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The nature of the Verwey transition occurring at TV ≈ 125 K in magnetite (Fe3O4) has been an outstanding problem over many decades. A complex low temperature electronic order was recently discovered and associated structural fluctuations persisting above TV are widely reported, but the origin of the underlying correlations and hence of the Verwey transition remains unclear. Here we show that local structural fluctuations in magnetite emerge below the Curie transition at TC ≈ 850 K, through X-ray pair distribution function analysis. Around 80% of the low temperature correlations emerge in proportion to magnetization below TC. This confirms that fluctuations in Fe-Fe bonding arising from magnetic order are the primary electronic instability and hence the origin of the Verwey transition. Such hidden instabilities may be important to other spin-polarised conductors and orbitally degenerate materials., The Verwey transition in magnetite was reported 80 years ago but identifying the underlying mechanism has been difficult. Here the authors show that structural distortions associated with the Verwey transition emerge as local fluctuations at the Curie temperature, confirming their link with magnetic order.

The beam diffusing properties of stacked layers of diffuser material were evaluated experimentally and compared to a Gaussian random phase screen model. The model was found to give promising accuracy in combination with a Lorentzian auto-correlation model. The tail behaviour of the angular scattering distribution as a function of number of diffusing layers was particularly well described by the model, and in the case of an amorphous carbon diffuser, the model could describe the whole of the scattering distribution convincingly. (C) 2019 Optical Society of America under the terms of the OSA Open Access Publishing Agreement

The influence of nanosilica on the crystallization behavior, rheology and mechanical properties of poly(ε-caprolactone) (PCL) nanocomposites was investigated. It was found that the effect of nanofiller addition is dependent on the molar mass of the polymer matrix. For the higher molar mass matrix, a modest nucleation effect was observed, while in the lower molar mass matrices, this effect was absent. For the investigated range of filler contents, a modest increase in both modulus and ultimate tensile properties of the composites was observed. Lower molar mass matrices revealed voiding during deformation, which could be partly suppressed by the addition of nanofiller. The higher molar mass matrix showed no voiding in either the neat polymer or nanocomposite.

Ti-alloys represent the principal structural materials in both aerospace development and metallic biomaterials. Key to optimizing their mechanical and functional behaviour is in-depth know-how of their phases and the complex interplay of diffusive vs. displacive phase transformations to permit the tailoring of intricate microstructures across a wide spectrum of configurations. Here, we report on structural changes and phase transformations of Ti–Nb alloys during heating by in situ synchrotron diffraction. These materials exhibit anisotropic thermal expansion yielding some of the largest linear expansion coefficients (+ 163.9×10−6 to −95.1×10−6 °C−1) ever reported. Moreover, we describe two pathways leading to the precipitation of the α-phase mediated by diffusion-based orthorhombic structures, α″lean and α″iso. Via coupling the lattice parameters to composition both phases evolve into α through rejection of Nb. These findings have the potential to promote new microstructural design approaches for Ti–Nb alloys and β-stabilized Ti-alloys in general., Nature Communications, 8 (1), ISSN:2041-1723

The crystal structures of new layered manganese bismuth tellurides with the compositions Mn0.85(3)Bi4.10(2)Te7 and Mn0.73(4)Bi6.18(2)Te10 were determined by single-crystal X-ray diffraction, including the use of microfocused synchrotron radiation. These analyses reveal that the layered structures deviate from the idealized stoichiometry of the 12P-GeBi4Te7 (space group P3m1) and 51R-GeBi6Te10 (space group R3m) structure types they adopt. Modified compositions Mn1–xBi4+2x/3Te7 (x = 0.15 – 0.2) and Mn1–xBi6+2x/3Te10 (x = 0.19 – 0.26) assume cation vacancies and lead to homogenous bulk samples as confirmed by Rietveld refinements. Electron diffraction patterns exhibit no diffuse streaks that would indicate stacking disorder. The alternating quintuple-layer [M2Te3] and septuple-layer [M3Te4] slabs (M = mixed occupied by Bi and Mn) with 1:1 sequence (12P stacking) in Mn0.85Bi4.10Te7 and 2:1 sequence (51R stacking) in Mn0.81Bi6.13Te10 were also observed in HRTEM images. Temperature-dependent powder diffraction and differential scanning calorimetry show that the compounds are high temperature phases, which are metastable at ambient temperature. Magnetization measurements are in accordance with a MnII oxidation state and point at predominantly ferromagnetic coupling in both compounds. The thermoelectric figures of merit of n-type conducting Mn0.85Bi4.10Te7 and Mn0.81Bi6.13Te10 reach zT = 0.25 at 375 °C and zT = 0.28 at 325 °C, respectively. Although the compounds are metastable, compact ingots exhibit still up to 80% of the main phases after thermoelectric measurements up to 400 °C.

Methane oxidation over Pd–Pt/$ \mathrm{Al}_2\text{ O}_3 $ model catalysts calcined at three different conditions is investigated using operando diffuse reflectance infrared Fourier transform spectroscopy and mass spectrometry, and in situ X-ray absorption spectroscopy while cycling the feed gas stoichiometry between lean (net-oxidising) and rich (net-reducing) conditions. When calcined in air, alloy Pd–Pt nanoparticles are present only on catalysts subjected to elevated temperature ($ 800\,^{\circ }\mathrm{C} $) whereas calcination at lower temperature (500 $ ^{\circ }\mathrm{C} $) leads to segregated Pt and Pd nanoparticles on the support. Here, we show that the alloy Pd–Pt nanoparticles undergo reversible changes in surface structure and composition during transient methane oxidation exposing a PdO surface during lean conditions and a metallic Pd–Pt surface (Pd enriched) under rich conditions. Alloyed particles seem more active for methane oxidation than their monometallic counterparts and, furthermore, an increased activity for methane oxidation is clearly observed under lean conditions when PdO has developed on the surface, analogous to monometallic Pd catalysts. Upon introducing rich conditions, partial oxidation of methane dominates over total oxidation forming adsorbed carbonyls on the noble metal particles. The carbonyl spectra for the three samples show clear differences originating from different surfaces exposed by alloyed vs. non-alloyed particles. The kinetics of the noble metal oxidation and reduction processes as well as carbonyl formation during transient methane oxidation are discussed.

