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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 × 300 × 300 μ 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 ∘ , 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 ≈ 0.003 to 0.006 ∘ . [ABSTRACT FROM AUTHOR]

Abstract: A novel synchrotron-based technique “high angular resolution 3DXRD” is presented in detail, and applied to the characterization of oxygen-free, high-conductivity copper at a tensile deformation of 2%. The position and shape in reciprocal space of 14 peaks originating from deeply embedded individual subgrains is reported. From this dataset the density of redundant dislocations in the individual subgrains is inferred to be below 12×1012 m−2 on average. It is found that the subgrains on average experience a reduction in strain of 0.9×10−4 with respect to the mean elastic strain of the full grain, a rather wide distribution of the strain difference between the subgrains (twice the standard deviation is 2.9×10−4), and a narrow internal strain distribution (upper limit is 2.4×10−4 full width at half maximum). [Copyright &y& Elsevier]

During plastic deformation of metals and alloys, dislocations arrange in ordered patterns. How and when these self-organization processes take place have remained elusive, because in situ observations have not been feasible. We present an x-ray diffraction method that provided data on the dynamics of individual, deeply embedded dislocation structures. During tensile deformation of pure copper, dislocation-free regions were identified. They showed an unexpected intermittent dynamics, for example, appearing and disappearing with proceeding deformation and even displaying transient splitting behavior. Insight into these processes is relevant for an understanding of the strength and work-hardening of deformed materials. [ABSTRACT FROM AUTHOR]

Abstract: Nucleation of recrystallization is studied in situ in the bulk by three-dimensional X-ray diffraction. Copper samples cold rolled 20% are investigated. The crystallographic orientations near triple junction lines are characterized before, during and after annealing. Three nuclei are identified and it is shown that two nuclei are twin related to their parent grain and one nucleus has an orientation, which is neither present in the deformed parent grains nor first order twin related to any of them. Data on the nucleation kinetics is also presented. [Copyright &y& Elsevier]

The aims of this study were to investigate possible sex differences in (a) intraoral pain evoked by topical application of capsaicin to the gingiva, and (b) the modulation of this pain by diffuse noxious inhibitory controls (DNIC). Three groups with a total of fifty-four healthy volunteers (20 men, 20 women using oral contraceptives (W+OC), 14 women not using (W-OC)) completed the study. In two sessions, intraoral pain was evoked by topical application of 30microL 5% capsaicin to the gingiva. Conditioning stimuli were applied with three min hand immersion in ice water in one session and 30 degrees C water (control) in another session. The capsaicin-evoked pain and the water-evoked pain were evaluated by the participants on visual analogue scales (VAS). No main effects of group in capsaicin-evoked pain (P>0.062) or water-evoked pain (P>0.149) were found. There was a significant group x time interaction (P<0.001) with W+OC reporting lower capsaicin-evoked pain scores than W-OC in the early phase (2-3min) and lower pain scores than men in the later phase (5-11min). The degree of modulation by DNIC did not differ between groups (P=0.636). In conclusion, for a superficial type of intraoral pain, only minor sex differences were found in pain intensity and no differences in the degree of endogenous modulation by DNIC. Female sex and the use of OC may not consistently be associated with higher sensitivity to pain. [ABSTRACT FROM AUTHOR]

Abstract: The aims of this study were to investigate possible sex differences in (a) intraoral pain evoked by topical application of capsaicin to the gingiva, and (b) the modulation of this pain by diffuse noxious inhibitory controls (DNIC). Three groups with a total of fifty-four healthy volunteers (20 men, 20 women using oral contraceptives (W+OC), 14 women not using (W−OC)) completed the study. In two sessions, intraoral pain was evoked by topical application of 30μL 5% capsaicin to the gingiva. Conditioning stimuli were applied with three min hand immersion in ice water in one session and 30°C water (control) in another session. The capsaicin-evoked pain and the water-evoked pain were evaluated by the participants on visual analogue scales (VAS). No main effects of group in capsaicin-evoked pain (P>0.062) or water-evoked pain (P>0.149) were found. There was a significant group x time interaction (P&#60;0.001) with W+OC reporting lower capsaicin-evoked pain scores than W−OC in the early phase (2–3min) and lower pain scores than men in the later phase (5–11min). The degree of modulation by DNIC did not differ between groups (P=0.636). In conclusion, for a superficial type of intraoral pain, only minor sex differences were found in pain intensity and no differences in the degree of endogenous modulation by DNIC. Female sex and the use of OC may not consistently be associated with higher sensitivity to pain. [Copyright &y& Elsevier]

