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Strength, ductility, and failure properties of metals are tailored by plastic deformation routes. Predicting these properties requires modeling of the structural dynamics and stress evolution taking place on several length scales. Progress has been hampered by a lack of representative 3D experimental data at industrially relevant degrees of deformation. We present an X-ray imaging based 3D mapping of an aluminum polycrystal deformed to the ultimate tensile strength (32% elongation). The extensive dataset reveals significant intra-grain stress variations (36 MPa) up to at least half of the inter-grain variations (76 MPa), which are dominated by grain orientation effects. Local intra-grain stress concentrations are candidates for damage nucleation. Such data are important for models of structure-property relations and damage., (© 2024. The Author(s).)

Dark-field X-ray microscopy (DFXM) is a full-field imaging technique that non-destructively maps the structure and local strain inside deeply embedded crystalline elements in three dimensions. In DFXM, an objective lens is placed along the diffracted beam to generate a magnified projection image of the local diffracted volume. This work explores contrast methods and optimizes the DFXM setup specifically for the case of mapping dislocations. Forward projections of detector images are generated using two complementary simulation tools based on geometrical optics and wavefront propagation, respectively. Weak and strong beam contrast and the mapping of strain components are studied. The feasibility of observing dislocations in a wall is elucidated as a function of the distance between neighbouring dislocations and the spatial resolution. Dislocation studies should be feasible with energy band widths of 10 -2 , of relevance for fourth-generation synchrotron and X-ray free-electron laser sources., (© Sina Borgi et al. 2024.)

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., (© The Author(s) 2023. Published by Oxford University Press on behalf of the Society for Experimental Biology. All rights reserved. For permissions, please email: journals.permissions@oup.com.)

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 [Formula: see text] 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., (© 2023. Springer Nature Limited.)

Liquid plays an important role in bone that has a complex 3D hierarchical pore structure. However, liquid (water) is difficult to discern from e.g. an organic matrix by X-ray imaging. Therefore, we use a correlative approach using both high resolution X-ray and neutron imaging. Human femoral bone with liquid adsorbed into some of the pores was imaged with both the Neutron Microscope at the ICON beamline, SINQ at PSI, and by lab-based μCT using 2.7 μm voxel size. Segmentation of the two datasets showed that, even though the liquid was clearly distinguishable in the neutron data and not in the X-ray data, it remained challenging to segment it from bone due to overlaps of peaks in the gray level histograms. In consequence, segmentations from X-ray and neutron data varied significantly. To address this issue, the segmented X-ray porosities was overlaid on the neutron data, making it possible to localize the liquid in the vascular porosities of the bone sample and use the neutron attenuation to identify it as H 2 O. The contrast in the neutron images was lowered slightly between the bone and the liquid compared to the bone and the air. This correlative study shows that the complementary use of X-rays and neutrons is very favorable, since H 2 O is very distinct in the neutron data, while D 2 O, H 2 O, and organic matter can barely be distinguished from air in the X-ray data., Competing Interests: Declaration of competing interest None., (Copyright © 2023 The Author(s). Published by Elsevier Inc. All rights reserved.)

The dynamics of lattice vibrations govern many material processes, such as acoustic wave propagation, displacive phase transitions, and ballistic thermal transport. The maximum velocity of these processes and their effects is determined by the speed of sound, which therefore defines the temporal resolution (picoseconds) needed to resolve these phenomena on their characteristic length scales (nanometers). Here, we present an X-ray microscope capable of imaging acoustic waves with subpicosecond resolution within mm-sized crystals. We directly visualize the generation, propagation, branching, and energy dissipation of longitudinal and transverse acoustic waves in diamond, demonstrating how mechanical energy thermalizes from picosecond to microsecond timescales. Bulk characterization techniques capable of resolving this level of structural detail have previously been available on millisecond time scales-orders of magnitude too slow to capture these fundamental phenomena in solid-state physics and geoscience. As such, the reported results provide broad insights into the interaction of acoustic waves with the structure of materials, and the availability of ultrafast time-resolved dark-field X-ray microscopy opens a vista of new opportunities for 3D imaging of materials dynamics on their intrinsic submicrosecond time scales.

