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212 results on '"Thierry Epicier"'

1. Protocrystallinity of Monodispersed Ultra-Small Templated Mesoporous Silica Nanoparticles

Author

Laurent Bonneviot, Belén Albela, Feifei Gao, Pascal Perriat, Thierry Epicier, and Mohamad El Eter

Subjects
mesoporous silica, nanoparticles, crystallinity, synthesis, monodispersion, porosity, Chemistry, QD1-999
Abstract

Monodisperse and semi-faceted ultra-small templated mesoporous silica nanoparticles (US-MSNs) of 20–25 nm were synthesized using short-time hydrolysis of tetraethoxysilane (TEOS) at room temperature, followed by a dilution for nucleation quenching. According to dynamic light scattering (DLS), a two-step pH adjustment was necessary for growth termination and colloidal stabilization. The pore size was controlled by cetyltrimethylammonium bromide (CTAB), and a tiny amount of neutral surfactant F127 was added to minimize the coalescence between US-MSNs and to favor the transition towards internal ordering. Flocculation eventually occurred, allowing us to harvest a powder by centrifugation (~60% silica yield after one month). Scanning transmission electron microscopy (STEM) and 3D high-resolution transmission electron microscopy (3D HR-TEM) images revealed that the US-MSNs are partially ordered. The 2D FT transform images provide evidence for the coexistence of four-, five-, and sixfold patterns characterizing an “on-the-edge” crystallization step between amorphous raspberry and hexagonal pore array morphologies, typical of a protocrystalline state. Calcination preserved this state and yielded a powder characterized by packing, developing a hierarchical porosity centered at 3.9 ± 0.2 (internal pores) and 68 ± 7 nm (packing voids) of high potential for support for separation and catalysis.

Published
2024
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2. Deep learning detection of nanoparticles and multiple object tracking of their dynamic evolution during in situ ETEM studies

Author

Khuram Faraz, Thomas Grenier, Christophe Ducottet, and Thierry Epicier

Subjects
Medicine, Science
Abstract

Abstract In situ transmission electron microscopy (TEM) studies of dynamic events produce large quantities of data especially under the form of images. In the important case of heterogeneous catalysis, environmental TEM (ETEM) under gas and temperature allows to follow a large population of supported nanoparticles (NPs) evolving under reactive conditions. Interpreting properly large image sequences gives precious information on the catalytic properties of the active phase by identifying causes for its deactivation. To perform a quantitative, objective and robust treatment, we propose an automatic procedure to track nanoparticles observed in Scanning ETEM (STEM in ETEM). Our approach involves deep learning and computer vision developments in multiple object tracking. At first, a registration step corrects the image displacements and misalignment inherent to the in situ acquisition. Then, a deep learning approach detects the nanoparticles on all frames of video sequences. Finally, an iterative tracking algorithm reconstructs their trajectories. This treatment allows to deduce quantitative and statistical features about their evolution or motion, such as a Brownian behavior and merging or crossing events. We treat the case of in situ calcination of palladium (oxide) / delta-alumina, where the present approach allows a discussion of operating processes such as Ostwald ripening or NP aggregative coalescence.

Published
2022
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3. MEASUREMENTS OF STRAIN FIELDS DUE TO NANOSCALE PRECIPITATES USING THE PHASE IMAGE METHOD

Author

Patricia Donnadieu, Kenji Matsuda, Thierry Epicier, and Joel Douin

Subjects
displacement field, HREM, phase image, Medicine (General), R5-920, Mathematics, QA1-939
Abstract

Owing the phase image method (Hytch, 1998), strain fields can be derived from HREM images. The method is here applied to the nanoscale precipitates responsible for hardening in Aluminum alloys. Since the method is a very sensitive one, we have examined the impact of several aspects of the image quality (noise, fluctuations, distortion). The strain field information derived from the HREM image analysis is further introduced in a simulation of the dislocation motion in the matrix.

Published
2011
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6. Morphology and topology assessment in hierarchical zeolite materials: adsorption hysteresis, scanning behavior, and domain theory

Author

Céline Pagis, David Laprune, Lucian Roiban, Thierry Epicier, Cécile Daniel, Alain Tuel, David Farrusseng, and Benoit Coasne

Subjects
Inorganic Chemistry
Abstract

The multiscale porosity of hierarchical zeolite materials is analyzed through advanced adsorption-based characterization in conjunction with additional techniques including electron tomography.