A number of properties of amorphous materials including fatigue, fracture and component performance are governed by the magnitude of strain fields around inhomogeneities such as inclusions, voids and cracks. At present, localized strain information is only available from surface probes such as optical or electron microscopy. This is unfortunate because surface and bulk characteristics in general differ. Hence, to a large extent, the assessment of strain distributions relies on untested models. Here we present a universal diffraction method for characterizing bulk stress and strain fields in amorphous materials and demonstrate its efficacy by work on a material of current interest in materials engineering: a bulk metallic glass. The macroscopic response is shown to be less stiff than the atomic next-neighbour bonds because of structural rearrangements at the scale of 4–10 Å. The method is also applicable to composites comprising an amorphous matrix and crystalline inclusions. [ABSTRACT FROM AUTHOR]

The three-dimensional X-ray diffraction (3DXRD) method is reviewed. The method is based on the use of high-energy X-rays from synchrotron sources and a 'tomographic' approach to diffraction. With 3DXRD the structure of the embedded grains within polycrystals or powders can be characterised non-destructively within millimetre to centimetre size specimens. Algorithms are presented that determine the position, volume, orientation, stress and phase for hundreds of grains simultaneously. For non-deformed materials three-dimensional maps of the grains are generated with a resolution of 5 µm. Moreover, for the first time the dynamics of the individual grains can be studied in the bulk of the material. As examples of use of the method, in situ studies of recrystallisation, deformation and phase transformations are summarised. Furthermore, the multi-grain indexing program GRAINDEX provides an alternative route to structure solution and refinement, complementary to single crystal and powder diffraction. [ABSTRACT FROM AUTHOR]

The vasculature along conifer needles is fundamentally different from that in angiosperm leaves as it contains a unique transfusion tissue inside the bundle sheath. In this study, we used specific tracers to identify the pathway of photoassimilates from mesophyll to phloem, and the opposing pathway of nutrients from xylem to mesophyll. For symplasmic transport we applied esculin to the tip of attached pine needles and followed its movement down the phloem. For apoplasmic transport we let detached needles take up a membrane-impermeable contrast agent and used micro-X-ray computed tomography to map critical water exchange interfaces and domain borders. Microscopy and segmentation of the X-ray data enabled us to render and quantify the functional 3D structure of the water-filled apoplasm and the complementary symplasmic domain. The transfusion tracheid system formed a sponge-like apoplasmic domain that was blocked at the bundle sheath. Transfusion parenchyma cell chains bridged this domain as tortuous symplasmic pathways with strong local anisotropy which, as evidenced by the accumulation of esculin, pointed to the phloem flanks as the preferred phloem-loading path. Simple estimates supported a pivotal role of the bundle sheath, showing that a bidirectional movement of nutrient ions and assimilates is feasible and emphasizing the role of the bundle sheath in nutrient and assimilate exchange. [ABSTRACT FROM AUTHOR]

A nondestructive probe for mapping elastic strains within polymers would be an asset for materials engineering: for validation of mechanical models and for understanding damage nucleation. As a step towards this aim we demonstrate an X-ray wide angle diffraction methodology probing strain tensor components on mesoscopic length scales, in the range 3-50 Å. We demonstrate its use on a 50 % semi-crystalline polyethylene sample subjected to tensile straining up to 8.8 % . The mesoscopic strains derived for the crystalline phase scale linearly with the macroscopic strain, in contrast to the crystallised volume fraction and the texture evolution. In the crystalline phase, the material becomes softer and exhibit a larger degree of alignment with decreasing distance in direct space. The inherent strain sensitivity is 10 - 5 . The prospect of 3D mapping of local strain and stress tensors is discussed. [ABSTRACT FROM AUTHOR]

