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1. Imaging the Breathing of a Platinum Nanoparticle in Electrochemical Environment

Author

Atlan, Clément, Chatelier, Corentin, Dupraz, Maxime, Martens, Isaac, Viola, Arnaud, Li, Ni, Gao, Lu, Leake, Steven J., Schülli, Tobias U., Eymery, Joël, Maillard, Frédéric, and Richard, Marie-Ingrid

Subjects
Condensed Matter - Materials Science
Abstract

Surface strain is widely used in gas phase catalysis and electrocatalysis to control the binding energies of adsorbates on metal surfaces. However, $in$ $situ$ or $operando$ strain measurements are experimentally challenging, especially on nanomaterials. Here, we take advantage of the 4$^{th}$ generation Extremely Brilliant Source at the European Synchrotron Radiation Facility (ESRF-EBS, Grenoble, France) to quantify the distribution of strain inside a Pt nanoparticle, and to determine its morphology in an electrochemical environment. Our results 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 results provide dynamic structural insights to better simulate and design efficient nanocatalysts for energy storage and conversion applications.

Published
2022
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5. Taking Bragg Coherent Diffraction Imaging to Higher Energies at Fourth Generation Synchrotrons: Nanoscale Characterization

Author

Richard, Marie-Ingrid, primary, Martens, Isaac, additional, Dupraz, Maxime, additional, Drnec, Jakub, additional, Honkimäki, Veijo, additional, Chatelier, Corentin, additional, Atlan, Clément, additional, Mirolo, Marta, additional, Levi, Mor, additional, Rabkin, Eugen, additional, Eymery, Joël, additional, Naidu, Akshata, additional, Schülli, Tobias U., additional, and Leake, Steven J., additional

Published
2023
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7. Unraveling the synergistic effects of Cu-Ag tandem catalysts during electrochemical CO2 reduction using nanofocused X-ray probes.

Author

Frisch, Marvin L., Wu, Longfei, Atlan, Clément, Ren, Zhe, Han, Madeleine, Tucoulou, Rémi, Liang, Liang, Lu, Jiasheng, Guo, An, Nong, Hong Nhan, Arinchtein, Aleks, Sprung, Michael, Villanova, Julie, Richard, Marie-Ingrid, and Strasser, Peter

Subjects
CATALYSTS, CATALYTIC activity, LATTICE dynamics, CARBON dioxide reduction, ELECTROLYTIC reduction, CATALYST structure, PHOTOCATHODES
Abstract

Controlling the selectivity of the electrocatalytic reduction of carbon dioxide into value-added chemicals continues to be a major challenge. Bulk and surface lattice strain in nanostructured electrocatalysts affect catalytic activity and selectivity. Here, we unravel the complex dynamics of synergistic lattice strain and stability effects of Cu-Ag tandem catalysts through a previously unexplored combination of in situ nanofocused X-ray absorption spectroscopy and Bragg coherent diffraction imaging. Three-dimensional strain maps reveal the lattice dynamics inside individual nanoparticles as a function of applied potential and product yields. Dynamic relations between strain, redox state, catalytic activity and selectivity are derived. Moderate Ag contents effectively reduce the competing evolution of H2 and, concomitantly, lead to an enhanced corrosion stability. Findings from this study evidence the power of advanced nanofocused spectroscopy techniques to provide new insights into the chemistry and structure of nanostructured catalysts. Combining in situ nanoprobe techniques paves the way for gaining insights into structure-selectivity relations for electrocatalysts. Herein, the dynamic evolution of lattice strain in individual nanoparticles is directly visualized with nanoscale resolution in Cu-Ag tandem catalysts during the electrocatalytic conversion of CO2 into value-added chemicals. [ABSTRACT FROM AUTHOR]

Published
2023
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8. 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

9. Breathing Pt nanoparticle imaged using in situ BCDI

Author

Atlan, Clément, Chatelier, Corentin, Martens, Isaac, Dupraz, Maxime, Leake, Steven, Richard, Marie-Ingrid, Viola, Arnaud, Maillard, Frédéric, 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), 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), European Synchroton Radiation Facility [Grenoble] (ESRF), ESRF, European Project: 818823,CARINE, and European Project: 952184,HERMES

