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12 results on '"Nanostructures et Rayons X (NRX)"'

1. Imaging the strain evolution of a platinum nanoparticle under electrochemical control

Author

Clément Atlan, Corentin Chatelier, Isaac Martens, Maxime Dupraz, Arnaud Viola, Ni Li, Lu Gao, Steven J. Leake, Tobias U. Schülli, Joël Eymery, Frédéric Maillard, Marie-Ingrid Richard, European Synchroton Radiation Facility [Grenoble] (ESRF), Electrochimie Interfaciale et Procédés (EIP), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI), Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Eindhoven University of Technology [Eindhoven] (TU/e), and European Project: 818823,CARINE

Subjects
[PHYS.MECA.MEMA]Physics [physics]/Mechanics [physics]/Mechanics of materials [physics.class-ph], Mechanics of Materials, Mechanical Engineering, General Materials Science, [CHIM.CATA]Chemical Sciences/Catalysis, [CHIM.MATE]Chemical Sciences/Material chemistry, General Chemistry, Condensed Matter Physics
Abstract

International audience; Surface strain is widely employed in gas phase catalysis and electrocatalysis to control the binding energies of adsorbates on active sites. However, in situ or operando strain measurements are experimentally challenging, especially on nanomaterials. Here, we exploit coherent diffraction at the new 4 th generation Extremely Brilliant Source at the European Synchrotron Radiation Facility (ESRF-EBS) to map and quantify strain inside individual Pt catalyst nanoparticles under electrochemical control. 3D nanoresolution strain microscopy together with density functional theory and atomistic simulations show for the first time evidence of heterogeneous and potential-dependent strain distribution between highly-coordinated ({100} and {111} facets) and under-coordinated atoms (edges and corners) as well as evidence of strain propagation from the surface to the bulk of the nanoparticle. These dynamic structural relationships directly inform the design of strain-engineered nanocatalysts for energy storage and conversion applications.

Published
2023
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2. Employing surface curvature for spatially resolved X‐ray reflectivity: graphene domains on liquid copper

Author

Valentina Belova, Maciej Jankowski, Mehdi Saedi, Irene M. N. Groot, Gilles Renaud, Oleg V. Konovalov, European Synchroton Radiation Facility [Grenoble] (ESRF), Leiden Institute of Chemistry, Universiteit Leiden, Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Nanostructures et Rayons X (NRX), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and European Project: 951943,DirectSepa

Subjects
[PHYS]Physics [physics], Mechanics of Materials, Mechanical Engineering
Abstract

Here we demonstrate the possibility of utilizing X-ray reflectivity for visualization with ~μm spatial resolution of a surface with a heterogeneous electron density due to a partial coverage by another nanometrically thin material. It requires the sample to be convexly bent, thus reflecting the collimated incident beam onto a magnified image recorded by a position-sensitive detector. By the use of a small, about ten microns, intense, and parallel beam such as provided by the most recent synchrotron sources, one can record such spatially resolved X-ray reflectivity with 0.1‒1 kHz frame rate. We demonstrate the use of the method for in situ, time-resolved characterization of single-layer graphene domains during their chemical vapor deposition on a naturally curved surface of a liquid copper drop. This method can follow the growth kinetics, including the coverage ratio, two-dimensional crystal (flake) sizes, and distances between flakes. By taking a single snapshot, we can reconstruct the individual X-ray reflectivity curves, of both covered and non-covered parts of the liquid surface, and thus deduce the corresponding electron density profiles perpendicular to the surface. The technique has a promising perspective for in situ study of two-dimensional materials, ultra-thin films, and self-assemblies on liquid as well as solid surfaces.

