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A novel y-y'-y" dual-superlattice superalloy, with promising mechanical properties up to elevated temperatures was recently reported. The present work employs state of the art chemical and spatial characterization techniques to study the effect systematic additions of Mo, W and Fe and variations in Nb and Al contents have on the phase fraction, thermal stability, elemental partitioning and mechanical properties. Alloys were produced through arc melting followed by heat treatment. Multi-scale characterization techniques and hardness testing were employed to characterize their microstructure, thermal stability and mechanical properties. Alterations in such properties or in elemental partitioning behaviour were then explained through thermodynamic modelling. A modest addition of 1.8 at.% Mo had a strong effect on the microstructure and thermal stability: it minimized microstructural coarsening during heat treatments while not significantly decreasing the y' solvus temperature. A reduction of Nb by 0.6 at.%, strongly reduced the y" volume fraction, without affecting the y' volume fraction. The reduced precipitate fraction led to a significant reduction in alloy hardness. Fe, added to achieve better processability and reduced material cost, decreased the y' solvus temperature and caused rapid microstructural coarsening during heat treatments, without affecting alloy hardness. A reduction of Al by 0.4 at.%, reduced the y' volume fraction and the y' solvus temperature, also without affecting alloy hardness. The addition of 0.9 at.% W decreased the y' solvus temperature but increased both precipitate volume fractions. These data will be invaluable to optimize current alloy design and to inform future alloy design efforts.

A new class of crack-resistant nickel-based superalloy containing high $\gamma^\prime$ fraction is studied for the laser-powder bed fusion (L-PBF) process. The effects of the (Nb+Ta)/Al ratio is emphasised, a strategy that is shown to confer excellent low-temperature strength whilst maintaining oxidation resistance at high temperatures via stable alumina scale formation. The processability of the new alloys is characterised with respect to defect assessment by micro-focus x-ray computed tomography; use is made of a prototype turbine blade geometry and the heritage alloy CM247LC as a benchmark. In all cases, some processing-related porosity is present in thin wall sections such as the trailing edge, but this can be avoided by judicious processing. The cracking seen in CM247LC -- in solid-state, liquation and solidification forms -- is avoided. A novel sub-solvus heat treatment strategy is proposed which takes advantage of AM not requiring solutioning; super-solvus heat treatment is inappropriate since it embrittles the material by deterioration of the texture and coarsening of grain boundary carbides. The tensile strength of the new superalloy is greatest when the Nb+Ta content is highest and exceeds that of CM247LC up to $\sim$900$\,$$^\circ$C. The oxidation resistance is best when Al content is highest, and oxidation-assisted cracking resistance maximized when the (Nb+Ta)/Al ratio is balanced. In all cases these are equivalent or superior to that of CM247LC. Nevertheless, the creep resistance of the new alloys is somewhat inferior to that of CM247LC for which the $\gamma^\prime$, C, and B contents are higher; this implies a processing/property trade-off which requires further clarification.

Atom probe tomography (APT), electron probe microanalysis (EPMA) and nanoindentation were used to characterise the oxygen-rich layer on an in-service jet engine compressor disc, manufactured from the titanium alloy TIMETAL 834. Oxygen ingress was quantified and related to changes in mechanical properties through nanoindentation studies. The relationship between oxygen concentration, microstructure, crystal orientation and hardness has been explored through correlative hardness mapping, EPMA and electron backscatter diffraction (EBSD). The role of microstructure on oxygen ingress has been studied and oxygen ingress along a potential alpha/ beta interface was directly observed on the nanoscale using APT.