The use of a phase-retrieval technique for propagation-based phase-contrast neutron imaging with a polychromatic beam is demonstrated. This enables imaging of samples with low absorption contrast and/or improving the signal-to-noise ratio to facilitate e.g. time-resolved measurements. A metal sample, designed to be close to a phase pure object, and a bone sample with canals partially filled with D 2 O were used for demonstrating the technique. These samples were imaged with a polychromatic neutron beam followed by phase retrieval. For both samples the signal-to-noise ratios were significantly improved and, in the case of the bone sample, the phase retrieval allowed for separation of bone and D 2 O, which is important for example for in situ flow experiments. The use of deuteration contrast avoids the use of chemical contrast enhancement and makes neutron imaging an interesting complementary method to X-ray imaging of bone., (© Maja Østergaard et al. 2023.)

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 ([Formula: see text] [Formula: see text]m[Formula: see text]) 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[Formula: see text], 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 [Formula: see text] 0.003 to 0.006[Formula: see text]., (© 2023. The Author(s).)

Three-dimensional X-ray diffraction microscopy, 3DXRD, has become an established tool for orientation and strain mapping of bulk polycrystals. However, it is limited to a finite spatial resolution of ∼1.5-3 µm. Presented here is a high-resolution modality of the technique, HR-3DXRD, for 3D mapping of submicrometre-sized crystallites or subgrains with high spatial and angular resolution. Specifically, the method is targeted to visualization of metal microstructures at industrially relevant degrees of plastic deformation. Exploiting intrinsic crystallographic properties of such microstructures, the high resolution is obtained by placing a high-resolution imaging detector in between the near-field and far-field regimes. This configuration enables 3D mapping of deformation microstructure by determining the centre of mass and volume of the subgrains and generating maps by tessellation. The setup is presented, together with a data analysis approach. Full-scale simulations are used to determine limitations and to demonstrate HR-3DXRD on realistic phantoms. Misalignments in the setup are shown to cause negligible shifts in the position and orientation of the subgrains. Decreasing the signal-to-noise ratio is observed to lead primarily to a loss in the number of determined diffraction spots. Simulations of an α-Fe sample deformed to a strain of ε vM = 0.3 and comprising 828 subgrains show that, despite the high degree of local texture, 772 of the subgrains are retrieved with a spatial accuracy of 0.1 µm and an orientation accuracy of 0.0005°., (© M. Kutsal et al. 2022.)

Purpose: Photon counting imaging detectors (PCD) has paved the way for spectral x-ray computed tomography (spectral CT), which simultaneously measures a sample's linear attenuation coefficient (LAC) at multiple energies. However, cadmium telluride (CdTe)-based PCDs working under high flux suffer from detector effects, such as charge sharing and photon pileup. These effects result in the severe spectral distortions of the measured spectra and significant deviation of the extracted LACs from the reference attenuation curve. We analyze the influence of the spectral distortion correction on material classification performance. Approach: We employ a spectral correction algorithm to reduce the primary spectral distortions. We use a method for material classification that measures system-independent material properties, such as electron density, ρ e , and effective atomic number, Z eff . These parameters are extracted from the LACs using attenuation decomposition and are independent of the scanner specification. The classification performance with the raw and corrected data is tested on different numbers of energy bins and projections and different radiation dose levels. We use experimental data with a broad range of materials in the range of 6 ≤ Z eff ≤ 15 , acquired with a custom laboratory instrument for spectral CT. Results: We show that using the spectral correction leads to an accuracy increase of 1.6 and 3.8 times in estimating ρ e and Z eff , respectively, when the image reconstruction is performed from only 12 projections and the 15 energy bins approach is used. Conclusions: The correction algorithm accurately reconstructs the measured attenuation curve and thus gives better classification performance., (© 2022 Society of Photo-Optical Instrumentation Engineers (SPIE).)

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 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., (Copyright © 2021 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works. Distributed under a Creative Commons Attribution NonCommercial License 4.0 (CC BY-NC).)

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.