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

International audience; The relationship between surface strain and the rate of a (electro-)catalytic reaction was unveiled by Hammer and Nørskov using density functional theory (DFT) calculations [1,2]. They proposed that the rate of the sluggish oxygen reduction reaction (ORR) would be enhanced on Pt-based catalysts binding *OH species ca. 0.10 - 0.15 eV more weakly than Pt(111), [1, 2] later experimentally verified using a Pt3Ni(111)-skin surface.[3] Nevertheless these predictions did not translate to Pt-based nanocatalysts, in part because these feature present multiple catalytic sites with a range of binding energies. Also, DFT calculations consider catalytic surfaces in vacuum, i.e. in the absence of water molecules and electric field. Hence, an in situ picture of how strain is distributed on Pt-based surfaces is still lacking.In this contribution, we took benefit of recent advances in Bragg Coherent Diffraction Imaging (BCDI) [4, 5] and of the fourth generation Extremely Brilliant Source of the European Synchrotron (ESRF-EBS, Grenoble, France) to map strain over Pt nanoparticles in electrochemical environment. Our results reveal that strain is heterogeneously distributed between highly- and weakly-coordinated surface atoms, and propagates from the surface to the bulk of the Pt nanoparticle as (bi)sulphates anions adsorb on the surface.

Published
2023

10. Operando potential-induced strain heterogeneity of a breathing Pt nanoparticle: MS40 - Operando and in-situ crystallographic studies

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 Rayonnement Synchrotron (NRS ), 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
[CHIM.MATE]Chemical Sciences/Material chemistry
Abstract

International audience; Pt nanoparticles and their alloys are frequently used as catalysts in a large number of (electro)chemical processes. Understanding how the structure of these catalysts evolve during the reaction is a major challenge to optimize their catalityc performance and activity. Since coherent X-ray diffraction imaging is a nondestructive technique, it allows for the in situ and operando 3D mapping of the sctuctural response of single nanoparticles during electrochemical reaction (i.e. for diffferent electrode potentials) and for different types of electrolyte. Here, we show that the use of this technique allows to follow the 3D evolution of the strain of a Pt nanoparticle during an electrochemical reaction (see Figure 1). More precisely, 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 (see Figure 2). The heterogeneity of strain distribution depends on the electrode potential and reaches as large as 0.08 % at oxygen reduction reaction-relevant potential. These results provide dynamic structural insights to better simulate and design efficient nanocatalysts for energy storage and conversion applications.

Published
2022

11. Structural disorder in ORR electrocatalysis: operation mode, practical descriptors to quantify and foreseen challenges

Author

Chattot, Raphaël, Atlan, Clément, Viola, Arnaud, Chatelier, Corentin, Martens, Isaac, Roiron, Camille, Drnec, Jakub, Bordet, Pierre, Richard, Marie‐ingrid, Dubau, Laetitia, Maillard, Frédéric, 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), 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), European Synchroton Radiation Facility [Grenoble] (ESRF), Matériaux, Rayonnements, Structure (NEEL - MRS), 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 ), ANR-19-ENER-0008,BRIDGE,Vers l'intégration de catalyseurs performants dans des électrodes de pile à combustible efficaces(2019), ANR-14-CE05-0003,HOLLOW,Au-delà des électrocatalyseurs traditionnels : des nanoparticules creuses de métal noble pour applications PEMFC(2014), European Project: 818823,CARINE, Maillard, Frédéric, Vers l'intégration de catalyseurs performants dans des électrodes de pile à combustible efficaces - - BRIDGE2019 - ANR-19-ENER-0008 - ANR-BMBF - VALID, Appel à projets générique - Au-delà des électrocatalyseurs traditionnels : des nanoparticules creuses de métal noble pour applications PEMFC - - HOLLOW2014 - ANR-14-CE05-0003 - Appel à projets générique - VALID, and Coherent diffrAction foR a look Inside Nanostructures towards atomic rEsolution: catalysis and interface - CARINE - 818823 - INCOMING