Published
2022
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7. Model catalysts synthesized by the di-block copolymer inverse micelle method: insights on nanoparticle formation and network stability within the environmental TEM. - VIRTUAL

Author

Cadete Santos Aires, F. J., Ehret, E., Bruno Domenichini, Burel, L., Thierry Epicier, IRCELYON-Méthodologies En Microscopie Environnementale (MEME), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRCELYON-Microscopie (MICROSCOPIE), and IRCELYON, ProductionsScientifiques

Subjects
[CHIM.CATA] Chemical Sciences/Catalysis, [SDE.ES] Environmental Sciences/Environmental and Society, [CHIM.CATA]Chemical Sciences/Catalysis, [SDE.ES]Environmental Sciences/Environmental and Society
Abstract

MICROSCOPIE+MEME+FCA:EEH:LBU:TEP; International audience; The di-block copolymer inverse micelle method, where an amphiphilic di-block copolymer dissolved in toluene creates a system of inverse micelles, is a rather simple method to obtain well controlled supported metallic nanoparticles once the micelle core is charged with metallic salts. Supported metallic catalysts can be obtained in this way on both flat (model catalysts) and powder (realistic catalysts) supports [1]. Our main interest deals with applications of bimetallic catalyst systems that we investigate from extended catalytic surfaces [2] to realistic catalysts [3]; the idea being to isolate and understand the role of important physico-chemical parameters on the catalytic behaviour of these systems in the shape of model catalytic surfaces and try to extrapolate them to realistic catalysts. This is very important for the controlled design of catalysts with specific properties. In this way we can, not only spend less active material (often rare and expensive), but also avoid unnecessary poisoning while keeping high activity (stability) and finely tune the selectivity to avoid deleterious unwanted products; these are important points to be able to achieve environmentally friendly and sustainable catalytic processes. Self-organized nanoparticles on flat surfaces is an intermediate configuration between extended catalytic surfaces and realistic catalysts and a necessary step to better extrapolate results between model and realistic systems. We have thus extended the di-block copolymer method to the synthesis of bimetallic catalysts [4]. In our presentation we will deal with a PdAu system, obtained from a PS-b-P2VP copolymer micellar solution that we transfer by spin-coating to a surface of a SiNx eletron-transparent films on dedicated microchips than are heated in Wildfire sample holder (DENS Solutions) within an objective lens aberration-corrected environmental TEM (Titan ETEM G2 80-300 kV from ThermoFisher Scientific) so that we can study in situ the behaviour of such a system in variable temperature and gas pressure. We observed the formation of the individual particles from the seeds within the core of the micelles in the presence of oxygen in variable temperature; sintering of the seeds within the micelle cores starts at 350°C and is completed at 500°C, temperatures that correspond, respectively, to the onset of the copolymer decomposition and to its quasi-completed decomposition [5]. We also observed that the network of nanoparticles is stable under oxygen up to 900°C and that, above this temperature, the network is modified only by the decomposition of the nanoparticles (when we approach their melting point).The authors acknowledge the French Microscopy and Atom probe network (METSA) and the Consortium Lyon – St-Etienne de Microscopie (CLYM) for supporting this work.References:[1] B. Roldan Cuenya, Accounts of Chemical Research 46 (2013) 1682.[2] MC Saint-Lager et al., ACS Catalysis 9 (2019) 4448.[2] B. Pongthawornsakun et al., Applied Catalysis A: General 549 (2018) 1.[4] E. Ehret et al., Nanoscale 7 (2015) 13239.[5] T. Orhan Lekesiz et al., Journal of Analytical and Applied Pyrolysis 106 (2014) 81.

Published
2021

8. Exploiting the dynamic properties of Pt on ceria for low-temperature CO oxidation

Author

Stéphane Loridant, Philippe Vernoux, G. Ferre, Christophe Geantet, Mimoun Aouine, Florian Maurer, Laurence Burel, Thierry Epicier, Jan-Dierk Grunwaldt, Spyridon Ntais, Françoise Bosselet, F.J. Cadete Santos Aires, Maria Casapu, IRCELYON-Catalytic and Atmospheric Reactivity for the Environment (CARE), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRCELYON-Microscopie (MICROSCOPIE), IRCELYON-Diffraction des rayons X (RX), IRCELYON-Catalyse Hétérogène pour la Transition Energétique (CATREN), and IRCELYON-Méthodologies En Microscopie Environnementale (MEME)

Subjects
Materials science, Diesel exhaust, chemistry.chemical_element, [CHIM.CATA]Chemical Sciences/Catalysis, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, [SDE.ES]Environmental Sciences/Environmental and Society, 01 natural sciences, Oxygen, Catalysis, 0104 chemical sciences, Propene, chemistry.chemical_compound, X-ray photoelectron spectroscopy, chemistry, Chemical engineering, Monolayer, Scanning transmission electron microscopy, 0210 nano-technology, Dispersion (chemistry)
Abstract