We report on a new X-ray imaging method, which generalizes Bragg ptychography to 3D mapping of embedded crystalline volumes within thick specimens. The sample is probed by a pencil X-ray beam. The diffracted beam is magnified by an objective and passes through a slit in the image plane to be monitored by a 2D detector in the far-field of the image plane. The dimensions of the incoming beam and the slit opening define a confocal Bragg volume. Scanning the sample with respect to this probe volume, an iterative oversampling routine is used to reconstruct the shape and projected displacement field of extended internal volumes. This routine takes into account the pupil function and known aberrations of the lens. We demonstrate the method by a numerical study of a 3.5 µm grain comprising a wall of edge dislocations. With a probe volume of ∼0.12 µm 3 and a compound refractive lens with a numerical aperture of 0.49×10 -3 as the objective, the dislocations are fully resolved with a displacement sensitivity of ∼10 pm. The spatial resolution is 26×27×123 nm 3 (rms), with the poor resolution along the optical axis being limited by the probe size. With a four times larger numerical aperture, the resolution becomes 16×8×123 nm 3 (rms). The lens aberrations are found to be not critical.

Non-destructive orientation mapping is an important characterization tool in materials science and geoscience for understanding and/or improving material properties based on their grain structure. Confocal Raman microscopy is a powerful non-destructive technique for chemical mapping of organic and inorganic materials. Here we demonstrate orientation mapping by means of Polarized Raman Microscopy (PRM). While the concept that PRM is sensitive to orientation changes is known, to our knowledge, an actual quantitative orientation mapping has never been presented before. Using a concept of ambiguity-free orientation determination analysis, we present fast and quantitative single-acquisition Raman-based orientation mapping by simultaneous registration of multiple Raman scattering spectra obtained at different polarizations. We demonstrate applications of this approach for two- and three-dimensional orientation mapping of a multigrain semiconductor, a pharmaceutical tablet formulation and a polycrystalline sapphire sample. This technique can potentially move traditional X-ray and electron diffraction type experiments into conventional optical laboratories.

The misfit dislocations formed at heteroepitaxial interfaces create long-ranging strain fields in addition to the epitaxial strain. For systems with strong lattice coupling, such as ferroic oxides, this results in unpredictable and potentially debilitating functionality and device performance. In this work, we use dark-field X-ray microscopy to map the lattice distortions around misfit dislocations in an epitaxial film of bismuth ferrite (BiFeO 3 ), a well-known multiferroic. We demonstrate the ability to precisely quantify weak, long-ranging strain fields and their associated symmetry lowering without modifying the mechanical state of the film. We isolate the screw and edge components of the individual dislocations and show how they result in weak charge heterogeneities via flexoelectric coupling. We show that even systems with small lattice mismatches and additional mechanisms of stress relief (such as mechanical twinning) may still give rise to measurable charge and strain heterogeneities that extend over mesoscopic length scales. This sets more stringent physical limitations on device size, dislocation density, and the achievable degree of lattice mismatch in epitaxial systems.

X-ray microscopy at photon energies above 15 keV is very attractive for the investigation of atomic and nanoscale properties of technologically relevant structural and bio materials. This method is limited by the quality of X-ray optics. Multilayer Laue lenses (MLLs) have the potential to make a major impact in this field because, as compared to other X-ray optics, they become more efficient and effective with increasing photon energy. In this work, MLLs were utilized with hard X-rays at photon energies up to 34.5 keV. The design, fabrication, and performance of these lenses are presented, and their application in several imaging configurations is described. In particular, two "full field" modes of imaging were explored, which provide various contrast modalities that are useful for materials characterisation. These include point projection imaging (or Gabor holography) for phase contrast imaging and direct imaging with both bright-field and dark-field illumination. With high-efficiency MLLs, such modes offer rapid data collection as compared with scanning methods as well as a large field of views.

Bragg coherent diffraction imaging (BCDI) is a powerful X-ray imaging technique for crystalline materials, providing high resolution maps of structure and strain. The technique is typically used to study a small isolated object, and is in general not compatible with a bulk polycrystalline sample, due to overlap of diffraction signals from various crystalline elements. In this paper, we present an imaging method for bulk samples, based on the use of a coherent source. The diffracted X-ray beam from a grain or domain of choice is magnified by an objective before being monitored by a 2D detector in the far field. The reconstruction principle is similar to the case of BCDI, while taking the magnification and pupil function into account. The concept is demonstrated using numerical simulations and reconstructions. We find that by using an object-lens distance shorter than the focal length, the numerical aperture is larger than in a traditional imaging geometry, and at the same time the setup is insensitive to small phase errors by lens imperfections. According to our simulations, we expect to be able to achieve a spatial resolution smaller than 20 nm when using the objective lens in this configuration.

