Correlating Atom Probe Crystallographic Measurements with Transmission Kikuchi Diffraction Data.

Correlative microscopy approaches offer synergistic solutions to many research problems. One such combination, that has been studied in limited detail, is the use of atom probe tomography (APT) and transmission Kikuchi diffraction (TKD) on the same tip specimen. By combining these two powerful microscopy techniques, the microstructure of important engineering alloys can be studied in greater detail. For the first time, the accuracy of crystallographic measurements made using APT will be independently verified using TKD. Experimental data from two atom probe tips, one a nanocrystalline Al-0.5Ag alloy specimen collected on a straight flight-path atom probe and the other a high purity Mo specimen collected on a reflectron-fitted instrument, will be compared. We find that the average minimum misorientation angle, calculated from calibrated atom probe reconstructions with two different pole combinations, deviate 0.7° and 1.4°, respectively, from the TKD results. The type of atom probe and experimental conditions appear to have some impact on this accuracy and the reconstruction and measurement procedures are likely to contribute further to degradation in angular resolution. The challenges and implications of this correlative approach will also be discussed.

Quaternion-based disorientation coloring of orientation maps.

The authors of the present work propose a color coding technique using quaternions for the display of crystallographic orientation data such as EBSD maps. The main difference to existing color coding techniques in this field is that it creates a color space, within which the perceived color differences are approximately proportional to Euclidean distances in the corresponding 3D quaternion vector space, and thus approximately proportional to mutual disorientation angles. Since all disorientation parameters (axis and angle pairs, but represented as quaternions) are taken into account, color ambiguities appearing in maps created by other techniques are successfully avoided, and the sub-grain orientation differences within grains can be unambiguously visualized.

Insights into the Silver Reflection Layer of a Vertical LED for Light Emission Optimization.

In this work, Ag as a highly reflective mirror layer of gallium nitride (GaN)-based blue vertical light-emitting diodes (VLEDs) has been systematically investigated by correlating scanning electron microscopy/energy dispersive X-ray spectroscopy/transmission Kikuchi diffraction/electron backscatter diffraction, aberration-corrected scanning transmission electron microscopy, and atomic force microscopy techniques. In the context of high-efficiency lighting, three critical aspects have been scrutinized on the nanoscale: (1) chemical diffusion, (2) grain morphology, and (3) surface topography of the Ag layer. We found that nanoscale inhomogeneous distribution of In in InGaN/GaN quantum wells (QWs), interfacial diffusion (In/Ga out-diffusion into the Ag layer and diffusion of Ag into p-GaN and QWs), and Ag agglomeration deteriorate the light reflectivity, which account for the decreased luminous efficiency in VLEDs. Meanwhile, the surface morphology and topographical analyses revealed the nanomorphology of the Ag layer, where a nanograin size of ∼300 nm with special nanotwinned boundaries and an extremely smooth surface of ∼3-4 nm are strongly desired for better reflectivity. Further, on the basis of these microscopy results, suggestions on light extraction optimization are given to improve the performance of GaN-based blue VLEDs. Our findings enable fresh and deep understanding of performance-microstructure correlation of LEDs on the nanoscale, providing guidance to the design and manufacture of high-performance LED devices.

Effect of triple junctions on deformation twinning in a nanostructured Cu-Zn alloy: A statistical study using transmission Kikuchi diffraction.

Scanning electron microscopy transmission Kikuchi diffraction is able to identify twins in nanocrystalline material, regardless of their crystallographic orientation. In this study, it was employed to characterize deformation twins in Cu/10 wt % Zn processed by high-pressure torsion. It was found that in 83% of grains containing twins, at least one twin intersects with a triple junction. This suggests that triple junctions could have promoted the nucleation of deformation twins. It should be cautioned that this technique might be unable to detect extremely small nanoscale twins thinner than its step size.

Orientation mapping of nanostructured materials using transmission Kikuchi diffraction in the scanning electron microscope.

In this study, the new technique of transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) has been applied for the first time to enable orientation mapping of bulk, nanostructured metals. The results show how the improved spatial resolution of SEM-TKD, compared to conventional EBSD, enables reliable mapping of truly nanostructured metals and alloys, with mean grain sizes in the 40-200 nm range. The spatial resolution of the technique is significantly below 10nm, and contrasting examples are shown from both dense (Ni) and lighter (Al-alloy) materials. Despite the burden of preparing thin, electron-transparent samples, orientation mapping using SEM-TKD is likely to become invaluable for routine characterisation of nanocrystalline and, potentially, highly deformed microstructures.

The first occurrence in the fossil record of an aquatic avian twig-nest with Phoenicopteriformes eggs: evolutionary implications.

BACKGROUND: We describe the first occurrence in the fossil record of an aquatic avian twig-nest with five eggs in situ (Early Miocene Tudela Formation, Ebro Basin, Spain). Extensive outcrops of this formation reveal autochthonous avian osteological and oological fossils that represent a single taxon identified as a basal phoenicopterid. Although the eggshell structure is definitively phoenicopterid, the characteristics of both the nest and the eggs are similar to those of modern grebes. These observations allow us to address the origin of the disparities between the sister taxa Podicipedidae and Phoenicopteridae crown clades, and traces the evolution of the nesting and reproductive environments for phoenicopteriforms. METHODOLOGY/PRINCIPAL FINDINGS: Multi-disciplinary analyses performed on fossilized vegetation and eggshells from the eggs in the nest and its embedding sediments indicate that this new phoenicopterid thrived under a semi-arid climate in an oligohaline (seasonally mesohaline) shallow endorheic lacustine environment. High-end microcharacterizations including SEM, TEM, and EBSD techniques were pivotal to identifying these phoenicopterid eggshells. Anatomical comparisons of the fossil bones with those of Phoenicopteriformes and Podicipediformes crown clades and extinct palaelodids confirm that this avian fossil assemblage belongs to a new and basal phoenicopterid. CONCLUSIONS/SIGNIFICANCE: Although the Podicipediformes-Phoenicopteriformes sister group relationship is now well supported, flamingos and grebes exhibit feeding, reproductive, and nesting strategies that diverge significantly. Our multi-disciplinary study is the first to reveal that the phoenicopteriform reproductive behaviour, nesting ecology and nest characteristics derived from grebe-like type strategies to reach the extremely specialized conditions observed in modern flamingo crown groups. Furthermore, our study enables us to map ecological and reproductive characters on the Phoenicopteriformes evolutionary lineage. Our results demonstrate that the nesting paleoenvironments of flamingos were closely linked to the unique ecology of this locality, which is a direct result of special climatic (high evaporitic regime) and geological (fault system) conditions.