examined, namely: (1) implantation-induced defects such as amophisation, dislocations, or 'bubble' formation in the near-surface region resulting from ion bombardment of the sample by the incident beam; (2) compositional artefacts due to implantation of the source ions and (3) material redeposition due to the milling process. It is shown that Xe⁺ pFIB milling is able to produce improved STEM/TEM samples compared to those produced by Ga⁺ milling, and is therefore the preferred specimen preparation route. Strategies for minimising the artefacts induced by Xe⁺ pFIB and Ga⁺ FIB are also proposed. LAY DESCRIPTION: FIB (focused ion beam) instruments have become one of the most important systems in the preparation of site-specific TEM specimens, which are typically 50-100 nm in thickness. TEM specimen preparation of Al alloys is particularly challenging, as convention Ga-ion FIB produces artefacts in these materials that make microstructural analysis difficult or impossible. Recently, the use of noble gas ion sources, such as Xe, has markedly improved milling speeds and is being used for the preparation of various materials. Hence, it is necessary to investigate the structural defects formed during FIB milling and assess the ion-induced chemical contamination in these TEM samples. Here we explore the feasibility and efficiency of using Xe⁺ PFIB as a TEM sample preparation route for Al alloys in comparison with the conventional Ga+FIB.