Ti has a high affinity for hydrogen and are 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 α grain boundaries and α/β phase boundaries in commercial pure Ti and α+β binary model alloys. No hydrides are observed in the α phase in alloys with Al addition or quenched-in Mo supersaturation.

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Titanium alloys are widely used in the aerospace industry, yet oxygen ingress can severely degrade the mechanical properties of titanium alloy components. 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). It has been found that the hardening effects of microstructure and crystallography are only significant at very low-oxygen concentrations, whereas interstitial solid solution hardening dominates by order of magnitude for higher oxygen concentrations. The role of microstructure on oxygen ingress has been studied and oxygen ingress along a potential α/β interface was directly observed on the nanoscale using APT.

A method is presented for the registration and correlation of property maps of materials, including data from nanoindentation hardness, Electron Back-Scattered Diffraction (EBSD), and Electron Micro-Probe Analysis (EPMA). This highly spatially resolved method allows for the study of micron-scale microstructural features, and has the capability to rapidly extract correlations between multiple features of interest from datasets containing thousands of data points. Two case studies are presented in commercially pure (CP) titanium: in the first instance, the effect of crystal anisotropy on measured hardness and, in the second instance, the effect of an oxygen diffusion layer on hardness. The independently collected property maps are registered using affine geometric transformations and are interpolated to allow for direct correlation. The results show strong agreement with trends observed in the literature, as well as providing a large dataset to facilitate future statistical analysis of microstructure-dependent mechanisms. Graphical abstract

Atom Probe Tomography is used to show that the α 2 phase (Ti 3 Al) forms upon ageing Ti-7Al at 550 o C with as little as 500 wppm oxygen. Notably, it is found that oxygen consistently partitions away from the α 2 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 α 2 formation despite partitioning away from it. Furthermore, nanohardness systematically measured with respect to ageing time and oxygen concentration suggests that α 2 precipitation is not the dominant hardening mechanism during aging.

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The kinetics of primary α-Ti colony/Widmanstätten plate growth from the β 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 µm min −1 at 850 • C, which was in good agreement with the model prediction of 0.36 µm 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 β 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 β 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.

The oxidation response and microstructural evolution of an Inconel 625 alloy exhaust manifold exposed to an automobile racing environment has been examined using a range of advanced electron microscopy-based techniques, atom probe tomography and high-sensitivity laser ablation mass spectrometry. The dynamic, corrosive gas conditions result in accelerated oxidation, with the inner exhaust surface also heavily contaminated by multiple species including Zn, P, K and Na. Nb carbides and Ti nitrides identified in stock control samples evolve into mixed (Ti, Nb)N species during exposure, decorated by smaller Mo, Si-rich precipitates. The exposed alloy component therefore reveals unique surface and subsurface features following in-service use.