Characterization of polycrystalline materials by X-ray diffraction contrast tomography

National audienceSynchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for characterizing the grain microstructure in a variety of polycrystalline mono-and multiphase materials. Direct visualization of the three-dimensional grain boundary network or of two-phase (duplex) grain structures by means of absorption and/or phase contrast techniques is possible, but restricted to specific material systems (Ludwig 2009b). However, conventional attenuation or phase contrast imaging techniques do not give access to the crystallographic orientation of the grains and additional diffraction measurements are required. On the other hand, three-dimensional X-ray diffraction methods like Differential Aperture X-ray Microscopy (DAXM, (Larson, 2002) or 3D X-ray Diffraction Microscopy (3DXRD) (Poulsen, 2004) can analyse the 3D grain structure and/or elastic strain tensors of individual grains in polycrystalline materials, but are blind to the microstructural features (inclusions, cracks and porosity) visible in attenuation and/or phase contrast imaging techniques . A recent extension of the 3DXRD methodology, termed X-ray diffraction contrast tomography (DCT) (Ludwig 2009a), combines the principles of 3DXRD and X-ray absorption tomography. With a single scan, DCT can provide simultaneous access to the grain shape, crystallographic orientation, full elastic strain tensor and the local attenuation coefficient distribution in three dimensions. The technique applies to a range of plastically undeformed, polycrystalline mono-phase materials, fulfilling some conditions on grain size and texture. The straightforward combination with in-situ microtomographic observations opens interesting new possibilities for the characterization of microstructure related damage and deformation mechanisms in these materials

Simulation par éléments finis de la déformation de polycristaux à partir d'images de tomographie par contraste de diffraction

National audienceLa tomographie par contraste de diffraction donne accès à la forme, l'orientation et l'état de déformation élastique des grains dans des volumes polycristallins pouvant contenir à l'heure actuelle jusqu'à mille grains. La combinaison de cette technique avec la méthode des éléments finis est particuliè- rement prometteuse pour analyser le rôle de la cristallographie locale sur les mécanismes de déformation et de dégradation dans des matériaux polycristallins. Dans ce travail, un échantillon polycristallin de titane est imagé en 3D puis maillé et sa déformation de traction est calculée par éléments finis.See http://hal.archives-ouvertes.fr/docs/00/59/29/18/ANNEX/r_974AO844.pd

The grain microstructure of polycrystalline materials as revealed by the combined use of synchrotron X-ray imaging and diffraction techniques

National audienceCombining the principles of x-ray imaging and diffraction techniques, it has recently become possible to map the 3D grain microstructure in a range of polycrystalline materials. Associating this 3D orientation mapping with conventional attenuation and/or phase contrast tomography yields a non-destructive characterization technique, enabling time-lapse observation of dynamic processes in the bulk of structural materials. The capabilities and limitations., as well as future perspectives of this new characterization approach will be discussed and illustrated on selected application examples

Three-dimensional grain mapping by x-ray diffraction contrast tomography and the use of Friedel pairs in diffraction data analysis

X-ray diffraction contrast tomography (DCT) is a technique for mapping grain shape and orientation in plastically undeformed polycrystals. In this paper, we describe a modified DCT data acquisition strategy which permits the incorporation of an innovative Friedel pair method for analyzing diffraction data. Diffraction spots are acquired during a 360 degrees rotation of the sample and are analyzed in terms of the Friedel pairs ((hkl) and (hkl) reflections, observed 180 degrees apart in rotation). The resulting increase in the accuracy with which the diffraction vectors are determined allows the use of improved algorithms for grain indexing (assigning diffraction spots to the grains from which they arise) and reconstruction. The accuracy of the resulting grain maps is quantified with reference to synchrotron microtomography data for a specimen made from a beta titanium system in which a second phase can be precipitated at grain boundaries, thereby revealing the grain shapes. The simple changes introduced to the DCT methodology are equally applicable to other variants of grain mapping. ©2009 American Institute of Physic

