Search

At two-thirds the weight of aluminum, magnesium alloys have the potential to significantly reduce the fuel consumption of transportation vehicles. These advancements depend on our ability to optimize the desirable versus undesirable effects of deformation twins: three dimensional (3D) microstructural domains that form under mechanical stresses. Previously only characterized using surface or thin-film measurements, here, we present the first 3D in-situ characterization of deformation twinning inside an embedded grain over mesoscopic fields of view using dark-field X-ray microscopy supported by crystal plasticity finite element analysis. The results reveal the important role of triple junctions on twin nucleation, that twin growth behavior is irregular and can occur in several directions simultaneously, and that twin-grain and twin-twin junctions are the sites of localized dislocation accumulation, a necessary precursor to crack initiation.

During plastic deformation of metals and alloys, dislocations self-organise in cells, which subsequently continuously decrease in size. How and when these processes take place has remained elusive, because observations of the structural dynamics in the bulk have not been feasible. We here present X-ray diffraction microscopy movies of the structural evolution during tensile deformation of a mm-sized aluminium (111) single crystal. The formation and subsequent development of 40,000 cells are visualised. We reveal that cells form in a stochastic and isotropic manner already at 1% strain. We show that the cell size and dislocation density distributions are log-normal and bi-modal Gaussian distributions, respectively, throughout. This insight leads to an interpretation of the formation and evolution steps in terms of universal stochastic multiplicative processes. This work will guide dislocation dynamics modelling, as it provides unique results on cell formation.

NaNbO3-based antiferroelectric materials offer a promising pathway towards greener and more cost-effective energy storage devices. However, their intrinsic structural instabilities often lead to reduced energy density that compromises their performance and longevity. In this brief communication, we demonstrate how Dark-Field X-ray Microscopy, when carried out on the characteristically weak 1/4{843}pc superstructure reflection, can map the antiferroelectric phase and its strain heterogeneity in typically small, deeply-embedded grains of a NaNbO3 and 0.95NaNbO3-0.05SrSnO3 ceramics, representative of different phase transition behavior. Our results clearly evidences the stabilizing effect of SrSnO3 on the antiferroelectric phase by enhancing the degree of mesostructural order. In doing so, our method establishes a new platform for exploring the impact of disorder on the long-range strain heterogeneity within antiferroelectrics and other materials with modulated crystal structures., Comment: 11 pages, 4 figures

Dislocation patterning and self-organization during plastic deformation are associated with work hardening, but the exact mechanisms remain elusive. This is partly because studies of the structure and local strain during the initial stages of plastic deformation has been a challenge. Here we use Dark Field X-ray Microscopy to generate 3D maps of embedded $350 \times 900 \times 72 \,\mu\mathrm{m}^3$ volumes within three pure Al single crystals, all oriented for double slip on the primary and conjugate slip systems. These were tensile deformed by 0.6$\%$, 1.7$\%$ and 3.6$\%$, respectively. Orientation maps revealed the existence of two distinct types of planar dislocation boundaries both at 0.6$\%$ and 1.7$\%$ but no systematic patterning. At 3.6$\%$, these boundaries have evolved into a well-defined checkerboard pattern, characteristic of Geometrically Necessary Boundaries, GNBs. The GNB spacing is $\approx$ 14 $\mu$m and the misorientation $\approx$ 0.2{\deg}, in fair agreement with those at higher strains. By contrast to the sharp boundaries observed at higher strains, the boundaries are associated with a sinusoidal orientation gradient. Maps of the elastic strain along the (111) direction exhibit fluctuations of $\pm 0.0002 $ with an average domain size of 3 $\mu$m.

The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, Dark Field X-ray Microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the $10^{12}$ photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.

Thermomechanical processing such as annealing is one of the main methods to tailor the mechanical properties of materials, however, much is unknown about the reorganization of dislocation structures deep inside macroscopic crystals that give rise to those changes. Here, we demonstrate the self-organization of dislocation structures upon high-temperature annealing in a mm-sized single crystal of aluminum. We map a large embedded 3D volume ($100\times300\times300$ $\mu $m$^3$) of dislocation structures using dark field x-ray microscopy (DFXM), a diffraction-based imaging technique. Over the wide field of view, DFXM's high angular resolution allows us to identify subgrains, separated by dislocation boundaries, which we identify and characterize down to the single-dislocation level using computer-vision methods. We demonstrate how even after long annealing times at high temperatures, the remaining low density of dislocations still pack into well-defined, straight dislocation boundaries (DBs) that lie on specific crystallographic planes. In contrast to conventional grain growth models, our results show that the dihedral angles at the triple junctions are not the predicted 120$\degree$, suggesting additional complexities in the boundary stabilization mechanisms. Mapping the local misorientation and lattice strain around these boundaries shows that the observed strain is shear, imparting an average misorientation around the DB of $\approx 0.003-0.006 \degree{}$

A Python package for the analysis of dark-field X-ray microscopy (DFXM) and rocking curve imaging (RCI) data is presented. \textit{darfix} provides a set of data processing and visualization tools that can be either imported as library components or accessed through a graphical user interface (GUI) as an Orange add-on. In the latter case, the different analysis modules can be easily chained to define computational workflows. Operations on larger-than-memory image sets are supported through the implementation of online versions of the data processing algorithms, effectively trading performance for feasibility when the computing resources are limited. The software can automatically extract the relevant instrument angle settings from the input files metadata. The currently available input file format is EDF and in future releases HDF5 will be incorporated., Comment: A data analysis package intended for x-ray imaging. The manuscript is to be submitted to Journal of Synchrotron Radiation

Dark-Field X-ray Microscopy (DFXM) is a diffraction-based synchrotron imaging techique capable of imaging defects in the bulk of extended crystalline samples. We present numerical simulations of image-formation in such a microscope using numerical integration of the dynamical Takagi-Taupin Equations (TTE) and wave front propagation. We validate our approach by comparing simulated images to experimental data from a near-perfect single crystal of diamond containing a single stacking fault defect in the illuminated volume.

Connecting a bulk material's microscopic defects to its macroscopic properties is an age-old problem in materials science. Long-range interactions between dislocations (line defects) are known to play a key role in how materials deform or melt, but we lack the tools to connect these dynamics to the macroscopic properties. We introduce time-resolved dark-field X-ray microscopy to directly visualize how dislocations move and interact over hundreds of micrometers, deep inside bulk aluminum. With real-time movies, we reveal the thermally-activated motion and interactions of dislocations that comprise a boundary, and show how weakened binding forces inhomogeneously destabilize the structure at 99% of the melting temperature. Connecting dynamics of the microstructure to its stability, we provide important opportunities to guide and validate multiscale models that are yet untested.

Pressure induced structural modifications in vitreous Ge$_{x}$Se$_{100-x}$ (where 10 $\leq$ x $\leq$ 25)are investigated using X-ray absorption spectroscopy (XAS) along with supplementary X-ray diffraction (XRD) experiments and ab initio molecular dynamics (AIMD) simulations. Universal changes in distances and angle distributions are observed when scaled to reduced densities. All compositions are observed to remain amorphous under pressure values up to 42 GPa. The Ge-Se interatomic distances extracted from XAS data show a two-step response to the applied pressure; a gradual decrease followed by an increase at around 15-20 GPa, depending on the composition. This increase is attributed to the metallization event that can be traced with the red shift in Ge K edge energy which is also identified by the principal peak position of the structure factor. The densification mechanisms are studied in details by means of AIMD simulations and compared to the experimental results. The evolution of bond angle distributions, interatomic distances and coordination numbers are examined and lead to similar pressure-induced structural changes for any composition.