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

International audience; Due to strain and ligand effects, the simultaneous presence of concave and convex surfaces and their highly-defective nanostructure (atomic vacancies, grain boundaries), highly defective hollow PtNi/C electrocatalysts have proven to enhance remarkably the oxygen reduction reaction (ORR) kinetics [1,2]. Likewise, PtNi aerogel [3], jagged PtNi nanowires [4,5] feature both high concentration of structural defects and enhanced ORR activity. On the other hand, and inspired from single crystal approach, nanostructured octahedral-shaped PtNi/C electrocatalysts exhibiting only Pt(111) facets are among the most active ORR electrocatalysts [6,7]. This presentation will show how structure-activity-stability relationships of these two classes of materials can be unified via two descriptors derived from structural and electrochemical parameters respectively [8,9]. A special emphasis will be given on the stability trends of these two families of ORR electrocatalysts.

Published
2022

14. Mapping Strain in Platinum Nanoparticles via Bragg Coherent Diffraction Imaging

Author

Atlan, Clément, Richard, Marie‐ingrid, Martens, Isaac, Dupraz, Maxime, Chatelier, Corentin, Viola, Arnaud, Leake, Steven, Maillard, Frédéric, 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), 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), European Synchroton Radiation Facility [Grenoble] (ESRF), Electrochimie Interfaciale et Procédés (EIP), 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 ), The Electrochemical Society, ANR-19-ENER-0008,BRIDGE,Vers l'intégration de catalyseurs performants dans des électrodes de pile à combustible efficaces(2019), and European Project: 818823,CARINE

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

International audience; Variations in the interatomic distances lead to altered d-band centre for a given metal, and provide an elegant way to control its activity towards (electro)catalytic reactions (“strain-engineering” approach). The effect of strain was rationalized within the frame of the d-band theory of Hammer and Nørskov in the late 1990s [1,2]. The authors predicted that the rate of the sluggish oxygen reduction reaction (ORR) can be enhanced on catalysts binding *OH ca. 0.10 - 0.15 eV more weakly than Pt(111), [1, 2] and this prediction was experimentally verified using a Pt3Ni(111)-skin surface.[3] Nevertheless, these predictions hardly translated to nanomaterials, because of the wide variety of catalytic sites configurations. Also, the d-band theory mostly considers catalytic surfaces in vacuum, without any effect related to the electrical double layer and adsorption/desorption processes. Hence, an in situ picture of how strain develops on Pt-based surfaces is still lacking.In this contribution, we took benefit of recent advances in Bragg Coherent Diffraction Imaging (BCDI) [4, 5] and of the fourth generation Extremely Brilliant Source of the European Synchrotron (ESRF-EBS, Grenoble, France) to map strain over Pt nanoparticles in situ. Our results show that adsorption of anions causes appearance of compressive strain at under-coordinated (edges and corners) atoms and tensile strain at highly-coordinated ({001} and {111} facets) atoms. Strain heterogeneity increases with the electrode potential and reaches as large as 0.08 %. at ORR-relevant potential. These results provide direct insights into the dynamics of Pt nanoparticles in an electrochemical environment, andhave direct consequences for electrocatalysis in general, and for ORR electrocatalysis in particular.

Published
2022

15. Operando potential-induced strain heterogeneity of a breathing Pt nanoparticle

Author

Atlan, Clément, Chatelier, Corentin, Viola, Arnaud, Dupraz, Maxime, Leake, Steven, Eymery, J., Maillard, Frédéric, Richard, Marie‐ingrid, Maillard, Frédéric, and Coherent diffrAction foR a look Inside Nanostructures towards atomic rEsolution: catalysis and interface - CARINE - 818823 - INCOMING

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

Pt nanoparticles and their alloys are frequently used as catalysts in a large number of (electro)chemical processes. Understanding how the structure of these catalysts evolve during the reaction is a major challenge to optimize their catalityc performance and activity. Since coherent X-ray diffraction imaging is a nondestructive technique, it allows for the in situ and operando 3D mapping of the sctuctural response of single nanoparticles during electrochemical reaction (i.e. for diffferent electrode potentials) and for different types of electrolyte. Here, we show that the use of this technique allows to follow the 3D evolution of the strain of a Pt nanoparticle during an electrochemical reaction (see Figure 1). More precisely, 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 (see Figure 2). The heterogeneity of strain distribution depends on the electrode potential and reaches as large as 0.08 % at oxygen reduction reaction-relevant potential. These results provide dynamic structural insights to better simulate and design efficient nanocatalysts for energy storage and conversion applications.