The T91 grade and similar 9Cr tempered-martensitic steels (also known as ferritic-martensitic) are leading candidate structural alloys for fast fission nuclear and fusion power reactors. At low temperatures (300 to 400 $^\circ$C) neutron irradiation hardens and embrittles these steels, therefore it is important to investigate the origin of this mode of life limiting property degradation. T91 steel specimens were separately neutron irradiated to 2.14 dpa at 327 $^\circ$C and 8.82 dpa at 377 $^\circ$C in the Idaho National Laboratory Advanced Test Reactor. Atom probe tomography was used to investigate the segregation driven formation of Mn-Ni-Si-rich (MNSPs) and Cu-rich (CRP) co-precipitates. The precipitates increase in size and, slightly, in volume fraction at the higher irradiation temperature and dose, while their corresponding compositions were very similar, falling near the Si(Mn,Ni) phase field in the Mn-Ni-Si projection of the Fe-based quaternary phase diagram. While the structure of the precipitates has not been characterized, this composition range is distinctly different than that of the typically cited G-phase. The precipitates are composed of CRP with MNSP appendages. Such features are often observed in neutron irradiated reactor pressure vessel (RPV) steels. However, the Si, Ni, Mn, P and Cu solutes concentrations are lower in the T91 than in typical RPV steels. Thus, in T91 precipitation primarily takes place in solute segregated regions of line and loop dislocations. These results are consistent with the model for radiation induced segregation driven precipitation of MNSPs proposed by Ke et al. Cr-rich alpha prime ($\alpha$') phase formation was not observed., Comment: Pre-print (not peer reviewed)

We report on a new algorithm for detection of crystallographic information in 3D, as retained in Atom Probe Tomography (APT), with improved robustness and signal detection performance. The algorithm is underpinned by 1D distribution functions, as per existing algorithms, but eliminates an unnecessary parameter as compared to current methods. By examining traditional distribution functions in an automated fashion in real space, rather than using Fourier transform approaches, we utilise an error metric based upon the expected value for a spatially random distribution for detecting crystallography. We show cases where the metric is able to successfully obtain orientation information, and show that it can function with high levels of additive and displacive background noise. We additionally compare this metric to Fourier transform methods, showing fewer artefacts when examining simulated datasets. An extension of the approach is used to aid the automatic detection of high-quality data regions within an entire dataset, albeit with a large increase in computational cost. This extension is demonstrated on acquired Aluminium and Tungsten APT datasets, and shown to be able to discern regions of the data which have relatively improved spatial data quality. Finally, this program has been made available for use in other laboratories undertaking their own analyses.

In this work, we demonstrate a new system for the examination of gas interactions with surfaces via Atom Probe Tomography. This system provides the capability to examine the surface and subsurface interactions of gases with a wide range of specimens, as well as a selection of input gas types. This system has been primarily developed to aid the investigation of hydrogen interactions with metallurgical samples, to better understand the phenomenon of hydrogen embrittlement. In its current form, it is able to operate at pressures from 10^-6 to 1000 mbar (abs), can operate using a variety of gasses, and is equipped with heating and cryogenic quenching capabilities. We use this system to examine the interaction of hydrogen with Pd, as well as the interaction of water vapour and oxygen in Mg samples.

Titanium is commonly added to nickel superalloys but has a well-documented detrimental effect on oxidation resistance. The present work constitutes the first atomistic-scale quantitative measurements of grain boundary and bulk compositions in the oxide scale of a current generation polycrystalline nickel superalloy performed through atom probe tomography. Titanium was found to be particularly detrimental to oxide scale growth through grain boundary diffusion.

Interfaces play critical roles in materials, and are usually both structurally and compositionally complex microstructural features. The precise characterization of their nature in three-dimensions at the atomic-scale is one of the grand challenges for microscopy and microanalysis, as this information is crucial to establish structure-property relationships. Atom probe tomography is well-suited to analyzing the chemistry of interfaces at the nanoscale. However, optimizing such microanalysis of interfaces requires great care in the implementation across all aspects of the technique, from specimen preparation to data analysis and ultimately the interpretation this information. This article provides critical perspectives on key aspects pertaining to spatial resolution limits and the issues with compositional analysis that can limit the quantification of interface measurements. Here, we use the example of grain boundaries in steels, however the results are applicable for the characterization of grain boundaries and transformation interfaces in a very wide range of industrially relevant engineering materials.