Polycrystals illuminated by high-energy X-rays or neutrons produce diffraction patterns in which the measured diffraction peaks encode the individual single crystal strain states. While state of the art X-ray and neutron diffraction approaches can be used to routinely recover per grain mean strain tensors, less work has been produced on the recovery of higher order statistics of the strain distributions across the individual grains. In the setting of small deformations, we consider the problem of estimating the crystal elastic strain tensor probability distribution from diffraction data. For the special case of multivariate Gaussian strain tensor probability distributions, we show that while the mean of the distribution is well defined from measurements, the covariance of strain has a null-space. We show that there exist exactly 6 orthogonal perturbations to this covariance matrix under which the measured strain signal is invariant. In particular, we provide analytical parametrisations of these perturbations together with the set of possible maximum-likelihood estimates for a multivariate Gaussian fit to data. The parametric description of the null-space provides insights into the strain PDF modes that cannot be accurately estimated from the diffraction data. Understanding these modes prevents erroneous conclusions from being drawn based on the data. Beyond Gaussian strain tensor probability densities, we derive an iterative radial basis regression scheme in which the strain tensor probability density is estimated by a sparse finite basis expansion. This is made possible by showing that the operator mapping the strain tensor probability density onto the measured histograms of directional strain is linear, without approximation. The utility of the proposed algorithm is demonstrated by numerical simulations in the setting of single crystal monochromatic X-ray scattering. The proposed regression methods were found to robustly reject outliers and accurately predict the strain tensor probability distributions in the presence of Gaussian measurement noise. [Display omitted] • Per-grain strain probability densities are extracted from X-ray diffraction data. • The presented method estimates the strain PDF from histograms of directional strain. • Gaussian strain PDFs have a closed form solutions and a known null-space. [ABSTRACT FROM AUTHOR]

Spectral X-ray Computed Tomography (CT) exploits advanced photon counting detectors (PCD) to measure a material's spectrally resolved linear attenuation coefficient (LAC) with the simultaneous spectral acquisition at multiple energy thresholds. We present a method for material classification using spectral CT. The method employs a basis material decomposition model and estimates the effective atomic number (Z eff) from the spectral LAC measurements. Basis material decomposition builds on the fact that the LAC of any material can be well approximated by a linear combination of LACs of basis materials, with known Z eff values at the extremes of the relevant Z eff range. Spectral distortions of the energy spectrum due to the physical interactions between photons and the multi-energy-bin PCD such as charge sharing and photon pileup are corrected by a spectral correction algorithm. The validation of the method has been performed with experimental data acquired with a custom laboratory instrument for spectral CT, examining "real life" phantoms with materials in the range of 6 ≤ Z eff ≤ 15. The classification performance is estimated for different numbers of projections, energy bins and basis materials in LAC decomposition. When using just 12 projections, 15 energy bins and two basis materials, the method gives a relative deviation of 2.2% for Z eff , while this deviation is 5.9% when spectral correction is not used. The classification method is now ready for use in security screening where modern spectral CT systems are employed. [ABSTRACT FROM AUTHOR]

We present the comparative study of the analytical forward model and the statistical simulation of the Compton single scatter in the positron emission tomography. The formula of the forward model has been obtained using the single scatter simulation approximation under simplified assumptions, and therefore we calculate scatter projections using independent Monte Carlo simulation mimicking the scatter physics. The numerical comparative study has been performed using a digital cylindrical phantom filled in with water and containing spherical sources of emission activity located at the central and several displaced positions. Good fits of the formula-based and statistically generated profiles of scatter projections are observed in the presented numerical results. [ABSTRACT FROM AUTHOR]

Most metals, ceramics, semiconductors and rocks are composed of small crystals known as grains. When annealed, this polycrystalline structure coarsens, thus allowing the properties of a material to be tailored for a particular application. The mobility of grain boundaries is thought to be determined by the crystallography of the adjacent crystals, but experimental validation in bulk polycrystalline materials is lacking. Here we developed a novel fitting methodology by direct comparison of a time-resolved three-dimensional experimental data to simulations of the evolution of 1501 grains in iron. The comparison allows reduced mobilities of 1619 grain boundaries to be determined simultaneously. We find that the reduced mobilities vary by three orders of magnitude and in general exhibit no correlation with the boundary's five macroscopic degrees of freedom, implying that grain growth is governed by other factors. [ABSTRACT FROM AUTHOR]