The characteristic functionality of ferroelectric materials is due to the symmetry of their crystalline structure. As such, ferroelectrics lend themselves to design approaches that manipulate this structural symmetry by introducing extrinsic strain. Using in situ dark-field X-ray microscopy to map lattice distortions around deeply embedded domain walls and grain boundaries in BaTiO 3 , we reveal that symmetry-breaking strain fields extend up to several micrometres from domain walls. As this exceeds the average domain width, no part of the material is elastically relaxed, and symmetry is universally broken. Such extrinsic strains are pivotal in defining the local properties and self-organization of embedded domain walls, and must be accounted for by emerging computational approaches to material design.

The fractional Fourier transform (FrFT) is introduced as a tool for numerical simulations of X-ray wavefront propagation. By removing the strict sampling requirements encountered in typical Fourier optics, simulations using the FrFT can be carried out with much decreased detail, allowing, for example, on-line simulation during experiments. Moreover, the additive index property of the FrFT allows the propagation through multiple optical components to be simulated in a single step, which is particularly useful for compound refractive lenses (CRLs). It is shown that it is possible to model the attenuation from the entire CRL using one or two effective apertures without loss of accuracy, greatly accelerating simulations involving CRLs. To demonstrate the applicability and accuracy of the FrFT, the imaging resolution of a CRL-based imaging system is estimated, and the FrFT approach is shown to be significantly more precise than comparable approaches using geometrical optics. Secondly, it is shown that extensive FrFT simulations of complex systems involving coherence and/or non-monochromatic sources can be carried out in minutes. Specifically, the chromatic aberrations as a function of source bandwidth are estimated, and it is found that the geometric optics greatly overestimates the aberration for energy bandwidths of around 1%.

A comprehensive optical description of compound refractive lenses (CRLs) in condensing and full-field X-ray microscopy applications is presented. The formalism extends ray-transfer matrix analysis by accounting for X-ray attenuation by the lens material. Closed analytical expressions for critical imaging parameters such as numerical aperture, spatial acceptance (vignetting), chromatic aberration and focal length are provided for both thin- and thick-lens imaging geometries. These expressions show that the numerical aperture will be maximized and chromatic aberration will be minimized at the thick-lens limit. This limit may be satisfied by a range of CRL geometries, suggesting alternative approaches to improving the resolution and efficiency of CRLs and X-ray microscopes.

Classical reconstruction methods for phase-contrast tomography consist of two stages: phase retrieval and tomographic reconstruction. A novel algebraic method combining the two was suggested by Kostenko et al. [Opt. Express21, 12185 (2013)OPEXFF1094-408710.1364/OE.21.012185], and preliminary results demonstrated improved reconstruction compared with a given two-stage method. Using simulated free-space propagation experiments with a single sample-detector distance, we thoroughly compare the novel method with the two-stage method to address limitations of the preliminary results. We demonstrate that the novel method is substantially more robust toward noise; our simulations point to a possible reduction in counting times by an order of magnitude.

A multigrain indexing algorithm for use with samples comprising an arbitrary number of known or unknown phases is presented. No a priori crystallographic knowledge is required. The algorithm applies to data acquired with a monochromatic beam and a conventional two-dimensional detector for diffraction. Initially, candidate grains are found by searching for crystallographic planes, using a Dirac comb convoluted with a box function as a filter. Next, candidate grains are validated and the unit cell is optimized. The algorithm is validated by simulations. Simulations of 500 cementite grains and ∼100 reflections per grain resulted in 99.2% of all grains being indexed correctly and 99.5% of the reflections becoming associated with the right grain. Simulations with 200 grains associated with four mineral phases and 50-700 reflections per grain resulted in 99.9% of all grains being indexed correctly and 99.9% of the reflections becoming associated with the right grain. The main limitation is in terms of overlap of diffraction spots and computing time. Potential areas of use include three-dimensional grain mapping, structural solution and refinement studies of complex samples, and studies of dilute phases.