Understanding the complex crystallization behavior of isotactic polypropylene (iPP) in conditions comparable to those found in polymer processing, where the polymer melt experiences a combination of high shear rates and elevated pressures, is key for modeling and therefore predicting the final structure and properties of iPP products. Coupling a unique experimental setup, capable to apply wall shear rates similar to those experienced during processing and carefully control the pressure before and after flow is imposed, with in situ X-ray scattering and diffraction techniques (SAXS and WAXD) at fast acquisition rates (up to 30 Hz), a well-defined series of short-term flow experiments are carried out using 16 different combinations of wall shear rates (ranging from 110 to 440 s–1) and pressures (100–400 bar). A complete overview on the kinetics of structure development during and after flow is presented. Information about shish formation and growth of α-phase parents lamellae from the shish backbones is extracted from SAXS; the overall apparent crystallinity evolution, amounts of different phases (α, β, and γ), and morphologies developing in the shear layer (parent and daughter lamellae both in α and γ phase) are fully quantified from the analysis of WAXD data. Both flow rate and pressure were found to have a significant influence on the nucleation and the growth process of oriented and isotropic structures. Flow affects shish formation and the growth of α-parents; pressure acts on relaxation times, enhancing the effect of flow, and (mainly) on the growth rate of γ-phase. The remarkably high amount of γ-lamellae found in the oriented layer strongly indicates the nucleation of γ directly from the shish backbone. All the observations were conceptually in agreement with the flow-induced crystallization model framework developed in our group and represent a unique and valuable data set that will be used to further validate and implement our numerical modeling, filling the gap for quantitatively modeling crystallization during complicated processing operations like injection molding.

By means of high-energy synchrotron X-ray diffraction, the interplay between martensite and retained austenite phases in steel during the application of stress has been analyzed. Martensite properties were varied through controlled reheating heat treatments in a low carbon Quenched and Partitioned (Q&P) steel consisting of retained austenite and martensite. The reheating treatments significantly altered martensite strength while keeping the same fractions of retained austenite as the non-reheated Q&P microstructures, resulting in different degrees of stress partitioning and work hardening of the individual microconstituents. Results of this study show that the strength ratio between the different phases in the microstructure plays a crucial role in the onset and rate of mechanically induced decomposition of retained austenite. Consequently, the strength ratio between phases controls the yielding and work-hardening of the material.

Residual stresses originating from elasto-plastic deformation during mechanical processing can be analyzed post-process with various known methods. A new measurement method to measure and evaluate the strain and stress fields in situ under the contact point during a deep rolling process was developed to describe the dependence of the residual stresses from the internal material load. Using synchrotron radiation at European Synchrotron Radiation Facility (ESRF) (ID11), diffraction measurements were performed in transmission geometry during dynamical loading with different process parameters. The strain and stress fields were analyzed with high spatial resolution in an 8 mm &times, 4 mm area around the contact point during the process using a 13-mm tungsten carbide roller on samples of AISI 4140H steel. Fast data acquisition allowed the reconstruction of full two-dimensional (2D) strain and stress maps. These could be used to determine the response from the initial material state in front of the roller to the mechanically loaded region with plastic deformation up to the processed material with the resulting residual stresses. This comprehensive analysis was then used to link the internal material load with the resulting residual stresses in the final material state.

The determination of residual stresses (RS) through X-Ray Diffraction (XRD) necessitates the knowledge of the X-Ray Elastic Constants (XEC) S1 and 1/2 S2 for the specific phase in presence. In the case of Ti-6Al-4V additive manufacturing (AM) elaboration method such as Powder Bed Laser Beam Melting (PB-LBM) results in a microstructure fully constituted α’ martensitic phase. The properties of this α’ martensite are largely unknown. The purpose of the present paper is to determine the XEC of the α’ martensitic phase. This is performed using an original methodology involving 2D X-Ray detection. The results shows significant differences with XEC values available for the α phase from Titanium.

Supplementary information accompanies this paper at https://doi.org/10.1038/s41598-018-31849-w.; International audience; Human vocal folds possess outstanding abilities to endure large, reversible deformations and to vibrate up to more than thousand cycles per second. This unique performance mainly results from their complex specific 3D and multiscale structure, which is very difficult to investigate experimentally and still presents challenges using either confocal microscopy, MRI or X-ray microtomography in absorption mode. To circumvent these difficulties, we used high-resolution synchrotron X-ray microtomography with phase retrieval and report the first ex vivo 3D images of human vocal-fold tissues at multiple scales. Various relevant descriptors of structure were extracted from the images: geometry of vocal folds at rest or in a stretched phonatory-like position, shape and size of their layered fibrous architectures, orientation, shape and size of the muscle fibres as well as the set of collagen and elastin fibre bundles constituting these layers. The developed methodology opens a promising insight into voice biomechanics, which will allow further assessment of the micromechanics of the vocal folds and their vibratory properties. This will then provide valuable guidelines for the design of new mimetic biomaterials for the next generation of artificial larynges.

The feasibility for multi-speckle XPCS measurements in the ultra-low-angle range is demonstrated. The performance of the setup is illustrated by means of colloidal dynamics., Multi-speckle X-ray photon correlation spectroscopy (XPCS) measurements in the ultra-small-angle range are performed using a long pinhole collimation instrument in combination with two-dimensional photon-counting and high-sensitivity imaging detectors. The feasibility of the presented setup to measure dynamics on different time and length scales pertinent to colloidal systems is shown. This setup offers new research opportunities, such as for example in the investigation of non-equilibrium dynamics in optically opaque, complex systems over length scales from tens of nanometres to several micrometres. In addition, due to the short duration of the X-ray exposure involved in the ultra-small-angle range, possible radiation-induced effects are alleviated. Furthermore, the performance of two different detectors, a photon-counting Pilatus 300K and an integrating FReLoN CCD, are compared, and their applicability for accurate XPCS measurements is demonstrated.

X-ray nanodiffraction is used to evaluate axial and tangential residual stress distributions in a W thin film deposited on the scalloped inner wall of a through-silicon via. The results reveal oscillatory stress distributions which correlate well with the scallop wavelength and morphology., Synchrotron X-ray nanodiffraction is used to analyse residual stress distributions in a 200 nm-thick W film deposited on the scalloped inner wall of a through-silicon via. The diffraction data are evaluated using a novel dedicated methodology which allows the quantification of axial and tangential stress components under the condition that radial stresses are negligible. The results reveal oscillatory axial stresses in the range of ∼445–885 MPa, with a distribution that correlates well with the scallop wavelength and morphology, as well as nearly constant tangential stresses of ∼800 MPa. The discrepancy with larger stress values obtained from a finite-element model, as well as from a blanket W film, is attributed to the morphology and microstructural nature of the W film in the via.