Placing a compound refractive lens (CRL) as an objective in a neutron beam generates new possibilities for 2D and 3D nondestructive mapping of the structure, strain and magnetic domains within extended objects. A condenser setup is introduced that allows correction for the lateral chromatic aberration. More generally, for full‐field microscopy the loss in performance caused by the chromatic aberration can be more than offset by introducing arrays of CRLs and exploiting the fact that the field of view can be much larger than the physical aperture of the CRL. Comments are made on the manufacture of such devices. The potential use is illustrated by comparisons between state‐of‐the‐art instrumentation and suggested approaches for bright‐field microscopy, small‐angle neutron scattering microscopy, grain mapping and mapping of stresses. Options are discussed for depth‐resolved imaging inspired by confocal light microscopy. Finally, experimental demonstrations are given of some of the basic properties of neutron full‐field imaging for a single CRL. [ABSTRACT FROM AUTHOR]

Grain evolution in pure iron is determined in three dimensions using diffraction contrast tomography at a synchrotron source. During annealing for 75 min at 800 ∘ C , the evolution of initially 1327 grains is quantified as a function of 15 time-steps. A comprehensive statistical analysis is provided based on the equivalent radius, the number of faces and the mean width parameters of the grains. We introduce analytical relations between these parameters, validate them, and discuss their physical meaning. While the sample is fully recrystallized, the growth is found not to be self-similar, as evidenced in changes in the distributions of normalized grain size and number of faces per grain. More importantly, a strong decrease in the slope of the growth rate over the mean width of grain faces is observed, indicating a slowdown of grain growth. The data is used to determine the applicability of the isotropic MacPherson-Srolovitz theory to an anisotropic material such as iron. Geometrical properties that are averaged over the entire grain ensemble are well described by the model, but the properties and evolution of the individual grains exhibit substantial scatter. [ABSTRACT FROM AUTHOR]

A method to determine material parameters by comparing the evolution of experimentally determined 3D microstructures to simulated 3D microstructures is proposed. The temporal evolution of a dendritic solid-liquid mixture is acquired in situ using x-ray tomography. Using a time step from these data as an initial condition in a phase-field simulation, the computed structure is compared to that measured experimentally at a later time. An optimization technique is used to find the material parameters that yield the best match of the simulated microstructure to the measured microstructure in a global manner. The proposed method is used to determine the liquid diffusion coefficient in an isothermal Al-Cu alloy. However, the method developed is broadly applicable to other experiments in which the evolution of the three-dimensional microstructure is determined in situ. We also discuss methods to describe the local variation of the best-fit parameters and the fidelity of the fitting. We find a liquid diffusion coefficient that is different from that measured using directional solidification. [ABSTRACT FROM AUTHOR]

The development of energy resolving photon counting detectors (PCD) has paved the way to spectral X-ray Computed Tomography (CT), with which one can simultaneously extract the energy dependence of a material's linear attenuation coefficient (LAC). Spectral CT has proved to be an advanced technique to classify materials based on their physical properties such as electron density (ρ e) and effective atomic number (Z eff). However, the application of spectral CT may be hindered by the poor image reconstruction quality when used for material identification in security screening where rapid scanning is required. Image reconstruction from few projections or low radiation exposure time would enable rapid scanning. The reconstruction quality for each energy bin may also be degraded since the division of photon counts into multiple energy bins naturally leads to higher noise levels. In this work, we explore how to perform accurate spectral CT reconstructions from such data, and propose L ∞ norm-based vectorial total variation (L ∞ -VTV) regularization that uses correlations between multiple energy bins. Using experimental data acquired with a custom laboratory instrument for spectral CT, the L ∞ -VTV is tested on "real life" phantoms consisting of materials in the range of 6 ≤ Z eff ≤ 15. For material classification from only 7 projections, the L ∞ -VTV gives the relative deviations of 3.5% for ρ e and 2.4% for Z eff , whereas the total nuclear variation (TNV) of another state-of-the-art joint reconstruction and the total variation (TV) yield those of 3.4% and 3.1%, and 3.8% and 4.2%, respectively. The L ∞ -VTV is now ready for use in security screening. • A joint reconstruction algorithm with L infinity norm improves image reconstruction. • The algorithm is robust to few projections and/or low photon counts. • Using correlations between multiple energy bins enhances material identification. • L infinity norm in the algorithm leads to suppression of outliers in gradient magnitudes. • High noise levels in specific energy bins can be alleviated using unaffected bins. [ABSTRACT FROM AUTHOR]