Many physical and mechanical properties of crystalline materials depend strongly on their internal structure, which is typically organized into grains and domains on several length scales. Here we present dark-field X-ray microscopy; a non-destructive microscopy technique for the three-dimensional mapping of orientations and stresses on lengths scales from 100 nm to 1 mm within embedded sampling volumes. The technique, which allows 'zooming' in and out in both direct and angular space, is demonstrated by an annealing study of plastically deformed aluminium. Facilitating the direct study of the interactions between crystalline elements is a key step towards the formulation and validation of multiscale models that account for the entire heterogeneity of a material. Furthermore, dark-field X-ray microscopy is well suited to applied topics, where the structural evolution of internal nanoscale elements (for example, positioned at interfaces) is crucial to the performance and lifetime of macro-scale devices and components thereof.

The potential in macromolecular crystallography for using multiple crystals to collect X-ray diffraction data simultaneously from assemblies of up to seven crystals is explored. The basic features of the algorithms used to extract data and their practical implementation are described. The procedure could be useful both in relation to diffraction data obtained from intergrown crystals and to alleviate the problem of rapid diffraction decay arising from the effects of radiation damage.

Over the past decade, efforts have been made to develop nondestructive techniques for three-dimensional (3D) grain-orientation mapping in crystalline materials. 3D x-ray diffraction microscopy and differential-aperture x-ray microscopy can now be used to generate 3D orientation maps with a spatial resolution of 200 nanometers (nm). We describe here a nondestructive technique that enables 3D orientation mapping in the transmission electron microscope of mono- and multiphase nanocrystalline materials with a spatial resolution reaching 1 nm. We demonstrate the technique by an experimental study of a nanocrystalline aluminum sample and use simulations to validate the principles involved.

We introduce the binary superposed phase retrieval problem that aims at reconstructing multiple 0/1-valued functions with nonoverlapping bounded supports from moduli of superpositions of several displaced copies of their individual Fourier transforms. We discuss an application in coherent diffraction imaging of crystalline objects, propose two algorithms, and evaluate their performance by means of simulations.

An iterative search method is proposed for obtaining orientation maps inside polycrystals from three-dimensional X-ray diffraction (3DXRD) data. In each step, detector pixel intensities are calculated by a forward model based on the current estimate of the orientation map. The pixel at which the experimentally measured value most exceeds the simulated one is identified. This difference can only be reduced by changing the current estimate at a location from a relatively small subset of all possible locations in the estimate and, at each such location, an increase at the identified pixel can only be achieved by changing the orientation in only a few possible ways. The method selects the location/orientation pair indicated as best by a function that measures data consistency combined with prior information on orientation maps. The superiority of the method to a previously published forward projection Monte Carlo optimization is demonstrated on simulated data.

A three-dimensional X-ray detector for imaging 30-200 keV photons is described. It comprises a set of semi-transparent structured scintillators, where each scintillator is a regular array of waveguides in silicon, and with pores filled with CsI. The performance of the detector is described theoretically and explored in detail through simulations. Based on available hardware, a spatial resolution of 1 microm is obtainable. The resolution of a single screen is shown to be determined only by the pitch, at least up to 100 keV. In comparison with conventional homogeneous screens, an improvement in efficiency by a factor of 5-15 is obtainable. The cross-talk between screens in the three-dimensional detector is shown to be negligible. The three-dimensional concept enables ray-tracing and super-resolution algorithms to be applied.

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.

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.

Using high-energy synchrotron radiation, structure factors of YBa(2)Cu(3)O(6.98) were measured at $\lambda$ = 0.124 A. Charge densities were derived using generalized structure factors and VALRAY and compared to densities refined from theoretical structure factors, which were calculated using the LAPW method and WIEN2k. Refinement agreement indices were R(F) = 0.0047 for the experimental and 0.0023 for the theoretical data set, respectively. Experimental and theoretical results generally agree well. A topological analysis shows that the structure is mainly ionic but depletion of charge density between Cu and O gives hints for covalency and confirms the general consensus of hole localization in these bonds.