This Perspective is part of the Up and Coming series. Abstract: Over the past few decades material scientists have developed a wide variety of approaches to deliberately introduce chemical and structural inhomogeneities into nanoparticles achieving for example intentional doping concentration gradients and multicomponent structures. This perspective presents a sense of how modern hard X ray spectroscopic methods far from merely providing new tools are extending the way we study and understand such complex nanoparticles. Particularly the possibility to select with high resolution the incident and emission hard X ray energies offers unprecedented site selectivity and rapid data acquisition helps to uncover the complex chemical world behind the state of the art synthetic methods like hot injection Brust Schiffrin supercritical flow and nonaqueous synthesis. Therefore today the in situ spectroscopic studies provide a new view into the genesis of heterogeneity in colloidal nanoparticles.

International audience; Many organisms use amorphous calcium carbonate (ACC) and control its stability by various additives and water; however, the underlying mechanisms are yet unclear. Here, the effect of water and inorganic additives commonly found in biology on the dynamics of the structure of ACC during crystallization and on the energetics of this process is studied. Total X-ray scattering and pair distribution function analysis show that the short- and mediumrange order of all studied ACC samples are similar; however, the use of in situ methodologies allow the observation of small structural modifications that are otherwise easily overlooked. Isothermal calorimetric coupled with microgravimetric measurements show that the presence of Mg2+ and of PO43− in ACC retards the crystallization whereas increased water content accelerates the transformation. The enthalpy of ACC with respect to calcite appears, however, independent of the additive concentration but decreases with water content. Surprisingly, the enthalpic contribution of water is compensated for by an equal and opposite entropic term leading to a net independence of ACCthermodynamic stability on its hydration level. Together, these results point toward a kinetic stabilization effect of inorganic additives and water, and may contribute to the understanding of the biological control of mineral stability.

International audience; The effect of the support material and chemical state of Rh in Rh/A(2)O(3) and Rh/SiO2 model catalysts during CO2 hydrogenation were studied by a combined array of in situ characterisation techniques including diffuse reflectance infrared Fourier transform spectroscopy, energy-dispersive X-ray absorption spectroscopy and high-energy X-ray diffraction at 250-350 degrees C and atmospheric pressure. CO2 methanation proceeds via intermediate formation of adsorbed CO species on metallic Rh, likely followed by their hydrogenation to methane. The linearly-bonded CO species is suggested to be a more active precursor in the hydrogenation compared to the bridge-bonded species, which seems to be related to particle size effects: for larger particles mainly the formation of inactive bridge-bonded CO species takes place. Further, analysis of the chemical state of Rh under the reaction conditions reveal a minor formation of RhOx from dissociation of CO2, which is a consequence of the increased activity observed over the Rh/Al2O3 catalyst.

The high-temperature creep behavior of a rafted [001] oriented AM1 Ni-based single crystal superalloy was investigated during in situ creep tests on synchrotrons. Experiments were performed at constant temperatures under variable applied stress in order to study the response (plastic strain, load transfer) to stress jumps. Using two different diffraction techniques in transmission (Laue) geometry, it was possible to measure the average lattice parameters of both the &gamma, matrix and the &gamma, &prime, rafts in the [100] direction at intervals shorter than 300 s. The absolute precision with both diffraction techniques of the constrained transverse mismatch (in the rafts&rsquo, plane) is about 10&minus, 5. After stress jumps, special attention is given to the evolution of plastic strain within the &gamma, channels. The relaxation of the Von Mises stress at leveled applied stress shows evidence of dislocation multiplication within the &gamma, channels. From the analysis, we showed an interaction between plastic stress and dislocation density of the &gamma, phase.

Recent years have seen the development of new iron-centered N-heterocyclic carbene (NHC) complexes for solar energy applications. Compared to typical ligand systems, the NHC ligands provide Fe complexes with longer-lived metal-to-ligand charge transfer (MLCT) states. This increased lifetime is ascribed to strong ligand field splitting provided by the NHC ligands that raises the energy levels of the metal centered (MC) states and therefore reduces the deactivation efficiency of MLCT states. Among currently known NHC systems, [Fe(btbip)2]2+ (btbip = 2,6-bis(3-tert-butyl-imidazol-1-ylidene)pyridine) is a unique complex as it exhibits a short-lived MC state with a lifetime on the scale of a few hundreds of picoseconds. Hence, this complex allows for a detailed investigation, using 100 ps X-ray pulses from a synchrotron, of strong ligand field effects on the intermediate MC state in an NHC complex. Here, we use time-resolved wide angle X-ray scattering (TRWAXS) aided by density functional theory (DFT) to investigate the molecular structure, energetics and lifetime of the high-energy MC state in the Fe-NHC complex [Fe(btbip)2]2+ after excitation to the MLCT manifold. We identify it as a 260 ps metal-centered quintet (5MC) state, and we refine the molecular structure of the excited-state complex verifying the DFT results. Using information about the hydrodynamic state of the solvent, we also determine, for the first time, the energy of the 5MC state as 0.75 + 0.15 eV. Our results demonstrate that due to the increased ligand field strength caused by NHC ligands, upon transition from the ground state to the 5MC state, the metal to ligand bonds extend by unusually large values: by 0.29 angstrom in the axial and 0.21 angstrom in the equatorial direction. These results imply that the transition in the photochemical properties from typical Fe complexes to novel NHC compounds is manifested not only in the destabilization of the MC states, but also in structural distortion of these states.