Published
2023
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3. M -plane AlGaN digital alloy for microwire UV-B LEDs

Author

Lucie Valera, Vincent Grenier, Sylvain Finot, Catherine Bougerol, Joël Eymery, Gwénolé Jacopin, Christophe Durand, Nanophysique et Semiconducteurs (NPSC), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Semi-conducteurs à large bande interdite (NEEL - SC2G), Institut Néel (NEEL), Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Nanophysique et Semiconducteurs (NEEL - NPSC), Modélisation et Exploration des Matériaux (MEM), Nanostructures et Rayons X (NRX), ANR-15-IDEX-0002,UGA,IDEX UGA(2015), and ANR-22-CE51-0032,HARAlN,Fabrication de nanosources émettant efficacement dans l'UV profond à partir de nanofils AlN à fort facteur de forme(2022)

Subjects
Physics and Astronomy (miscellaneous), [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

International audience; The growth of non-polar AlGaN digital alloy (DA) is achieved by metal-organic vapor phase epitaxy using GaN microwire m-facets as the template. This AlGaN DA consisting of five periods of two monolayer-thick layers of GaN and AlGaN (approximately 50% Al-content) is integrated into the middle of an n-p GaN/AlGaN junction to design core-shell wire- μLED. The optical emission of the active zone investigated by 5 K cathodoluminescence is consistent with the AlGaN bulk alloy behavior. Several contributions from 295 to 310 nm are attributed to the lesser thickness and/or composition fluctuations of AlGaN DA. Single-wire μLED is fabricated using a lithography process, and I–V measurements confirm a diode rectifying behavior. Room temperature UV electroluminescence originating from m-plane AlGaN DA is accomplished at 310 nm.

Published
2023
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4. Superstructures, Commensurations, and Rotation of Single-Layer TaS 2 on Au(111) Induced by Cs Intercalation/Deintercalation

Author

Xiaorong Weng, Philippe David, Valérie Guisset, Lucio Martinelli, Olivier Geaymond, Johann Coraux, Gilles Renaud, Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)

Subjects
[PHYS]Physics [physics], General Engineering, General Physics and Astronomy, General Materials Science
Abstract

International audience

Published
2023
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5. In situ and operando 3D imaging of Pt and Pd electrocatalytic nanocrystals

Author

Atlan, Clément, Chatelier, Corentin, Viola, Arnaud, Dupraz, Maxime, Leake, Steven, Eymery, J., Maillard, Frédéric, Richard, Marie‐ingrid, European Synchroton Radiation Facility [Grenoble] (ESRF), Electrochimie Interfaciale et Procédés (EIP), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI), Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), The Minerals, Metals & Materials Society (TMS), European Project: 818823,CARINE, European Project: 952184,HERMES, and Nanostructures et Rayonnement Synchrotron (NRS )

Subjects
[CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.CATA]Chemical Sciences/Catalysis
Abstract

International audience; Structural properties of transition metal are critical to understand the catalytic behavior of electrochemical processes. Here we show that 200 nm Pt and 500 nm Pd nanocrystals can be probed in situ and operando through Bragg Coherent X-ray Diffraction Imaging. This lens-less technique enables determining the morphology as well as mapping the strain and displacement fields of such nanoparticles. By measuring the Pt 002 Bragg reflection we show evidence of heterogeneous and potential-dependent strain distribution between highly-coordinated ({100} and {111} facets) and under-coordinated atoms (edges and corners) as well as evidence of strain propagation from the surface to the bulk of the nanoparticle. This allows to unveil adsorption sites. We also demonstrate that the formation of highly strained palladium hydride nanocrystals can be tracked under potential control. Even though the beta phase (hydrogen rich) Bragg peak comes and vanishes at relevant potentials, the nanocrystal does not recover its pristine morphology.

