Michael Moody

We describe a method to estimate background noise in atom probe tomography (APT) mass spectra and to use this information to enhance both background correction and quantification. Our approach is mathematically general in form for any detector exhibiting Poisson noise with a fixed data acquisition time window, at voltages varying through the experiment. We show that this accurately estimates the background observed in real experiments. The method requires, as a minimum, the z-coordinate and mass-to-charge-state data as input and can be applied retrospectively. Further improvements are obtained with additional information such as acquisition voltage. Using this method allows for improved estimation of variance in the background, and more robust quantification, with quantified count limits at parts-per-million concentrations. To demonstrate applications, we show a simple peak detection implementation, which quantitatively suppresses false positives arising from random noise sources. We additionally quantify the detectability of 121-Sb in a standardized-doped Si microtip as (1.5 × 10−5, 3.8 × 10−5) atomic fraction, α = 0.95. This technique is applicable to all modes of APT data acquisition and is highly general in nature, ultimately allowing for improvements in analyzing low ionic count species in datasets.

© 2020 Acta Materialia Inc. Atom Probe Tomography is used to show that the α2 phase (Ti3Al) forms upon ageing Ti–7Al at 550 °C with as little as 500 wppm oxygen. Notably, it is found that oxygen consistently partitions away from the α2 precipitates to the α matrix. The role of aluminium concentration and oxygen solubility on oxygen partitioning preference is also investigated. Based on our observations, we propose a mechanism by which oxygen encourages α2 formation despite partitioning away from it. Furthermore, nanohardness systematically measured with respect to ageing time and oxygen concentration suggests that α2 precipitation is not the dominant hardening mechanism during ageing.

© 2020 Acta Materialia Inc. The microstructure of the surface oxide film formed on an Fe-9Cr Ferritic-Martensitic (F-M) steel after exposure to deaerated high-temperature steam at 600°C for 100 h has been analyzed in detail by advanced characterization techniques. The surface oxide film has been revealed to have a triplex structure, including an outer oxide layer, an inner oxide layer, and an internal oxide layer. Although the outer and inner oxide layers are continuous, the internal oxide layer has been proved to consist of interconnected metallic and chromite phases, which is a typical feature of internal oxidation. The formation mechanisms of each layer have been discussed, finding that, contrary to what the available space model suggests, an external oxidation is not the controlling oxidation mechanism of F-M steels in high-temperature steam. The higher resolution used in this study confirms that the controlling mechanism is internal oxidation.