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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.
Polycrystalline Ni-based superalloys for aerospace and power generation applications are often precipitation hardened to achieve strengthening at elevated temperatures. Here, atom probe microscopy has become an essential tool to study the complex morphology of nanoscale precipitates. This study focuses on Alloy 718, which is hardened by semi-coherent, ordered γ′ (Ni3(Al, Ti)) and γ″ (Ni3(Nb)) particles. According to previous research, these particles often occur as duplets or triplets with a stacking sequence dependent on prior processing. This creates various interfaces with a strong impact on the mechanical properties, highlighting the importance of quantitative studies which are challenging with electron microscopy. We present atom probe data reconstruction and analysis approaches particularly suited for precipitation hardened superalloys. While voltage atom probe allows for an accurate reconstruction, the acquired data volume is often limited. Laser-assisted atom probe provides statistically significant data, but the loss of crystallographic information requires correlation with voltage-mode datasets. We further describe an advanced iso-surface method where initially arbitrarily chosen concentration thresholds of Al + Ti for γ′ and Nb for γ″ particles are optimized. Recognizing the importance of the precipitate stacking order, the different types of precipitate interfaces are quantified, and these methods may be applicable to other engineering alloys.
Correlative microscopy approaches offer synergistic solutions to many research problems. One such combination, that has been studied in limited detail, is the use of atom probe tomography (APT) and transmission Kikuchi diffraction (TKD) on the same tip specimen. By combining these two powerful microscopy techniques, the microstructure of important engineering alloys can be studied in greater detail. For the first time, the accuracy of crystallographic measurements made using APT will be independently verified using TKD. Experimental data from two atom probe tips, one a nanocrystalline Al–0.5Ag alloy specimen collected on a straight flight-path atom probe and the other a high purity Mo specimen collected on a reflectron-fitted instrument, will be compared. We find that the average minimum misorientation angle, calculated from calibrated atom probe reconstructions with two different pole combinations, deviate 0.7° and 1.4°, respectively, from the TKD results. The type of atom probe and experimental conditions appear to have some impact on this accuracy and the reconstruction and measurement procedures are likely to contribute further to degradation in angular resolution. The challenges and implications of this correlative approach will also be discussed.
The ternary system Fe - 25 at% Co - 9 at% Mo shows an age hardening behavior similar to aluminum alloys. After solution annealing followed by rapid quenching, the Fe-Co-matrix is hardened during subsequent aging through precipitation of the intermetallic µ-phase (Fe,Co)7Mo6. In aged condition the entire Mo content is present in coarse primary and fine µ-phase particles and, therefore, the matrix consists exclusively of 71 at% Fe and 29 at% Co. The binary system Fe-Co shows a transformation from the disordered bcc structure to the ordered B2 structure between 25 and 72 at% Co at a critical ordering temperature ranging from room temperature to 723°C. As a consequence, the remaining overaged matrix in the Fe - 25 at% Co - 9 at% Mo system should also show such a transition. However, an ordered phase is brittle and, thus, not wanted for many applications. Better mechanical properties in terms of ductility can be achieved with a partially or fully disordered phase. Such a state can be obtained by rapid quenching from temperatures above the critical ordering temperature. In this study such an approach was implemented on the ternary Fe - 25 at% Co - 9 at% Mo alloy. The effect of different cooling rates on the mechanical properties was investigated by means of hardness testing. The actual ordering transition of the Fe - 29 at% Co matrix was determined with differential scanning calorimetry and neutron diffraction.
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