X-ray Laue microdiffraction aims to characterize microstructural and mechanical fields in polycrystalline specimens at the sub-micrometre scale with a strain resolution of ∼10. Here, a new and unique Laue microdiffraction setup and alignment procedure is presented, allowing measurements at temperatures as high as 1500 K, with the objective to extend the technique for the study of crystalline phase transitions and associated strain-field evolution that occur at high temperatures. A method is provided to measure the real temperature encountered by the specimen, which can be critical for precise phase-transition studies, as well as a strategy to calibrate the setup geometry to account for the sample and furnace dilation using a standard α-alumina single crystal. A first application to phase transitions in a polycrystalline specimen of pure zirconia is provided as an illustrative example.
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http://dx.doi.org/10.1107/S1600576724001821 | DOI Listing |
J Appl Crystallogr
April 2024
PIMM (UMR CNRS 8006), CNRS, ENSAM, Cnam, HESAM, 155 Boulevard de l'Hopital, Paris 75013, France.
X-ray Laue microdiffraction aims to characterize microstructural and mechanical fields in polycrystalline specimens at the sub-micrometre scale with a strain resolution of ∼10. Here, a new and unique Laue microdiffraction setup and alignment procedure is presented, allowing measurements at temperatures as high as 1500 K, with the objective to extend the technique for the study of crystalline phase transitions and associated strain-field evolution that occur at high temperatures. A method is provided to measure the real temperature encountered by the specimen, which can be critical for precise phase-transition studies, as well as a strategy to calibrate the setup geometry to account for the sample and furnace dilation using a standard α-alumina single crystal.
View Article and Find Full Text PDFMaterials (Basel)
April 2023
Institute of Stochastics, Ulm University, 89096 Ulm, Germany.
Laue microdiffraction is an X-ray diffraction technique that allows for the non-destructive acquisition of spatial maps of crystallographic orientation and the strain state of (poly)crystalline specimens. To do so, diffraction patterns, consisting of thousands of Laue spots, are collected and analyzed at each location of the spatial maps. Each spot of these so-called Laue patterns has to be accurately characterized with respect to its position, size and shape for subsequent analyses including indexing and strain analysis.
View Article and Find Full Text PDFJ Appl Crystallogr
October 2022
Department of Civil and Mechanical Engineering, Technical University of Denmark, Kongens Lyngby, 2800, Denmark.
X-ray Laue diffraction is an important method for characterizing the local crystallographic orientation and elastic strain in polycrystalline materials. Existing analysis methods are designed mainly to index a single or a few Laue diffraction pattern(s) recorded in a detector image. In this work, a novel method called dictionary-branch-bound (DBB) is presented to determine the crystallographic orientations of multiple crystals simultaneously illuminated by a parallel X-ray incident beam, using only the spot positions in a detector image.
View Article and Find Full Text PDFJ Appl Crystallogr
August 2022
Univ. Grenoble Alpes, UMR SYMMES CNRS-CEA, 17 avenue des Martyrs, Grenoble 38000, France.
A feed-forward neural-network-based model is presented to index, in real time, the diffraction spots recorded during synchrotron X-ray Laue microdiffraction experiments. Data dimensionality reduction is applied to extract physical 1D features from the 2D X-ray diffraction Laue images, thereby making it possible to train a neural network on the fly for any crystal system. The capabilities of the LaueNN model are illustrated through three examples: a two-phase nano-structure, a textured high-symmetry specimen deformed and a polycrystalline low-symmetry material.
View Article and Find Full Text PDFACS Appl Mater Interfaces
July 2022
MBLEM, Department of Engineering Science, University of Oxford, Oxford OX1 3PJ, U.K.
To explore an effective route of customizing the superelasticity (SE) of NiTi shape memory alloys via modifying the grain structure, binary NiTi (wt) alloys were fabricated in as-cast, hot swaged, and hot-rolled conditions, presenting contrasting grain sizes and grain boundary types. synchrotron X-ray Laue microdiffraction and synchrotron X-ray powder diffraction techniques were employed to unravel the underlying grain structure mechanisms that cause the diversity of SE performance among the three materials. The evolution of lattice rotation, strain field, and phase transformation has been revealed at the micro- and mesoscale, and the effect of grain structure on SE performance has been quantified.
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