Published
2022

16. S4 - Cristallographie in situ, operando

Author

Atlan, Clément, Martens, Isaac, Dupraz, Maxime, Eymery, J., Maillard, Frédéric, Chatelier, Corentin, Richard, Marie‐ingrid, 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), 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), and European Project: 818823,CARINE

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

International audience; Les nanoparticules de Pt et leurs alliages sont fréquemment utilisés comme catalyseurs dans un grand nombre de processus (électro)-chimiques. Comprendre comment la structure de ces catalyseurs évolue en cours de réaction est un défi majeur pour optimiser leur performance et activité catalytique. Grâce à la haute cohérence des rayons X obtenus en milieu synchrotron et de par leur nature non destructive, l'imagerie par diffraction cohérente des rayons X permet de cartographier in situ, operando (en cours d'opération) et en 3D la réponse structurelle de nanoparticules uniques (déplacement, contraintes, forme, défauts etc.). L'évolution du champ de déplacement est ainsi directement mesurable en cours de réaction électrochimique (i.e., en faisant varier le potentiel d'électrode) ou encore dans des milieux différents (pour différentes électrolytes). Ici, nous présentons l'utilisation de cette technique qui permet de suivre l'évolution en 3D de la déformation d'une nanoparticule de Pt (cf. Figure) durant une réaction d'oxydation (Oxygen Evolution Reaction). Cela permet d'élucider les effets de déformation entre différents types de facettes, arêtes et coins ; ce qui ne pouvait être obtenu avec des surfaces modèles monocristallines.

Published
2021

17. Evolution de la déformation d'une nanoparticle de Pt durant une réaction électrochimique

Author

Atlan, Clément, Martens, Isaac, Dupraz, Maxime, Eymery, J., Maillard, Frédéric, Chatelier, Corentin, Richard, Marie‐ingrid, Maillard, Frédéric, and Coherent diffrAction foR a look Inside Nanostructures towards atomic rEsolution: catalysis and interface - CARINE - 818823 - INCOMING

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

Les nanoparticules de Pt et leurs alliages sont fréquemment utilisés comme catalyseurs dans un grand nombre de processus (électro)-chimiques. Comprendre comment la structure de ces catalyseurs évolue en cours de réaction est un défi majeur pour optimiser leur performance et activité catalytique. Grâce à la haute cohérence des rayons X obtenus en milieu synchrotron et de par leur nature non destructive, l'imagerie par diffraction cohérente des rayons X permet de cartographier in situ, operando (en cours d'opération) et en 3D la réponse structurelle de nanoparticules uniques (déplacement, contraintes, forme, défauts etc.). L'évolution du champ de déplacement est ainsi directement mesurable en cours de réaction électrochimique (i.e., en faisant varier le potentiel d'électrode) ou encore dans des milieux différents (pour différentes électrolytes). Ici, nous présentons l'utilisation de cette technique qui permet de suivre l'évolution en 3D de la déformation d'une nanoparticule de Pt (cf. Figure) durant une réaction d'oxydation (Oxygen Evolution Reaction). Cela permet d'élucider les effets de déformation entre différents types de facettes, arêtes et coins ; ce qui ne pouvait être obtenu avec des surfaces modèles monocristallines.

Published
2021

18. Hétérogénéité des déformations induites par le potentiel d'électrode mise en lumière par diffraction cohérente de Bragg in situ

Author

Atlan, Clément, Gao, Lu, Martens, Isaac, Dupraz, Maxime, Chatelier, Corentin, Viola, Arnaud, Li, Ni, Leake, Steven, Eymery, J., Maillard, Frédéric, Richard, Marie‐ingrid, Maillard, Frédéric, Coherent diffrAction foR a look Inside Nanostructures towards atomic rEsolution: catalysis and interface - CARINE - 818823 - INCOMING, 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), 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), Eindhoven University of Technology [Eindhoven] (TU/e), and European Project: 818823,CARINE