Both a cured cement paste and a paste undergoing in situ hydration have been characterized using state-of-the-art synchrotron diffraction tomography. The mineralogy, macroporosity and carbonation phenomena of the samples have been determined., To understand the main properties of cement, a ubiquitous material, a sound description of its chemistry and mineralogy, including its reactivity in aggressive environments and its mechanical properties, is vital. In particular, the porosity distribution and associated sample carbonation, both of which affect cement’s properties and durability, should be quantified accurately, and their kinetics and mechanisms of formation known both in detail and in situ. However, traditional methods of cement mineralogy analysis (e.g. chemical mapping) involve sample preparation (e.g. slicing) that can be destructive and/or expose cement to the atmosphere, leading to preparation artefacts (e.g. dehydration). In addition, the kinetics of mineralogical development during hydration, and associated porosity development, cannot be examined. To circumvent these issues, X-ray diffraction computed tomography (XRD-CT) has been used. This allowed the mineralogy of ternary blended cement composed of clinker, fly ash and blast furnace slag to be deciphered. Consistent with previous results obtained for both powdered samples and dilute systems, it was possible, using a consolidated cement paste (with a water-to-solid ratio akin to that used in civil engineering), to determine that the mineralogy consists of alite (only detected in the in situ hydration experiment), calcite, calcium silicate hydrates (C-S-H), ettringite, mullite, portlandite, and an amorphous fraction of unreacted slag and fly ash. Mineralogical evolution during the first hydration steps indicated fast ferrite reactivity. Insights were also gained into how the cement porosity evolves over time and into associated spatially and time-resolved carbonation mechanisms. It was observed that macroporosity developed in less than 30 h of hydration, with pore sizes reaching about 100–150 µm in width. Carbonation was not observed for this time scale, but was found to affect the first 100 µm of cement located around macropores in a sample cured for six months. Regarding this carbonation, the only mineral detected was calcite.

The alpha-(Per)(2)[M(mnt)(2)] compounds with M = Pt and Au are isostructural two-chain solids that in addition to partially oxidized conducting perylene chains also contain anionic chains that can be either paramagnetic in the case of M = Pt or diamagnetic for M = Au. The electrical transport and magnetic properties of the solid solutions (Per)(2)[Pt-x-Au(1-x)(mnt)(2)] were investigated. The incorporation of paramagnetic [Pt(mnt)(2)] impurities in the diamagnetic chains, and the effect of breaking the paramagnetic chains with diamagnetic centers for the low and high Pt range of concentrations were respectively probed. In the low Pt concentration range, there is a fast decrease of the metal-to-insulator transition from 12.4 K in the pure Au compound to 9.7 K for x = 0.1 comparable to the 8.1 K in the pure Pt compound. In the range x = 0.5-0.95, only beta-phase crystals could be obtained. The spin-Peierls transition of the pure Pt compound, simultaneous with metal-to-insulator (Peierls) transition is still present for 2% of diamagnetic impurities (x = 0.98) with transition temperature barely affected. Single crystal X-ray diffraction data obtained a high-quality structural refinement of the alpha- phase of the Au and Pt compounds. The beta-phase structure was found to be composed of ordered layers with segregated donors and anion stacks, which alternate with disordered layers. The semiconducting properties of the beta-phase are due to the disorder localization effects. info:eu-repo/semantics/publishedVersion

Bragg diffraction imaging enables the quality of synthetic single-crystal diamond substrates and their overgrown, mostly doped, diamond layers to be characterized. This is very important for improving diamond-based devices produced for X-ray optics and power electronics applications. The usual first step for this characterization is white-beam X-ray diffraction topography, which is a simple and fast method to identify the extended defects (dislocations, growth sectors, boundaries, stacking faults, overall curvatureetc.) within the crystal. This allows easy and quick comparison of the crystal quality of diamond plates available from various commercial suppliers. When needed, rocking curve imaging (RCI) is also employed, which is the quantitative counterpart of monochromatic Bragg diffraction imaging. RCI enables the local determination of both the effective misorientation, which results from lattice parameter variation and the local lattice tilt, and the local Bragg position. Maps derived from these parameters are used to measure the magnitude of the distortions associated with polishing damage and the depth of this damage within the volume of the crystal. For overgrown layers, these maps also reveal the distortion induced by the incorporation of impurities such as boron, or the lattice parameter variations associated with the presence of growth-incorporated nitrogen. These techniques are described, and their capabilities for studying the quality of diamond substrates and overgrown layers, and the surface damage caused by mechanical polishing, are illustrated by examples.

Studies of brain cytoarchitecture in mammals are routinely performed by serial sectioning of the specimen and staining of the sections. The procedure is labor-intensive and the 3D architecture can only be determined after aligning individual 2D sections, leading to a reconstructed volume with non-isotropic resolution. Propagation-based x-ray phase-contrast tomography offers a unique potential for high-resolution 3D imaging of intact biological specimen due to the high penetration depth and potential resolution. We here show that even compact laboratory CT at an optimized liquid-metal jet microfocus source combined with suitable phase-retrieval algorithms and a novel tissue preparation can provide cellular and subcellular resolution in millimeter sized samples of mouse brain. We removed water and lipids from entire mouse brains and measured the remaining dry tissue matrix in air, lowering absorption but increasing phase contrast. We present single-cell resolution images of mouse brain cytoarchitecture and show that axons can be revealed in myelinated fiber bundles. In contrast to optical 3D techniques our approach does neither require staining of cells nor tissue clearing, procedures that are increasingly difficult to apply with increasing sample and brain sizes. The approach thus opens a novel route for high-resolution high-throughput studies of brain architecture in mammals.

The effect of ceria doping by oxide surface modification and controlled metal surface modification (CSM) on the structure-function properties of Rh/γ-Al2O3 catalysts in the process of CO oxidation were studied by a combined array of Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS)/Energy Dispersive X-ray Absorption Fine Structure/Mass Spectrometry techniques applied simultaneously under time-resolved, in situ conditions in the temperature range of 298–573 K. The addition of each promoter element by CSM exhibits multiple effects on the catalysts structure. The DRIFTS/XAS studies indicate that CeOx facilitate the protection of Rh particles against extensive oxidation in atmospheres of air, O2 and CO, without reducing the coverage of oxidisable adsorbed CO.

This paper presents a multifunctional polymer surface that provides superhydrophobicity and self–cleaning functions together with an enhancement in mechanical and electrical performance. These functionalities are produced by nanoimprinting high aspect ratio pillar arrays on polymeric matrix incorporating functional reinforcing elements. Two distinct matrix-filler systems are investigated specifically, Carbon Nanotube reinforced Polystyrene (CNT-PS) and Reduced Graphene Oxide reinforced Polyvinylidene Difluoride (RGO-PVDF). Mechanical characterization of the topographies by quantitative nanoindentation and nanoscratch tests are performed to evidence a considerable increase in stiffness, Young’s modulus and critical failure load with respect to the pristine polymers. The improvement on the mechanical properties is rationalized in terms of effective dispersion and penetration of the fillers into the imprinted structures as determined by confocal Raman and SEM studies. In addition, an increase in the degree of crystallization for the PVDF-RGO imprinted nanocomposite possibly accounts for the larger enhancement observed. Improvement of the mechanical ruggedness of functional textured surfaces with appropriate fillers will enable the implementation of multifunctional nanotextured materials in real applications.