Published
2023

6. Anomalous Glide Plane in Platinum Nano- and Microcrystals

Author

Marie-Ingrid Richard, Stéphane Labat, Maxime Dupraz, Jérôme Carnis, Lu Gao, Michaël Texier, Ni Li, Longfei Wu, Jan P. Hofmann, Mor Levi, Steven J. Leake, Sergey Lazarev, Michael Sprung, Emiel J.M. Hensen, Eugen Rabkin, Olivier Thomas, Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), European Synchroton Radiation Facility [Grenoble] (ESRF), Institut des Matériaux, de Microélectronique et des Nanosciences de Provence (IM2NP), Aix Marseille Université (AMU)-Université de Toulon (UTLN)-Centre National de la Recherche Scientifique (CNRS), Eindhoven University of Technology [Eindhoven] (TU/e), Technische Universität Darmstadt - Technical University of Darmstadt (TU Darmstadt), Technion - Israel Institute of Technology [Haifa], Deutsches Elektronen-Synchrotron [Hamburg] (DESY), Technische Universiteit Eindhoven (TU/e), ANR-21-CE08-0033,DINACS,Défauts dans les nanocristaux: Imagerie par diffraction cohérente des rayons X et simulations(2021), European Project: 818823,CARINE, Inorganic Materials & Catalysis, and EIRES Chem. for Sustainable Energy Systems

Subjects
[PHYS]Physics [physics], Glide planes, Bragg coherent diffraction imaging, General Engineering, General Physics and Astronomy, General Materials Science, platinum, defects, dislocations
Abstract

International audience; At the nanoscale, the properties of materials depend critically on the presence of crystal defects. However, imaging and characterising the structure of defects in three dimensions inside a crystal remain a challenge. Here, by using Bragg coherent diffraction imaging, we observe an unexpected anomalous {110} glide plane in two Pt sub-micrometer crystals grown by very different processes and having very different morphologies. The structure of the defects (type, associated glide plane and lattice displacement) is imaged in these faceted Pt crystals. Using this non-invasive technique both plasticity and unusual defect behaviour can be probed at the nanoscale.

Published
2023
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7. UV emission from MOVPE nanowire LEDs

Author

Durand, Christophe, Grenier, Vincent, Finot, Sylvain, Valera, Lucie, Bougerol, C., Eymery, Joël, Jacopin, Gwenolé, Nanophysique et Semiconducteurs (NPSC), PHotonique, ELectronique et Ingénierie QuantiqueS (PHELIQS), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Semi-conducteurs à large bande interdite (NEEL - SC2G), Institut Néel (NEEL), Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Nanophysique et Semiconducteurs (NEEL - NPSC), Modélisation et Exploration des Matériaux (MEM), Nanostructures et Rayons X (NRX), and SPIE

Subjects
[PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [SPI.OPTI]Engineering Sciences [physics]/Optics / Photonic, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

International audience; The use of nanowires has recently emerged to go further in the development of nitride UV LEDs, especially to improve the efficiency or to make micro-sized UV-sources and flexible LEDs/photodetectors. Our current research interest is focused on the core-shell UV quantum wells grown by industrial MOVPE epitaxy tool. Several types of core-shell quantum wells have been successfully achieved: GaN/InAlN for UV-A, GaN/AlGaN or AlGaN/AlGaN for UV-A and UV-B. When the UV GaN/AlGaN QWs are embedded in a core-shell AlGaN p-n junction, the electroluminescence is demonstrated on single-wire μLEDs in the UV-A and UV-B. The further development of core-shell GaN/AlGaN monolayered system is also shown with demonstration of UV-B emission for single-wire μLEDs.

Published
2023
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8. Taking Bragg Coherent Diffraction Imaging to Higher Energies at Fourth Generation Synchrotrons: Nanoscale Characterization

Author

Richard, Marie-Ingrid, Martens, Isaac, Dupraz, Maxime, Drnec, Jakub, Honkimäki, Veijo, Chatelier, Corentin, Atlan, Clément, Mirolo, Marta, Levi, Mor, Rabkin, Eugen, Eymery, Joël, Naidu, Akshata, Schülli, Tobias, Leake, Steven, Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), European Synchroton Radiation Facility [Grenoble] (ESRF), European Synchrotron Radiation Facility (ESRF), Technion - Israel Institute of Technology [Haifa], Nanostructures et Rayonnement Synchrotron (NRS ), European Synchrotron Research Facility, and European Project: 818823,CARINE

Subjects
[PHYS]Physics [physics], Bragg coherent diffraction imaging, strain, high-energy Bragg coherent diffraction imaging nanostructures strain morphology diffraction, nanostructures, morphology, diffraction, [CHIM.CRIS]Chemical Sciences/Cristallography, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], high-energy, [CHIM.MATE]Chemical Sciences/Material chemistry, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat]
Abstract