The purpose of this study has been to establish the incidence of gestational hypertension (GH) in women with gestational diabetes mellitus (GDM) and to examine the frequency of complications in women with co-existent GDM and GH. Furthermore, we wished to evaluate the significance of urine albumin excretion determined by the urine albumin creatinine ratio (ACR). A total of 215 successive pregnancies with risk factors for gestational diabetes, as defined by the Danish National Board of Health screened for gestational diabetes by the WHO criteria, were reviewed. Women who had a normal OGTT during the screening served as controls. Gestational hypertension was defined as a mean arterial pressure (MAP) >105 mmHg (systolic BP > or = 140 mmHg and/or diastolic BP > or = 90 mmHg). The two groups were comparable with regard to initial body mass index (BMI) and MAP. GH appeared with a higher frequency in women with GDM (28%) than in women with normal OGTT (10%) P=0.003 chi(2) test. Serious complications (perinatal mortality, malformations, acute caesarean section) also appeared with a higher frequency in women with GH and GDM (10%) than in women with GH but with normal OGTT (2%) P=0.0083 chi(2) test. We observed a significant increase in ACR in the group with complications (GDM and GH) during gestation regardless of intensive antihypertensive treatment. We also observed that ACR was significantly higher in women with GDM and GH when compared to women with GDM and a normal blood pressure. The BMI was consistently higher in women with GH, regardless of whether they had GDM or not as compared to the normotensive group. GH appears with a higher frequency in women with GDM and the co-existence seems correlated with a higher frequency of complications. The correlation between urine albumin excretion and complications might suggest that regulating GH should strive to normalise ACR in women with GDM.

The mechanical properties of polycrystalline materials are largely determined by the kinetics of the phase transformations during the production process. Progress in x-ray diffraction instrumentation at synchrotron sources has created an opportunity to study the transformation kinetics at the level of individual grains. Our measurements show that the activation energy for grain nucleation is at least two orders of magnitude smaller than that predicted by thermodynamic models. The observed growth curves of the newly formed grains confirm the parabolic growth model but also show three fundamentally different types of growth. Insight into the grain nucleation and growth mechanisms during phase transformations contributes to the development of materials with optimal mechanical properties.

Texture evolution governs many of the physical, chemical, and mechanical properties of polycrystalline materials, but texture models have only been tested on the macroscopic level, which makes it hard to distinguish between approaches that are conceptually very different. Here, we present a universal method for providing data on the underlying structural dynamics at the grain and subgrain level. The method is based on diffraction with focused hard x-rays. First results relate to the tensile deformation of pure aluminum. Experimental grain rotations are inconsistent with the classical Taylor and Sachs models.

Traditionally, depth resolution in diffraction experiments is obtained by inserting pinholes in both the incoming and diffracted beam. For materials science investigations of local strain and texture properties this leads to very slow data-acquisition rates, especially when characterization is performed on the level of the individual grains. To circumvent this problem a conical slit has been manufactured by wire-electrodischarge machining. The conical slit has six 25 microm-thick conically shaped openings matching six of the Debye-Scherrer cones from a face-centred-cubic powder. By combining the slit with a microfocused incoming beam of hard X-rays, an embedded gauge volume is defined. Using a two-dimensional detector, fast and complete information can be obtained regarding the texture and strain properties of the material within this particular gauge volume. The average machining and assemblage errors of the conical slit are found both to be of the order of 5 microm. An algorithm for alignment of the slit is established, and the potential of the technique is illustrated with an example of grain mapping in a 4.5 mm-thick Cu sample.

Objective: To examine the complications in gestational diabetes mellitus with special reference to the significance of the threshold for the oral glucose tolerance test (OGTT, plasma glucose > or = 7.8 mmol/l (equivalent to blood glucose 6.9 mmol/l) (WHO criteria) or blood glucose > 6.7 mmol/l (local criteria) after 2 h 75 g oral glucose load)., Design: Prospective descriptive study., Setting: From April 1, 1995 to April 1, 1997 a screening for gestational diabetes mellitus (GDM) according to the recommendations from the Danish board of health was performed in Ribe county., Subjects: Pregnant women in Ribe county (n = 6158)., Main Outcome Measures: Complications during pregnancy and the outcome., Results: Two hundred and twenty (3.6%) women had GDM by the local selection criteria and 2.8% according to the WHO criteria. The study revealed a significantly increased frequency of malformations (7.3% vs. 1.2%, p < 0.0001) and preeclampsia (15.5% vs. 1%, p < 0.0001) in the group with GDM independent of selection criteria (obesity vs. family history and glucosuria). The frequency of preeclampsia appeared higher in the group with obesity (p = 0.040). Malformations appeared with identical frequency in the groups with OGGT threshold higher than blood glucose 6.9 mmol/l (plasma glucose 7.8 mmol/l) (WHO criteria) and with blood glucose between 6.7 and 6.9 mmol/l, whereas preeclampsia did not occur with higher frequency in the latter group., Conclusion: Complications appear frequently in women with an abnormal OGGT, and obesity predisposes to preeclampsia. The use of the WHO criteria for screening for GDM would miss a number of women with complications.

