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The segregation of reactive elements (REs) along thermally grown oxide (TGO) grain boundaries has been associated to slower oxide growth kinetics and improved creep properties. However, the incorporation and diffusion of these elements into the TGO during oxidation of Ni alloys remains an open question. In this work, electron backscatter diffraction in transmission mode (t-EBSD) was used to investigate the microstructure of TGO within the thermal barrier coating on a Ni-based superalloy, and atom probe tomography (APT) was used to quantify the segregation behavior of REs to α-Al2O3 grain boundaries. Integrating the two techniques enables a higher level of site-specific analysis compared to the routine focused ion beam lift-out sample preparation method without t-EBSD. Needle-shaped APT specimens readily meet the thickness criterion for electron diffraction analysis. Transmission EBSD provides an immediate feedback on grain orientation and grain boundary location within the APT specimens to help target grain boundaries in the TGO. Segregation behavior of REs is discussed in terms of the grain boundary character and relative location in TGO.
Atom probe tomography (APT) is a technique that has expanded significantly in terms of adoption, dataset size, and quality during the past 15 years. The sophistication used to ensure ultimate analysis precision has not kept pace. The earliest APT datasets were small enough that deadtime and background considerations for processing mass spectrum peaks were secondary. Today, datasets can reach beyond a billion atoms so that high precision data processing procedures and corrections need to be considered to attain reliable accuracy at the parts-per-million level. This paper considers options for mass spectrum ranging, deadtime corrections, and error propagation as applied to an extrinsic-silicon standard specimen to attain agreement for silicon isotopic fraction measurements across multiple instruments, instrument types, and acquisition conditions. Precision consistent with those predicted by counting statistics is attained showing agreement in silicon isotope fraction measurements across multiple instruments, instrument platforms, and analysis conditions.
Specimen survivability is a primary concern to those who utilize atom probe tomography (APT) for materials analysis. The state-of-the-art in understanding survivability might best be described as common-sense application of basic physics principles to describe failure mechanisms. For example, APT samples are placed under near-failure mechanical-stress conditions, so reduction in the force required to initiate field evaporation must provide for higher survivability—a common sense explanation of survivability. However, the interplay of various analytical conditions (or instrumentation) and how they influence survivability (e.g., decreasing the applied evaporation field improves survivability), and which factors have more impact than others has not been studied. In this paper, we report on the systematic analysis of a material composed of a silicon-dioxide layer surrounded on two sides by silicon. In total, 261 specimens were fabricated and analyzed under a variety of conditions to correlate statistically significant survivability trends with analysis conditions and other specimen characteristics. The primary result suggests that, while applied field/force plays an obvious role in survivability for this material, the applied field alone does not predict survivability trends for silicon/silicon-dioxide interfaces. The rate at which ions are extracted from the specimen (both in terms of ions-per-pulse and pulse-frequency) has similar importance.
The semiconductor industry has seen tremendous progress over the last few decades with continuous reduction in transistor size to improve device performance. Miniaturization of devices has led to changes in the dopants and dielectric layers incorporated. As the gradual shift from two-dimensional metal-oxide semiconductor field-effect transistor to three-dimensional (3D) field-effect transistors (finFETs) occurred, it has become imperative to understand compositional variability with nanoscale spatial resolution. Compositional changes can affect device performance primarily through fluctuations in threshold voltage and channel current density. Traditional techniques such as scanning electron microscope and focused ion beam no longer provide the required resolution to probe the physical structure and chemical composition of individual fins. Hence advanced multimodal characterization approaches are required to better understand electronic devices. Herein, we report the study of 14 nm commercial finFETs using atom probe tomography (APT) and scanning transmission electron microscopy–energy-dispersive X-ray spectroscopy (STEM-EDS). Complimentary compositional maps were obtained using both techniques with analysis of the gate dielectrics and silicon fin. APT additionally provided 3D information and allowed analysis of the distribution of low atomic number dopant elements (e.g., boron), which are elusive when using STEM-EDS.