The mutable collagenous tissue (MCT) of echinoderms (e.g., sea cucumbers and starfish) is a remarkable example of a biological material that has the unique attribute, among collagenous tissues, of being able to rapidly change its stiffness and extensibility under neural control. However, the mechanisms of MCT have not been characterized at the nanoscale. Using synchrotron small-angle X-ray diffraction to probe time-dependent changes in fibrillar structure during in situ tensile testing of sea cucumber dermis, we investigate the ultrastructural mechanics of MCT by measuring fibril strain at different chemically induced mechanical states. By measuring a variable interfibrillar stiffness (EIF), the mechanism of mutability at the nanoscale can be demonstrated directly. A model of stiffness modulation via enhanced fibrillar recruitment is developed to explain the biophysical mechanisms of MCT. Understanding the mechanisms of MCT quantitatively may have applications in development of new types of mechanically tunable biomaterials.

A collection of more than 1800 carbonized papyri, discovered in the Roman ‘Villa dei Papiri’ at Herculaneum is the unique classical library survived from antiquity. These papyri were charred during 79 A.D. Vesuvius eruption, a circumstance which providentially preserved them until now. This magnificent collection contains an impressive amount of treatises by Greek philosophers and, especially, Philodemus of Gadara, an Epicurean thinker of 1st century BC. We read many portions of text hidden inside carbonized Herculaneum papyri using enhanced X-ray phase-contrast tomography non-destructive technique and a new set of numerical algorithms for ‘virtual-unrolling’. Our success lies in revealing the largest portion of Greek text ever detected so far inside unopened scrolls, with unprecedented spatial resolution and contrast, all without damaging these precious historical manuscripts. Parts of text have been decoded and the ‘voice’ of the Epicurean philosopher Philodemus is brought back again after 2000 years from Herculaneum papyri.

The complex mechanical properties of biomaterials such as hair, horn, skin, or bone are determined by the architecture of the underlying fibrous bionetworks. Although much is known about the influence of the cytoskeleton on the mechanics of isolated cells, this has been less studied in tridimensional tissues. We used the hair follicle as a model to link changes in the keratin network composition and architecture to the mechanical properties of the nascent hair. We show using atomic force microscopy that the soft keratinocyte matrix at the base of the follicle stiffens by a factor of ∼360, from 30 kPa to 11 MPa along the first millimeter of the follicle. The early mechanical stiffening is concomitant to an increase in diameter of the keratin macrofibrils, their continuous compaction, and increasingly parallel orientation. The related stiffening of the material follows a power law, typical of the mechanics of nonthermal bending-dominated fiber networks. In addition, we used X-ray diffraction to monitor changes in the (supra)molecular organization within the keratin fibers. At later keratinization stages, the inner mechanical properties of the macrofibrils dominate the stiffening due to the progressive setting up of the cystine network. Our findings corroborate existing models on the sequence of biological and structural events during hair keratinization.

A compact design for a miniature tensile stress rig, compatible with the space and weight constraints imposed by near-field diffraction imaging techniques, is presented. The device can carry tensile loads up to 500 N and is driven by a piezoelectric actuator which can work in a static and dynamic regime up to frequencies of 100 Hz., Multi-modal characterization of polycrystalline materials by combined use of three-dimensional (3D) X-ray diffraction and imaging techniques may be considered as the 3D equivalent of surface studies in the electron microscope combining diffraction and other imaging modalities. Since acquisition times at synchrotron sources are nowadays compatible with four-dimensional (time lapse) studies, suitable mechanical testing devices are needed which enable switching between these different imaging modalities over the course of a mechanical test. Here a specifically designed tensile device, fulfilling severe space constraints and permitting to switch between X-ray (holo)tomography, diffraction contrast tomography and topotomography, is presented. As a proof of concept the 3D characterization of an Al–Li alloy multicrystal by means of diffraction contrast tomography is presented, followed by repeated topotomography characterization of one selected grain at increasing levels of deformation. Signatures of slip bands and sudden lattice rotations inside the grain have been shown by means of in situ topography carried out during the load ramps, and diffraction spot peak broadening has been monitored throughout the experiment.

Out-of-equilibrium phenomena are attracting high interest in physics, materials science, chemistry and life sciences. In this state, the study of structural fluctuations at different length scales in time and space are necessary to achieve significant advances in the understanding of structure-functionality relationship. The visualization of patterns arising from spatiotemporal fluctuations is nowadays possible thanks to new advances in X-ray instrumentation development that combine high resolution both in space and in time. We present novel experimental approaches using high brilliance synchrotron radiation sources, fast detectors and focusing optics, joint with advanced data analysis based on automated statistical, mathematical and imaging processing tools. This approach has been used to investigate structural fluctuations in out-of-equilibrium systems in the novel field of inhomogeneous quantum complex matter at the crossing point of technology, physics and biology. In particular, we discuss how nanoscale complexity controls the emergence of high temperature superconductivity (HTS), myelin functionality and formation of hybrid organic-inorganic nanostructures. The emergent complex geometries, opening novel venues to quantum technology and to development of quantum physics of living systems, are discussed, 18 pages, 7 figures

The grain structure of a slightly deformed Al–0.3 wt%Mn alloy was reconstructed using diffraction contrast tomography (DCT) and high-energy diffraction microscopy (HEDM). The direct comparison shows that DCT can detect subgrain boundaries with disorientations as low as 1° and that HEDM and DCT grain boundaries are on average 4 µm apart from each other., The grain structure of an Al–0.3 wt%Mn alloy deformed to 1% strain was reconstructed using diffraction contrast tomography (DCT) and high-energy diffraction microscopy (HEDM). 14 equally spaced HEDM layers were acquired and their exact location within the DCT volume was determined using a generic algorithm minimizing a function of the local disorientations between the two data sets. The microstructures were then compared in terms of the mean crystal orientations and shapes of the grains. The comparison shows that DCT can detect subgrain boundaries with disorientations as low as 1° and that HEDM and DCT grain boundaries are on average 4 µm apart from each other. The results are important for studies targeting the determination of grain volume. For the case of a polycrystal with an average grain size of about 100 µm, a relative deviation of about ≤10% was found between the two techniques.