MICROSCOPIE:RX+CARE:ECI2D:MEME+GFE:MAO:FBS:LBU:CGE:TEP:SLO:PVE; International audience; This study explores the dynamic properties of Pt/CeO2 catalysts to develop active catalytic converters for diesel exhausts. It is now well established that single Pt atoms can be stabilised on ceria surface defects under oxidising conditions. However, their catalytic activity is rather poor. A reducing treatment is required to build more active Pt nanoparticles. A Pt/CeO2 catalyst, containing mainly atomically dispersed Pt species, was exposed to reduction steps either at 250 or 500 °C to build Pt nanoparticles. Their redispersion after oxidising treatments in oxygen at three temperatures (room temperature, 250 °C and 500 °C) as well as in a simulated diesel exhaust gas was deeply investigated using different characterisation techniques such as high angle annular dark field scanning transmission electron microscopy, in situ Raman spectroscopy, in situ X-ray diffraction, X-ray photoelectron spectroscopy and H2-temperature-programmed reduction. The arrangement of close packed Pt clusters is a permanent event at low temperatures (

Published
2020
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10. Arrays of bimetallic nanoparticles obtained by the block copolymer inverse micelle method

Author

Ehret, E., Thierry Epicier, Beyou, E., Bruno Domenichini, Mamontov, G. V., Bugrova, T. A., Aouine, M., Burel, L., Cadete Santos Aires, F. J., IRCELYON-Méthodologies En Microscopie Environnementale (MEME), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRCELYON-Microscopie (MICROSCOPIE), and IRCELYON, ProductionsScientifiques

Subjects
[CHIM.CATA] Chemical Sciences/Catalysis, [SDE.ES] Environmental Sciences/Environmental and Society, [CHIM.CATA]Chemical Sciences/Catalysis, [SDE.ES]Environmental Sciences/Environmental and Society
Abstract

MICROSCOPIE+MEME+EEH:TEP:MAO:LBU:FCA; International audience; We used self-assembled block copolymer templates to generate arrays of bimetallic nanoparticles. In this approach, a block copolymer consisting of hydrophilic and hydrophobic blocks is dissolved in a selective solvent such as toluene in order to obtain inverse micelles. The core of such inverse micelles can then be functionalized with metal precursors ligated by complexation or protonisation to the inner polymer block. The reverse micelles can then be transferred from the solution to the substrate by using, for instance, standard spin or dip coating techniques. The obtained layer exhibits a rather high degree of hexagonal order, reflecting the packing of spherical micelles.We present results on the formation of arrays of both PdAg and PdAu nanoparticles obtained by this method. For the latter a specific study on the stability of the array at high temperatures under oxygen pressure was performed within an objective-lens aberration-corrected environmental transmission electron microscope (Titan ETEM G2 80-300 kV from ThermoFisher Scientific).

Published
2021

12. In-situ annealing transmission electron microscopy of plasmonic thin films composed of bimetallic Au-Ag nanoparticles dispersed in a TiO2 matrix

Author

Joel Nuno Pinto Borges, Thierry Epicier, Eduardo Alves, Diogo Emanuel Carvalho Costa, Marcos Rodrigues, N.P. Barradas, Mimoun Aouine, Philippe Steyer, Lucian Roiban, Filipe Vaz, IRCELYON-Microscopie (MICROSCOPIE), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and IRCELYON-Méthodologies En Microscopie Environnementale (MEME)

Subjects
Materials science, Annealing (metallurgy), Nanoparticle, 02 engineering and technology, Thermal treatment, [CHIM.CATA]Chemical Sciences/Catalysis, Sputter deposition, 010402 general chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 01 natural sciences, [SDE.ES]Environmental Sciences/Environmental and Society, 0104 chemical sciences, Surfaces, Coatings and Films, Chemical engineering, Transmission electron microscopy, Thin film, 0210 nano-technology, Instrumentation, Bimetallic strip, Localized surface plasmon
Abstract