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

International audience

Published
2021

19. Unveiling Core–Shell Structure Formation in a Ni3Fe Nanoparticle with In Situ Multi-Bragg Coherent Diffraction Imaging

Author

Chatelier, Corentin, Atlan, Clément, Dupraz, Maxime, Leake, Steven, Li, Ni, Schülli, Tobias U., Levi, Mor, Rabkin, Eugen, Favre, Luc, Labat, Stéphane, Eymery, Joël, and Richard, Marie-Ingrid

Abstract

Solid-state reactions play a key role in materials science. The evolution of the structure of a single 350 nm Ni3Fe nanoparticle, i.e., its morphology (facets) as well as its deformation field, has been followed by applying multireflection Bragg coherent diffraction imaging. Through this approach, we unveiled a demixing process that occurs at high temperatures (600 °C) under an Ar atmosphere. This process leads to the gradual emergence of a highly strained core–shell structure, distinguished by two distinct lattice parameters with a difference of 0.4%. Concurrently, this transformation causes the facets to vanish, ultimately yielding a rounded core–shell nanoparticle. This final structure comprises a Ni3Fe core surrounded by a 40 nm Ni-rich outer shell due to preferential iron oxidation. Providing in situ 3D imaging of the lattice parameters at the nanometer scale while varying the temperature, this study─with the support of atomistic simulations─not only showcases the power of in situ multireflection BCDI but also provides valuable insights into the mechanisms at work during a solid-state reaction characterized by a core–shell transition.

Published
2024
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20. Capturing Catalyst Strain Dynamics during OperandoCO Oxidation

Author

Grimes, Michael, Atlan, Clément, Chatelier, Corentin, Bellec, Ewen, Olson, Kyle, Simonne, David, Levi, Mor, Schülli, Tobias U., Leake, Steven J., Rabkin, Eugen, Eymery, Joël, and Richard, Marie-Ingrid

Abstract

Understanding the strain dynamic behavior of catalysts is crucial for the development of cost-effective, efficient, stable, and long-lasting catalysts. Using time-resolved Bragg coherent diffraction imaging at the fourth generation Extremely Brilliant Source of the European Synchrotron (ESRF-EBS), we achieved subsecond time resolution during operandochemical reactions. Upon investigation of Pt nanoparticles during CO oxidation, the three-dimensional strain profile highlights significant changes in the surface and subsurface regions, where localized strain is probed along the [111] direction. Notably, a rapid increase in tensile strain was observed at the top and bottom Pt {111} facets during CO adsorption. Moreover, we detected oscillatory strain changes (6.4 s period) linked to CO adsorption during oxidation, where a time resolution of 0.25 s was achieved. This approach allows for the study of adsorption dynamics of catalytic nanomaterials at the single-particle level under operandoconditions, which provides insight into nanoscale catalytic mechanisms.

Published
2024
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21. Unveiling Core-Shell Structure Formation in a Ni 3 Fe Nanoparticle with In Situ Multi-Bragg Coherent Diffraction Imaging.

Author

Chatelier C, Atlan C, Dupraz M, Leake S, Li N, Schülli TU, Levi M, Rabkin E, Favre L, Labat S, Eymery J, and Richard MI

Abstract

Solid-state reactions play a key role in materials science. The evolution of the structure of a single 350 nm Ni 3 Fe nanoparticle, i.e. , its morphology (facets) as well as its deformation field, has been followed by applying multireflection Bragg coherent diffraction imaging. Through this approach, we unveiled a demixing process that occurs at high temperatures (600 °C) under an Ar atmosphere. This process leads to the gradual emergence of a highly strained core-shell structure, distinguished by two distinct lattice parameters with a difference of 0.4%. Concurrently, this transformation causes the facets to vanish, ultimately yielding a rounded core-shell nanoparticle. This final structure comprises a Ni 3 Fe core surrounded by a 40 nm Ni-rich outer shell due to preferential iron oxidation. Providing in situ 3D imaging of the lattice parameters at the nanometer scale while varying the temperature, this study─with the support of atomistic simulations─not only showcases the power of in situ multireflection BCDI but also provides valuable insights into the mechanisms at work during a solid-state reaction characterized by a core-shell transition.

Published
2024
Full Text
View/download PDF

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