Novel focusing optical devices have been developed for synchrotron radiation in the energy range 40-100 keV. Firstly, a narrow-band-pass focusing energy-tuneable fixed-exit monochromator was constructed by combining meridionally bent Laue and Bragg crystals. Dispersion compensation was applied to retain the high momentum resolution despite the beam divergence caused by the focusing. Next, microfocusing was achieved by a bent multilayer arranged behind the crystal monochromator and alternatively by a bent Laue crystal. A 1.2 micro m-high line focus was obtained at 90 keV. The properties of the different set-ups are described and potential applications are discussed. First experiments were performed, investigating with high spatial resolution the residual strain gradients in layered polycrystalline materials. The results underline that focused high-energy synchrotron radiation can provide unique information on the mesoscopic scale to the materials scientist, complementary to existing techniques based on conventional X-ray sources, neutron scattering or electron microscopy.

The triple-crystal diffractometer installed at HASYLAB beamline BW5 with a high-field wiggler of critical energy 27 keV for DORIS III, operated at 4.5 GeV electron energy, is described. Samples can be mounted in large cryostats or furnaces normally used in neutron scattering experiments. The instrument has been successfully applied to measure structure factors S(Q) in liquids and amorphous materials, to collect full data sets of highly accurate structure factors for charge-density work, to measure the spin component of the ground-state magnetization in transition-metal and rare-earth compounds, to study the diffuse scattering from stacking faults and dislocation loops in Si single crystals, and for the investigation of various aspects of structural phase transitions: critical scattering in SrTiO3, oxygen order and stripe order in high-To materials. A crossed-beam technique allows for local studies of texture, internal strain and phase changes in the bulk of materials.

The large penetration power of high-energy X-rays (>60 keV) raises interesting prospects for new types of structural characterizations of polycrystalline materials. It becomes possible in a non-destructive manner to perform local studies, within the bulk of the material, of the fundamental materials physics properties: grain orientations, strain, dislocation densities etc. In favourable cases these properties may be mapped in three dimensions with a spatial resolution that matches the dimensions of the individual grains. Imbedded volumes and interfaces become accessible. Moreover, the high energies allow better in-situ studies of samples in complicated environments (industrial process optimization). General techniques for research in this energy range have been developed using broad-band angle-dispersive methods, on-line two-dimensional detectors and conical slits. Characterizations have been made at the level of the individual grains and grain boundaries as well as on ensembles of grains. The spatial resolution is presently of the order of 10-100 micom. Four examples of applications are presented along with an outlook.

The haemodynamic changes in pregnancy result in decrease in haemoglobin and haematocrit. It has previously been demonstrated that absence of this decrease or even increase in the haemoglobin concentration (Hb) and haematocrit (Hct) values measured in the third trimester or late in the second trimester can be correlated to increased risk of development of hypertension, pre-eclampsia and intrauterine growth retardation. In the present investigation, the authors have investigated whether the abovementioned complications of pregnancy can also be correlated to high Hb and high Hct measured early in the third trimester. The investigation included 373 healthy pregnant women, 46 of whom had Hb greater than or equal to 8.3 mmol/l in the 13th-19th weeks. Complications of pregnancy occurred in 17.4% of the 46 women. Among the remaining 327 pregnant women with Hb less than 8.3 mmol/l, complications of pregnancy were observed in only 5.8%. This difference is significant. The blood volume increases by approximately 1.5 litre during pregnancy. The plasma volume increases by 50% from the seventh to the 32nd week and thereafter remains constant until delivery. The erythrocyte volume increases first from approximately the 16th week and increases by a total of 25%. The early increase in plasma volume results in a decrease in the haemoglobin concentration (Hb) and in the haematocrit (Hct) value. During the third trimester, Hb and Hct increase again as a result of the increased erythrocyte volume. A positive correlation has been demonstrated between the magnitude of the plasma volume in the third trimester and the birth weight and a negative correlation between Hb in the third trimester and the birth weight.(ABSTRACT TRUNCATED AT 250 WORDS)