4D characterization of metals by 3DXRD

31st Riso International Symposium on Materials Science, Roskilde, DENMARK, SEP 06-10, 2010International audienceThe status of 3DXRD microscopy is reviewed, with a special view to applications in metallurgy. Various approaches are compared in terms of perfounance. In addition several recent advances are presented, such as a 3D grain map with an unprecedented spatial resolution of 500 nm, first results from the commissioning of a novel 3D detector set-up and a validation of the box-scan procedure

Heterogeneous grain-scale response in ferroic polycrystals under electric field

Understanding coupling of ferroic properties over grain boundaries and within clusters of grains in polycrystalline materials is hindered due to a lack of direct experimental methods to probe the behaviour of individual grains in the bulk of a material. Here, a variant of three-dimensional X-ray diffraction (3D-XRD) is used to resolve the non-180?? ferroelectric domain switching strain components of 191 grains from the bulk of a polycrystalline electro-ceramic that has undergone an electric-field-induced phase transformation. It is found that while the orientation of a given grain relative to the field direction has a significant influence on the phase and resultant domain texture, there are large deviations from the average behaviour at the grain scale. It is suggested that these deviations arise from local strain and electric field neighbourhoods being highly heterogeneous within the bulk polycrystal. Additionally, the minimisation of electrostatic potentials at the grain boundaries due to interacting ferroelectric domains must also be considered. It is found that the local grain-scale deviations average out over approximately 10-20 grains. These results provide unique insight into the grain-scale interactions of ferroic materials and will be of value for future efforts to comprehensively model these and related materials at that length-scaleopen

Valaciclovir to prevent Cytomegalovirus mediated adverse modulation of the immune system in ANCA-associated vasculitis (CANVAS):study protocol for a randomised controlled trial

BACKGROUND: The ANCA-associated vasculitides (AAV) are systemic autoimmune inflammatory disorders characterised by necrotising inflammation affecting small to medium-sized blood vessels. Despite improvements in survival, infection and cardiovascular disease remain leading causes of morbidity and mortality. Considerable evidence suggests that CD4 + CD28null T-cell expansions, predominantly seen in Cytomegalovirus (CMV) seropositive individuals, are associated with systemic dysregulation of immune function leading to a heightened risk of infection and cardiovascular disease. In patients with AAV, CD4 + CD28null expansions are driven by CMV and are associated with an increased risk of infection and mortality. The aim of this study is to explore in detail the ways in which CMV modulates the immune system and to determine whether treatment with valaciclovir blocks subclinical CMV reactivation in CMV seropositive AAV patients and ameliorates the CMV-induced adverse effects on the immune system. METHODS/DESIGN: CANVAS is a single-centre prospective open-label randomised controlled proof-of-concept trial of 50 adult CMV seropositive patients with stable AAV. Participants will be randomly allocated to receive valaciclovir orally (2 g QDS or reduced according to renal function) or no additional treatment for 6 months with an additional 6-month follow-up period. The primary outcome is the proportion of patients with CMV reactivation, as assessed by measurable viral load on quantitative blood and urine CMV polymerase chain reaction. The secondary outcomes are safety, change in the proportion of CD4+ CMV-specific T-cell population (defined as CD4 + CD28null cells) and change in soluble markers of inflammation from baseline to 6 months. Further tertiary and exploratory outcomes include persistence of the effect of valaciclovir on the proportion of CD4 + CD28null cells at 6 months post completion of treatment, change in the immune phenotype of CD4+ T cells and change in blood pressure and arterial stiffness parameters from baseline to 6 months. DISCUSSION: The results of this study will enable larger studies to be conducted to determine whether by controlling subclinical CMV reactivation, we can improve clinical endpoints such as infection and cardiovascular disease. The potential impact of this study is not limited to AAV, as CD4 + CD28null cells have been linked to adverse outcomes in other inflammatory conditions and in the context of an ageing immune system. TRIAL REGISTRATION: ClinicalTrials.gov Identifier NCT01633476 (registered 29 June 2012). ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (doi:10.1186/s13063-016-1482-2) contains supplementary material, which is available to authorized users

First laboratory X‐ray diffraction contrast tomography for grain mapping of polycrystals

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