The kinetics of primary alpha-Ti colony/Widmanstatten plate growth from the beta are examined, comparing model to experiment. The plate growth velocity depends sensitively both on the diffusivity D(T) of the rate-limiting species and on the supersaturation around the growing plate. These result in a maxima in growth velocity around 40 K below the transus, once sufficient supersaturation is available to drive plate growth. In Ti-6246, the plate growth velocity was found to be around 0.32 um min-1 at 850 oC, which was in good agreement with the model prediction of 0.36 um min-1 . The solute field around the growing plates, and the plate thickness, was found to be quite variable, due to the intergrowth of plates and soft impingement. This solute field was found to extend to up to 30 nm, and the interface concentration in the beta was found to be around 6.4 at.% Mo. It was found that increasing O content will have minimal effect on the plate lengths expected during continuous cooling; in contrast, Mo approximately doubles the plate lengths obtained for every 2 wt.% Mo reduction. Alloys using V as the beta stabiliser instead of Mo are expected to have much faster plate growth kinetics at nominally equivalent V contents. These findings will provide a useful tool for the integrated design of alloys and process routes to achieve tailored microstructures., Comment: Revised version resubmitted to journal

Ti has a high affinity for hydrogen and is a typical hydride formers. Ti-hydride are brittle phases which probably cause premature failure of Ti-alloys. Here, we used atom probe tomography and electron microscopy to investigate the hydrogen distribution in a set of specimens of commercially pure Ti, model and commercial Ti-alloys. Although likely partly introduced during specimen preparation with the focused-ion beam, we show formation of Ti-hydrides along {\alpha} grain boundaries and {\alpha}/\b{eta} phase boundaries in commercial pure Ti and {\alpha}+\b{eta} binary model alloys. No hydrides are observed in the {\alpha} phase in alloys with Al addition or quenched-in Mo supersaturation., Comment: Published in Acta Materialia in 2018

This work describes extensions to existing level-set algorithms developed for application within the field of Atom Probe Tomography (APT). We present a new simulation tool for the simulation of 3D tomographic volumes, using advanced level set methods. By combining narrow-band, B-Tree and particle-tracing approaches from level-set methods, we demonstrate a practical tool for simulating shape changes to APT samples under applied electrostatic fields, in three dimensions. This work builds upon our previous studies by allowing for non-axially symmetric solutions, with minimal loss in computational speed, whilst retaining numerical accuracy.

In this work, we report on the atom probe tomography analysis of two metallic hydrides formed by pressurized charging using an ex situ hydrogen charging cell, in the pressure range of 200-500 kPa (2-5 bar). Specifically we report on the deuterium charging of Pd/Rh and V systems. Using this ex situ system, we demonstrate the successful loading and subsequent atom probe analysis of deuterium within a Pd/Rh alloy, and demonstrate that deuterium is likely present within the oxide-metal interface of a native oxide formed on vanadium. Through these experiments, we demonstrate the feasibility of ex situ hydrogen analysis for hydrides via atom probe tomography, and thus a practical route to three-dimensional imaging of hydrogen in hydrides at the atomic scale.

In this paper we present a detailed analysis of the structural, electronic, and optical properties of an $m$-plane (In,Ga)N/GaN quantum well structure grown by metal organic vapor phase epitaxy. The sample has been structurally characterized by x-ray diffraction, scanning transmission electron microscopy, and 3D atom probe tomography. The optical properties of the sample have been studied by photoluminescence (PL), time-resolved PL spectroscopy, and polarized PL excitation spectroscopy. The PL spectrum consisted of a very broad PL line with a high degree of optical linear polarization. To understand the optical properties we have performed atomistic tight-binding calculations, and based on our initial atom probe tomography data, the model includes the effects of strain and built-in field variations arising from random alloy fluctuations. Furthermore, we included Coulomb effects in the calculations. Our microscopic theoretical description reveals strong hole wave function localization effects due to random alloy fluctuations, resulting in strong variations in ground state energies and consequently the corresponding transition energies. This is consistent with the experimentally observed broad PL peak. Furthermore, when including Coulomb contributions in the calculations we find strong exciton localization effects which explain the form of the PL decay transients. Additionally, the theoretical results confirm the experimentally observed high degree of optical linear polarization. Overall, the theoretical data are in very good agreement with the experimental findings, highlighting the strong impact of the microscopic alloy structure on the optoelectronic properties of these systems., Comment: 13 pages, 12 figures