• 3D X-ray diffraction yields per-grain strain, texture, twin relations and structure. • Applicable to a broad scope of functional polycrystalline materials. • Demonstrated by application to a kesterite (CZTS) thin film solar cell. • CZTS is a technologically interesting case with complex phase composition. • 3DXRD may detect and characterize secondary phases not otherwise distinguishable. [Display omitted] The non-destructive structural characterization of individual grains in thin-films photovoltaics based on polycrystalline materials is a powerful tool for revealing important details of the microstructure of solar cell absorbers. Here, we use three-dimensional X-ray diffraction (3DXRD) to obtain statistics on the phase, size, orientation and strain tensors of the grains, as well as their twin relations in Cu 2 ZnSnS 4 (CZTS) absorbers. Moreover, this powerful approach allows the non-ambiguous determination of phases with distinct optical and electrical properties but similar lattice parameters, such as CZTS and ZnS. Our analysis over cumulative statistics of nearly 600 grains in polycrystalline CZTS reveals that a fraction of 2.5% corresponds to the ZnS secondary phase. Statistics of the strain distribution in the polycrystalline CZTS layer indicate an average tensile stress in the plane of the film of ~70 MPa and a compressive stress along the normal to the film of ~145 MPa. We found that 41% of the total number of grains in CZTS absorbers are Σ3 twins. We calculate the frequency of the six types of Σ3 boundaries, revealing that the 180° rotation along the axis<221>is the most frequent. Accessing the microstructure opens the possibility to study its influence on the properties of the film, such as bandgap variations due to strain or the role of twin boundaries in the charge transport mechanisms. [ABSTRACT FROM AUTHOR]

The article discusses a research study which examines the usefulness of multiple crystals in collecting X-ray diffraction data simultaneously from assemblies of up to seven crystals with regard to macromolecular crytallography. It describes the features of the algorithms used to extract data and their practical implementation. It explains that this procedure could be of good use to obtain data on intergrown crystals and deal with rapid diffraction decay.

A variety of features broadly classed as deformation microstructure elements are created during the plastic deformation of polycrystalline metals. While virtually all elements of deformation microstructure are composed of dislocations, describing the creation and evolution of larger-scale elements in terms of interactions between individual dislocations is a goal that has not yet been achieved. A hierarchical approach is thus favored in which structure creation and evolution are described at a range of length scales, from the nanometer to millimeter scale. [Copyright &y& Elsevier]

First results are presented on the simultaneous observation of the elastic strain tensor as a function of load of 10 individual grains, deeply embedded in the bulk of a polycrystalline Al tensile sample. The experimental technique is based on the use of focused high energy synchrotron radiation in transmission geometry. After each load step diffraction patterns are collected with a large-area X-ray detector system for a series of different angular and lateral sample positions. An automated indexing routine was used to assign sets of diffraction spots to individual grains. The strain tensor components as well as the individual grain position within the sample were then fitted from the diffraction spot positions. A maximum tensile load of 48 MPa was applied. Deviations in strain of up to 600 × 10-6 are observed between respective strain components of individual grains. [Copyright &y& Elsevier]

Studies the structural factors of YBa[sub 2]Cu[sub 3]O[sub 6.98] using high-energy synchrotron radiation. Derivation of charge densities using generalized structure factors and VALRAY; Comparison of the charge densities with densities refined from theoretical structure factors; Refinement agreement indices for the experimental and for the theoretical data set.

We present a method for material classifications in spectral X-ray Computed Tomography (SCT) taking advantage of energy-resolving 2D detectors to simultaneously extract the energy dependence of a material's linear attenuation coefficient (LAC). The method employs an attenuation decomposition presented by Alvarez et al., and estimates system-independent material properties of electron density (ρ e) and effective atomic number (Z eff), independent of the scanner, from the energy-dependent LAC measurements. The method uses a spectral correction algorithm and the energy range is truncated to exclude bins with photon starvation and spectral distortion present even after correction of detector response. A novel technique of energy bin selection is used for optimized classification performance. The method is tested against another SCT classification method called SRZE for inspecting materials in the range of 6 ≤ Z eff ≤ 23. Our method aims at an increase in the speed of pot processing workflow after the data acquisition, and it achieves explicitly up to 32 times better time efficiency for the reconstruction with comparable accuracy for a range of materials important in threat detection. • Just two spectral detector energy bins needed for accurate material identification. • Correction of the spectral detector response is required for accurate classification. • The low- to high-energy threshold are optimized above 100 keV. • Non-overlapping energy bins improve classification performance. [ABSTRACT FROM AUTHOR]