International audience; High-energy Bragg coherent diffraction imaging (BCDI) can enable three-dimensional imaging of atomic structure within individual crystallites in complex environments. Here, we show that sufficient coherent photon flux is available to extend the BCDI technique to higher energies to: 1) obtain improved strain information and sensitivity 1 at the nanoscale with higher order Bragg reflections, 2) exploit BCDI in embedded materials or complex operando environments, 3) reduce x-ray induced sample modification and 4) minimize dynamical scattering effects. We demonstrate the nanoscale imaging technique on the same sub-micron sized crystal at 8.5, 19.9 and 33.4 keV by taking advantage of the brilliance and coherence of the fourth generation Extremely Brilliant Source of the ID01 beamline at ESRF-The European Synchrotron (Grenoble, France). The photon flux, data quality, resolution and strain information are compared. We also show first coherent diffraction measurements performed at the ID31-EBS beamline at an energy of 41 keV.

Published
2023
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9. Structural evolution of nanoparticles under realistic conditions observed with Bragg coherent X-ray imaging

Author

Richard, M.I., Dupraz, M., Chatelier, C., Atlan, C., Bellec, E., Li, N., Labat, S., Schülli, T., Rabkin, E., Thomas, O., Eymery, J., Leake, S., Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), CRG & Grands instruments (NEEL - CRG), Institut Néel (NEEL), Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), European Synchroton Radiation Facility [Grenoble] (ESRF), Institut des Matériaux, de Microélectronique et des Nanosciences de Provence (IM2NP), Aix Marseille Université (AMU)-Université de Toulon (UTLN)-Centre National de la Recherche Scientifique (CNRS), and Technion - Israel Institute of Technology [Haifa]

Subjects
Inorganic Chemistry, Structural Biology, General Materials Science, Physical and Theoretical Chemistry, Condensed Matter Physics, Biochemistry, [SPI.MAT]Engineering Sciences [physics]/Materials
Published
2022
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10. In situ 3D observations of a core–shell volume transition in an Ni 3 Fe nanocrystal using Bragg coherent X-ray diffraction imaging

Author

C. Chatelier, C. Atlan, M. Dupraz, N. Li, E. Rabkin, S. Labat, J. Eymery, M.I. Richard, Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), CRG & Grands instruments (NEEL - CRG), Institut Néel (NEEL), Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), European Synchroton Radiation Facility [Grenoble] (ESRF), Technion - Israel Institute of Technology [Haifa], Institut des Matériaux, de Microélectronique et des Nanosciences de Provence (IM2NP), and Aix Marseille Université (AMU)-Université de Toulon (UTLN)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Inorganic Chemistry, Structural Biology, General Materials Science, Physical and Theoretical Chemistry, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], Condensed Matter Physics, Biochemistry, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

Coherent X-ray Diffraction Imaging (CDI) [1] allows for the in situ 3D mapping of the structural changes during phasetransitions and chemical reactions, with a fair spatial resolution of the order of magnitude of 10 nm [2]. Using thistechnique in multi-Bragg conditions (Bragg CDI on multiple reflections), it was possible to follow the structural evolution(change in morphology, variation of the displacement and strain fields) as a function of temperature in a 300 nm Ni 3Fenanocrystal. During this volume transition, which happens between 500°C and 600°C, a core-shell structure isprogressively observed with two distinct lattice parameters (difference of 0.39%, corresponding to two different Ni:Feratios), leading to highly strained and coherent domains. A rounding of the particle is also observed, with a disappearingof the initial facets. Static molecular calculations (LAMMPS) of different systems, such as faceted and core-shellnanoparticles, complete this work and allow for the confirmation of a core-shell structure. This study shows the perfectability of modern phase retrieval methods to reconstruct highly strained systems such as core-shell nanoparticles.