ID16B is a versatile hard X-ray nanoprobe devoted to X-ray nano-analysis. It combines X-ray fluorescence, X-ray diffraction, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques., Within the framework of the ESRF Phase I Upgrade Programme, a new state-of-the-art synchrotron beamline ID16B has been recently developed for hard X-ray nano-analysis. The construction of ID16B was driven by research areas with major scientific and societal impact such as nanotechnology, earth and environmental sciences, and bio-medical research. Based on a canted undulator source, this long beamline provides hard X-ray nanobeams optimized mainly for spectroscopic applications, including the combination of X-ray fluorescence, X-ray diffraction, X-ray excited optical luminescence, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques. Its end-station re-uses part of the apparatus of the earlier ID22 beamline, while improving and enlarging the spectroscopic capabilities: for example, the experimental arrangement offers improved lateral spatial resolution (∼50 nm), a larger and more flexible capability for in situ experiments, and monochromatic nanobeams tunable over a wider energy range which now includes the hard X-ray regime (5–70 keV). This paper describes the characteristics of this new facility, short-term technical developments and the first scientific results.

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions., Scientific Reports, 6, ISSN:2045-2322

Polymorphism is the ability of a solid material to exist in more than one phase or crystal structure. Polymorphism may occur in metals, alloys, ceramics, minerals, polymers, and pharmaceutical substances. Unresolved are the conditions for preferential nucleation during polymorphic transformations in which structural relationships or special crystallographic orientation relationships (OR’s) form between the nucleus and surrounding matrix grains. We measured in-situ and simultaneously the nucleation rates of grains that have zero, one, two, three and four special OR’s with the surrounding parent grains. These experiments show a trend in which the activation energy for nucleation becomes smaller – and therefore nucleation more probable - with increasing number of special OR’s. These insights contribute to steering the processing of polymorphic materials with tailored properties, since preferential nucleation affects which crystal structure forms, the average grain size and texture of the material, and thereby - to a large extent - the final properties of the material.

Due to the rising need for clean energy, thermoelectricity has raised as a potential alternative to reduce dependence on fossil fuels. Specifically, thermoelectric devices based on polymers could offer an efficient path for near-room temperature energy harvesters. Thus, control over thermoelectric properties of conducting polymers is crucial and, herein, the structural, electrical and thermoelectric properties of poly(3,4-ethylenedioxythiophene) (PEDOT) thin films doped with p-toluenesulfonate (Tos) molecules were investigated with regards to thin film processing. PEDOT:Tos thin films were prepared by in-situ polymerization of (3,4-ethylenedioxythiophene) monomers in presence of iron(III) p-toluenesulfonate with different co-solvents in order to tune the film structure. While the Seebeck coefficient remained constant, a large improvement in the electrical conductivity was observed for thin films processed with high boiling point additives. The increase of electrical conductivity was found to be solely in-plane mobility-driven. Probing the thin film structure by Grazing Incidence Wide Angle X-ray Scattering has shown that this behavior is dictated by the structural properties of the PEDOT:Tos films; specifically by the thin film crystallinity combined to the preferential edge-on orientation of the PEDOT crystallites. Consequentially enhancement of the power factor from 25 to 78.5 μW/mK2 has been readily obtained for PEDOT:Tos thin films following this methodology.

Framboidal triblock copolymer vesicles prepared via RAFT-mediated PISA are characterized by SAXS and TEM; a Pickering emulsifier adsorption efficiency of up to 94% is obtained for a mean globule size of 45 nm., Pickering emulsions offer important advantages over conventional surfactant-stabilized emulsions, including enhanced long-term stability, more reproducible formulations and reduced foaming problems. The recent development of polymerization-induced self-assembly (PISA) offers considerable scope for the design of a wide range of block copolymer nanoparticles with tunable surface wettability that may serve as bespoke Pickering emulsifiers. In the present study, we exploit PISA to design a series of model framboidal ABC triblock copolymer vesicles with exquisite control over surface roughness. Transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) were utilized to characterize these nanoparticles, which were subsequently used to stabilize n-dodecane emulsion droplets in water. The adsorption efficiency, Aeff, of the nanoparticles at the n-dodecane/water interface was determined as a function of increasing vesicle surface roughness using a turbidimetry assay. A strong correlation between surface roughness and Aeff was observed, with Aeff increasing from 36% up to 94%. This is a significant improvement in Pickering emulsifier efficiency compared to that reported previously for similar vesicles with smooth surfaces. In summary, nanoparticles with appreciable surface roughness are much more effective Pickering emulsifiers and this parameter can be readily fine-tuned using a highly efficient PISA formulation.

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 internal structure of materials determines many of their physical and mechanical properties. Here, the authors have developed a non-destructive X-ray microscopy technique for layer-by-layer mapping of crystallographic orientations and stresses to obtain a three-dimensional reconstruction of a material.

In this contribution, for the first time, the polarity of fullerene derivatives is tailored to enhance the miscibility between the host and dopant molecules. A fullerene derivative with a hydrophilic triethylene glycol type side chain (PTEG-1) is used as the host and (4-(1,3-dimethyl-2,3-dihydro-1H-benzoimidazol-2-yl)phenyl)dimethylamine n-DMBI) as the dopant. Thereby, the doping efficiency can be greatly improved to around 18% (

International audience; The presence of grain boundaries in single crystal castings is intolerable owing to the detrimental impact on creep and fatigue behaviour. Whilst the origins of many defects such as freckles have been understood since the 1970s, other defects such as slivers, or indeed the small mosaicity observed in many castings have eluded comprehensive treatments. In the present work, in situ X-ray imaging has been used to examine the origin of misorientation defects that arise during solidification. Dendrite deformation was observed, which impacted growth characteristics and led to a permanent misoriention. Digital image correlation analysis showed the dendrites becoming increasingly bent as solidification progressed. In order to probe the deformation modes further, a method was devised to convert standard EBSD data into measurements of bending and torsion angle.It was demonstrated that such defects form as the result of bending moments arising from differential thermal contraction and gravity.

