The almost limitless variations in potential compositions of high entropy alloys necessitates the use of computational methods when attempting to optimise for any given application. However, the accuracy of the current thermodynamic approaches commonly being used for this purpose remains under debate, as relatively few validatory studies have been performed. Within the CrMnFeCoNi family of alloys, the formation of the phase and how it is influenced by compositional variations is of particular interest for elevated temperature structural applications. Here, the role of Ni on the formation of the phase has been studied through a systematic series of CrMnFeCoNix alloys, 0 x 1.5, following 1000 hour exposures at temperatures typically found to promote formation. Ni was found to have a significant effect on the phase stability of these alloys, suppressing the phase such that a single solid solution phase was the only stable phase in the CrMnFeCoNi1.5 alloy, whilst the CrMnFeCo alloy formed the phase during solidification. The corresponding thermodynamic predictions varied dramatically from the experimentally observed microstructures, indicating that the underlying databases require further optimisation. Interestingly, it was found that a relatively simple electronic structure based approach, New PhaComp, provided much more accurate predictions of the observed phase formation in the CrMnFeCoNix and CrMnxFeCoNi systems and could be manipulated to obtain formation temperatures. As such, this method could be extremely useful to those wanting to design CrMnFeCoNi high entropy alloys that are free from the phase.

The routine and unique determination of minor phases in microstructures is critical to materials science. In metallurgy alone, applications include alloy and process development and the understanding of degradation in service. We develop a correlative method, exploring superalloy microstructures which are examined in the scanning electron microscope (SEM) using simultaneous energy dispersive X-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD). This is performed at an appropriate length scale for characterisation of carbide phases, shape, size, location, and distribution. EDS and EBSD data are generated using two different physical processes, but each provide a signature of the material interacting with the incoming electron beam. Recent advances in post-processing, driven by 'big data' approaches, include use of principal component analysis (PCA). Components are subsequently characterised to assign labels to a mapped region. To provide physically meaningful signals, the principal components may be rotated to control the distribution of variance. In this work, we develop this method further through a weighted PCA approach. We use the EDS and EBSD signals concurrently, thereby labelling each region using both EDS (chemistry) and EBSD (crystal structure) information. This provides a new method of amplifying signal-to-noise for very small phases in mapped regions, especially where the EDS or EBSD signal is not unique enough alone for classification.

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The α/β interface in Ti-6Al-2Sn-4Zr-6Mo (Ti-6246) is investigated via centre of symmetry analysis, both as-grown and after 10% cold work. Semi-coherent interface steps are observed at a spacing of 4.5 ±1.13 atoms in the as-grown condition, in good agreement with theory prediction (4.32 and 4.25 atoms). Lattice accommodation is observed, with elongation along [1210] α and contraction along [1010] α . Deformed α exhibited larger, less coherent steps with slip bands lying in {110} β . This indicates dislocation pile-up at the grain boundary, a precursor to globularisation, offering insight into the effect of deformation processing on the interface, which is important for titanium alloy processing route design.

A correlative approach is employed to simultaneously assess structure and chemistry of (carbide and boride) precipitates in a set of novel Co/Ni-base superalloys. Structure is derived from electron backscatter diffraction (EBSD) with pattern template matching, and chemistry obtained with energy dispersive X-ray spectroscopy (EDS). It is found that the principal carbide in these alloys is Mo and W rich with the M6C structure. An M2B boride also exhibiting Mo and W segregation is observed at B levels above approximately 0.085 at. pct. These phases are challenging to distinguish in an SEM with chemical information (EDS or backscatter Z-contrast) alone, without the structural information provided by EBSD. Only correlative chemical and structural fingerprinting is necessary and sufficient to fully define a phase. The identified phases are dissimilar to those predicted using ThermoCalc. We additionally perform an assessment of the grain boundary serratability in these alloys, and observe that significant amplitude is only obtained in the absence of pinning intergranular precipitates.