Published
2022
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11. Coherent diffraction imaging at space-group forbidden reflections

Author

Beutier, Guillaume, Eymery, Joel, Dupraz, Maxime, Richard, Marie-Ingrid, Wartelle, Alexis, Verdier, Marc, de Boissieu, Marc, Collins, Steven, Bellec, Ewen, Favre-Nicolin, Vincent, Leake, Steven, Science et Ingénierie des Matériaux et Procédés (SIMaP), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), CRG & Grands instruments (NEEL - CRG), Institut Néel (NEEL), Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), DIAMOND Light source, European Synchroton Radiation Facility [Grenoble] (ESRF), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Diamond Light Source Limited [Didcot, UK], Harwell Science and Innovation Campus [Didcot, UK], and the ESRF for beamtime allocation under project number MI-1377

Subjects
Inorganic Chemistry, Structural Biology, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM.CRIS]Chemical Sciences/Cristallography, General Materials Science, [CHIM.MATE]Chemical Sciences/Material chemistry, [PHYS.COND.CM-SCE]Physics [physics]/Condensed Matter [cond-mat]/Strongly Correlated Electrons [cond-mat.str-el], [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], Physical and Theoretical Chemistry, Condensed Matter Physics, Biochemistry, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

On one hand, coherent diffraction imaging (CDI) in Bragg geometry has emerged as a unique 3D microscopy ofnanocrystals thanks to 3rd generation synchrotron sources. Away from absorption edges and at space-groupallowed reflections, it provides not only the electronic density but also, encoded in the phase, the atomicdisplacement field with respect to the mean lattice, which in turn reveals crystal strain, defects, and domains.On the other hand, some crystal structures have crystallographic reflections which are forbidden by the space-group symmetry but can nevertheless be observed at a suitable X-ray absorption edge, due to the anisotropy of thetensor of scattering (ATS). They are several orders of magnitude weaker than allowed reflections, but theabsence of Thomson scattering allows the observation of various electronic phenomena related to electronic orders(magnetic, charge, orbital), as well as static and dynamic atomic displacements.The new generation of synchrotron sources, such as the ESRF “Extremely Bright Source”, opens opportunities toperform CDI on such weak reflections. Here we report on the measurement of the (115) forbidden reflection of aGaN nanopillar at the Ga K edge. Sufficient statistics could be obtained in a total accumulation time of~30 minutes for an entire rocking curve to retrieve the phase of the scattering function. Suchmeasurement at high temperatures would provide an image of the inhomogeneity of thermal motion in the crystal,which would be particularly interesting close to surfaces, inversion domain boundaries, and crystal defects. Thisproof-of-principle experiment demonstrates that forbidden reflections are a new opportunity for CDI with the newsynchrotron sources.

Published
2021
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12. Revisiting Phase Transformation Mechanisms in LiNi 0.5 Mn 1.5 O 4 High Voltage Cathodes with Operando Microdiffraction

Author

Isaac Martens, Nikita Vostrov, Marta Mirolo, Mattia Colalongo, Peter Kúš, Marie-Ingrid Richard, Lianzhou Wang, Xiaobo Zhu, Tobias U. Schülli, Jakub Drnec, European Synchroton Radiation Facility [Grenoble] (ESRF), Nanostructures et Rayons X (NRX), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), and European Project: 818823,CARINE

Subjects
General Chemical Engineering, Biomedical Engineering, [CHIM]Chemical Sciences, General Materials Science
Abstract

International audience; Understanding the phase transition mechanisms of active materials inside Li-ion batteries is critical for rechargeability and optimizing the power/energy density of devices. In this work, high-energy microfocused X-ray diffraction is used to measure in operando the state-of-charge heterogeneities inside a high-voltage spinel (LiMn1.5Ni0.5O4, LMNO) cathode. The structure of an active material which resists complete delithiation is studied to move toward unlocking the full storage capacity of ion-conductive spinels. High-precision diffraction also reveals nonlinear coupling between strain and lithiation state inside the cathode at high voltages, which suggests the phase diagram of this material is more complex than previously assumed. X-ray diffraction depth-profiling shows that large lithiation heterogeneities through the cross-section of the electrode are formed even at low currents and that decoupling these gradients are necessary to study the phase transitions in detail.

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