Inline holography is a common phase-contrast imaging method which uses free-space propagation to encode the phase signal into measured intensities. However, quantitative retrieval of the sample's image remains challenging, imposing constraints on the nature of the sample or on the propagation distance. Here, we present a way of simultaneously retrieving the sample's complex-valued transmission function and the incident illumination function from near-field diffraction patterns. The procedure relies on the measurement diversity created by lateral translations of the sample with respect to a structured illumination. The reconstruction approach, in essence identical to that employed in ptychography, is applied to hard X-ray synchrotron measurements and to simulations. Compared to other inline holography techniques, we expect near-field ptychography to reduce reconstruction artefacts by factoring out wavefront imperfections and relaxing constraints on the sample's scattering properties, thus ultimately improving the robustness of propagation-based X-ray phase tomography.

X-ray absorption spectroscopy and X-ray diffraction are suitable probes of the chemical state of a catalyst under working conditions but are limited to bulk information. Here we show in two case studies related to hydrothermal aging and chemical modification of model automotive catalysts that enhanced detailed information of structural changes can be obtained when the two methods are combined with a concentration modulated excitation (cME) approach and phase sensitive detection (PSD). The catalysts are subject to a modulation experiment consisting of the periodic variation of the gas feed composition to the catalyst and the time-resolved data are additionally treated by PSD. In the case of a 2 wt% Rh/Al2O3 catalyst, a very small fraction (ca. 2%) of Rh remaining exposed at the alumina surface after hydrothermal aging at 1273 K can be detected by PSD. This Rh is sensitive to the red-ox oscillations of the experiment and is likely responsible for the observed catalytic activity and selectivity during NO reduction by CO. In the case of a 1.6 wt% Pd/Al2O3-Ce1−xZrxO2 catalyst, preliminary results of cME-XRD demonstrate that access to the kinetics of the whole material at work can be obtained. Both the red-ox processes involving the oxygen storage support and the Pd component can be followed with great precision. PSD enables the differentiation between Pd deposited on Al2O3 or on Ce1−xZrxO2. Modification of the catalyst by phosphorous clearly induces loss of the structural dynamics required for oxygen storage capacity that is provided by the Ce4+/Ce3+ pair. The two case studies demonstrate that detailed kinetics of subtle changes can be uncovered by the combination of in situ X-ray absorption and high energy diffraction methods with PSD., Physical Chemistry Chemical Physics, 15 (22), ISSN:1463-9084, ISSN:1463-9076

The self-assembly in aqueous solution of the alanine-rich peptide A12R2 containing twelve alanine residues and two arginine residues has been investigated. This oligomeric peptide was synthesized via NCA-polymerization methods. The surfactant-like peptide is found via FTIR to form antiparallel dimers which aggregate into twisted fibrils, as revealed by cryogenic-transmission electron microscopy. The fibril substructure is probed via detailed X-ray scattering experiments, and are uniquely comprised of\ud twisted tapes only 5 nm wide, set by the width of the antiparallel A12R2 dimers. The packing of the alanine residues leads to distinct “b-sheet” spacings compared to those for amyloid-forming peptides. For this peptide, b-sheet structure coexists with some a-helical content. These ultrafine amyloid fibrils present arginine at high density on their surfaces, and this may lead to applications in\ud nanobiotechnology.

Several ways of tuning a higher asymmetry factor (>10) in V-channel X-ray monochromators, for metrological and imaging applications, were analysed. A more than sixfold intensity increase for compositionally and thermally tuned cases was achieved., While channel-cut crystals, in which the diffracting surfaces in an asymmetric cut are kept parallel, can provide beam collimation and spectral beam shaping, they can in addition provide beam compression or expansion if the cut is V-shaped. The compression/expansion ratio depends in this case on the total asymmetry factor. If the Ge(220) diffraction planes and a total asymmetry factor in excess of 10 are used, the rocking curves of two diffractors will have a sufficient overlap only if the second diffractor is tuned slightly with respect to the first one. This study compares and analyses several ways of overcoming this mismatch, which is due to refraction, when the Cu Kα1 beam is compressed 21-fold in a V21 monochromator. A more than sixfold intensity increase was obtained if the matching was improved either by a compositional variation or by a thermal deformation. This provided an intensity gain compared with the use of a simple slit in a symmetrical channel-cut monochromator. The first attempt to overcome the mismatch by introducing different types of X-ray prisms for the required beam deflection is described as well. The performance of the V-shaped monochromators is demonstrated in two applications. A narrow collimated monochromatic beam obtained in the beam compressing mode was used for high-resolution grazing-incidence small-angle X-ray scattering measurements of a silicon sample with corrupted surface. In addition, a two-dimensional Bragg magnifier, based on two crossed V15 channel monochromators in beam expansion mode and tuned by means of unequal asymmetries, was successfully applied to high-resolution imaging of test structures in combination with a Medipix detector.

Metal-oxide tunnel junctions made by optical lithography were studied by X-ray diffraction (imaging approach with diffraction contrast) to access local distortions of the crystalline planes of the constituting layers. The effect of the size (10–150 µm) and shape (disc, square and rectangle) of the junction was investigated., X-ray diffraction techniques are used in imaging mode in order to characterize micrometre-sized objects. The samples used as models are metal–oxide tunnel junctions made by optical lithography, with lateral sizes ranging from 150 µm down to 10 µm and various shapes: discs, squares and rectangles. Two approaches are described and compared, both using diffraction contrast: full-field imaging (topography) and raster imaging (scanning probe) using a micrometre-sized focused X-ray beam. It is shown that the full-field image gives access to macroscopic distortions (e.g. sample bending), while the local distortions, at the micrometre scale (e.g. tilts of the crystalline planes in the vicinity of the junction edges), can be accurately characterized only using focused X-ray beams. These local defects are dependent on the junction shape and larger by one order of magnitude than the macroscopic curvature of the sample.

