Plasma focused ion beam microscopy (PFIB) is a recent nanofabrication technique that is suitable for site-specific atom probe sample preparation. Higher milling rates and fewer artifacts make it superior to Ga+ FIBs for the preparation of samples where large volumes of material must be removed, for example, when trying to avoid lift-out techniques. Transmission Kikuchi diffraction (TKD) is a method that has facilitated phase identification and crystallographic measurements in such electron transparent samples. We propose a procedure for preparing atom probe tomography (APT) tips from mechanically prepared ribbons by using PFIB. This is highly suitable for the preparation of atom probe tips of interfaces such as interphase boundaries from challenging materials where lift-out tips easily fracture. Our method, in combination with TKD, allows the positioning of regions of interest such as interfaces close to the apex of the tip. We showcase the efficacy of the proposed method in a case study on Alloy 718, where the interface between γ-matrix and δ-phase has not been yet extensively explored through APT due to preparation challenges. Results show depletion of γ″-precipitates near the γ/δ interface. A quantitative evaluation of the composition of phases in the bulk versus near the interface is achieved.

Nonmetallic inclusion (NMI) populations in superelastic (SE) Nitinol fine wires (<140 μm in diameter) were investigated by combining plasma focused ion beam (PFIB) serial sectioning with scanning electron microscopy (SEM). High purity (HP)—lower oxygen content and standard purity (SP)—higher oxygen content Nitinol wires were sectioned and imaged. The three-dimensional (3D) reconstructions provided more complete connectivity of NMIs and pores as well as information about the distribution of the features within the wire volume that is not possible with traditional two-dimensional (2D) imaging techniques. NMIs were present alone and with pores in the leading and/or trailing edges of the inclusions, in addition to stringers (i.e., fractured, elongated NMI, and intermixed with pores adjacent to each other), all of which were parallel to the wire drawing axis. The area percentages for the NMIs were 0.01% (HP Nitinol) and 0.04% (SP Nitinol), while the volume percentages measured 0.09% (HP Nitinol) and 0.47% (SP Nitinol). The combined PFIB-SEM serial sectioning approach provided the requisite resolution necessary to distinguish between NMIs and pores at micron and submicron sizes. Information gathered from this technique can be used to better inform models and predictions for fatigue lifetimes based on statistical analyses of these feature populations.