Despite intensive research a physical explanation of high Tc superconductors remains elusive. One reason for this is that these materials have generally a very complex structure making useless theoretical models for a homogeneous system. Little is known on the control of the critical temperature by the space disposition of defects because of lack of suitable experimental probes. X-ray diffraction and neutron scattering experiments used to investigate y oxygen dopants in YBa2Cu3O 6+y lack of spatial resolution. Here we report the spatial imaging of dopants distribution in-homogeneity in YBa2Cu3O6.67 using scanning nano X-ray diffraction. By changing the X-ray beam size from 1 micron to 300 nm of diameter, the lattice inhomogeneity increases. The ordered oxygen puddles size distribution vary between 6-8 nm using 1x1 {\mu}m2 beam, while it is between 5-12 nm with a fat tail using the 300x300 nm2 beam. The increased inhomogeneity at the nanoscale points toward an intrinsic granular complexity., Comment: letter, 4 figures

WOS:000323520600021; International audience; In time-resolved laser pump, X-ray probe wide-angle X-ray scattering experiments on systems in solution the structural response of the system is accompanied by a solvent response. The solvent response is caused by reorganization of the bulk solvent following the laser pump event, and in order to extract the structural information of the solute, the solvent response has to be treated. Methodologies capable of doing so include both theoretical modelling and experimental determination of the solvent response. In the work presented here, we have investigated how to obtain a reproducible solvent response-the solvent term-experimentally when applying laser pump, X-ray probe time-resolved wide-angle X-ray scattering. The solvent term describes difference scattering arising from the structural response of the solvent to changes in the hydrodynamic parameters: pressure, temperature and density. We present results based on NIR and dye mediated solvent heating, and demonstrate that the solvent response is independent of the heating method. The NIR heating is shown to be rendered unusable by higher order effects under certain experimental conditions, while the dye mediated solvent heating is demonstrated to exhibit first order behaviour with respect to the amount of energy deposited in the solution. We introduce a standardized method for recording solvent responses in laser pump, X-ray probe time-resolved X-ray wide-angle scattering experiments by using dye mediated solvent heating. Furthermore, we have generated a library of solvent terms, which can be used to describe the solvent term in any TRWAXS experiment, and made it available online.

A preliminary structural investigation of local disorder in fully oxidized La2 NiO4+δ was performed by Pair Distribution Function (PDF) analyses of X-ray and neutron powder diffraction data. X-ray diffraction data were recorded in-situ on warming from room temperature up to 450 ∘ C.

International audience; We present the recently developed technique of Dark Field X-Ray Microscopy that utilizes the diffraction of hard X-rays from individual grains or subgrains at the (sub)micrometre-scale embedded within mm-sized samples. By magnifying the diffracted signal, 3D mapping of orientations and strains inside the selected grain is performed with an angular resolution of 0.005 and a spatial resolution of 200 nm. Furthermore, the speed of the measurements at high-intensity synchrotron facilities allows for fast non-destructive in situ determination of structural changes induced by annealing or other external influences. The capabilities of Dark Field X-Ray Microscopy are illustrated by examples from an ongoing study of recrystallization of 50% cold-rolled A11050 specimens

The metatarsal lyriform organ of the Central American wandering spider Cupiennius salei is its most sensitive vibration detector. It is able to sense a wide range of vibration stimuli over four orders of magnitude in frequency between at least as low as 0.1 Hz and several kilohertz. Transmission of the vibrations to the slit organ is controlled by a cuticular pad in front of it. While the mechanism of high-frequency stimulus transfer (above ca 40 Hz) is well understood and related to the viscoelastic properties of the pad's epicuticle, it is not yet clear how low-frequency stimuli (less than 40 Hz) are transmitted. Here, we study how the pad material affects the pad's mechanical properties and thus its role in the transfer of the stimulus, using a variety of experimental techniques, such as X-ray micro-computed tomography for three-dimensional imaging, X-ray scattering for structural analysis, and atomic force microscopy and scanning electron microscopy for surface imaging. The mechanical properties were investigated using scanning acoustic microscopy and nanoindentation. We show that large tarsal deflections cause large deformation in the distal highly hydrated part of the pad. Beyond this region, a sclerotized region serves as a supporting frame which resists the deformation and is displaced to push against the slits, with displacement values considerably scaled down to only a few micrometres. Unravelling the structural arrangement in such specialized structures may provide conceptual ideas for the design of new materials capable of controlling a technical sensor's specificity and selectivity, which is so typical of biological sensors.

Degradation of the myelin sheath is a common pathology underlying demyelinating neurological diseases from Multiple Sclerosis to Leukodistrophies. Although large malformations of myelin ultrastructure in the advanced stages of Wallerian degradation is known, its subtle structural variations at early stages of demyelination remains poorly characterized. This is partly due to the lack of suitable and non-invasive experimental probes possessing sufficient resolution to detect the degradation. Here we report the feasibility of the application of an innovative non-invasive local structure experimental approach for imaging the changes of statistical structural fluctuations in the first stage of myelin degeneration. Scanning micro X-ray diffraction, using advances in synchrotron x-ray beam focusing, fast data collection, paired with spatial statistical analysis, has been used to unveil temporal changes in the myelin structure of dissected nerves following extraction of the Xenopus laevis sciatic nerve. The early myelin degeneration is a specific ordered compacted phase preceding the swollen myelin phase of Wallerian degradation. Our demonstration of the feasibility of the statistical analysis of SmXRD measurements using biological tissue paves the way for further structural investigations of degradation and death of neurons and other cells and tissues in diverse pathological states where nanoscale structural changes may be uncovered., Comment: 16 pages, 6 figures

International audience; 2D area detectors like CCD or pixel detectors have become popular in the last 15 years for diffraction experiments (e.g. for WAXS, SAXS, single crystal and powder diffraction (XRPD)). These detectors have a large sensitive area of millions of pixels with high spatial resolution. The software package pyFAI has been designed to reduce SAXS, WAXS and XRPD images taken with those detectors into 1D curves (azimuthal integration) usable by other software for in-depth analysis such as Rietveld refinement, or 2D images (a radial transformation named caking). As a library, the aim of pyFAI is to be integrated into other tools like PyMca or EDNA with a clean pythonic interface. However pyFAI features also command line tools for batch processing, converting data into q-space (q being the momentum transfer) or 2 theta-space (theta being the Bragg angle) and a calibration graphical interface for optimizing the geometry of the experiment using the Debye-Scherrer rings of a reference sample. PyFAI shares the geometry definition of SPD but can directly import geometries determined by the software FIT2D. PyFAI has been designed to work with any kind of detector and geometry (transmission or reflection) and relies on FabIO, a library able to read more than 20 image formats produced by detectors from 12 different manufacturers. During the transformation from cartesian space (x, y) to polar space (2 theta, chi), both local and total intensities are conserved in order to obtain accurate quantitative results. Technical details on how this integration is implemented and how it has been ported to native code and parallelized on graphic cards are discussed in this paper