This work was focused on the characterization of plasmonic thin films composed of Au–Ag nanoparticles dispersed in a TiO2 dielectric matrix in comparison with the monometallic Au/TiO2 plasmonic system. The thin films were prepared by reactive DC magnetron sputtering, followed by thermal annealing at different temperatures to promote nanoparticles' growth. Thermal treatment from 400 °C induced the appearance of Localized Surface Plasmon Resonances (LSPRs) in both Au/TiO2 and Au–Ag/TiO2 thin films. The latter showed a wider LSPR response, due to the broader size distribution of nanoparticles (analyzed by transmission electron microscopy, TEM). Further nanometer-scale chemical analysis allowed to confirm the presence of Au–Ag bimetallic nanoparticles. To thoroughly study the influence of the annealing treatment on the nanoparticles' growth, Au–Ag/TiO2 was also deposited on heating TEM nano-chips for in-situ annealing experiments. The formation of silver aggregates was found in the sample as-deposited, with these precipitates dissolving in the matrix with the increase of annealing temperature up to 200 °C. For higher temperatures, nanoparticles’ real-time growth was observed, together with the crystallization of the TiO2 matrix above 550 °C. Besides, the plasmonic Au–Ag/TiO2 thin films revealed LSPR sensitivity when in contact with different dielectric media, highlighting their potential as refractive index sensors.

Published
2021
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13. Thermal behaviour of caesium implanted in UO$_2$ : A comparative study with the xenon behaviour

Author

O. Dieste, Thierry Epicier, B. Marchand, R. Dubourg, C. Panetier, Clotilde Gaillard, Nathalie Moncoffre, Y. Pipon, D. Mangin, R. Ducher, Thierry Wiss, Louis Raimbault, Institut de Physique des 2 Infinis de Lyon (IP2I Lyon), Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon, Institut Jean Lamour (IJL), Université de Lorraine (UL)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA), and École des Mines de Paris

Subjects
[PHYS]Physics [physics], Nuclear and High Energy Physics, Materials science, Growth kinetics, Analytical chemistry, chemistry.chemical_element, 02 engineering and technology, UO2, 021001 nanoscience & nanotechnology, UO 2, 01 natural sciences, 010305 fluids & plasmas, bubbles, Xenon, Nuclear Energy and Engineering, chemistry, Xe, Caesium, 0103 physical sciences, Thermal, TEM, General Materials Science, 0210 nano-technology, Cs, SIMS
Abstract

International audience; • SIMS and TEM techniques were combined to compare the thermal behaviour of Cs and Xe in UO 2 . • Both elements form bubbles with different growth kinetics. • At 1600 °C, caesium is found to be highly mobile in the UO 2 matrix while Xe distribution does not evolve.

Published
2021
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14. Correlative STEM-HAADF and STEM-EDX tomography for the 3D morphological and chemical analysis of semiconductor devices

Author

Zineb Saghi, Martin Jacob, Julien Sorel, Thierry Epicier, Adeline Grenier, Frédéric Mazen, Rafael Bortolin Pinhiero, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), IRCELYON-Méthodologies En Microscopie Environnementale (MEME), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
010302 applied physics, Correlative, Materials science, 02 engineering and technology, Semiconductor device, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 01 natural sciences, Electronic, Optical and Magnetic Materials, [SPI.MAT]Engineering Sciences [physics]/Materials, Electron tomography, 0103 physical sciences, Materials Chemistry, Tomography, Electrical and Electronic Engineering, 0210 nano-technology, Biomedical engineering
Abstract

3D analysis of an arsenic-doped silicon fin sample is performed in a transmission electron microscope (TEM). High angle annular dark-field scanning TEM (STEM-HAADF) and energy-dispersive x-ray spectroscopy (STEM-EDX) modes are used simultaneously to extract 3D complementary multi-resolution information about the sample. The small pixel size and angular step chosen for the STEM-HAADF acquisition yield reliable information about the sidewall roughness and the arsenic clusters’ average volume. The chemical sensitivity of STEM-EDX tomography gives insights into the 3D conformality of the arsenic implantation and its depth distribution. Non-negative matrix factorization method is employed to identify the chemical phases present in the sample automatically. A total variation minimization algorithm, implemented in 3D, produces high-quality volumes from heavily undersampled datasets. The extension of this correlative approach to electron energy-loss spectroscopy STEM tomography and atom probe tomography is also discussed.

Published
2021
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15. Self-Organized Bimetallic Catalysts Obtained from Di-Block Copolymer Micellar Solutions: Nanoparticle Formation and Network Stability at High Temperature under Gas Pressure within the Environmental TEM

Author

Ehret, E., Cadete Santos Aires, F. J., Bruno Domenichini, Burel, L., Thierry Epicier, IRCELYON, ProductionsScientifiques, IRCELYON-Méthodologies En Microscopie Environnementale (MEME), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and IRCELYON-Microscopie (MICROSCOPIE)

Subjects
[CHIM.CATA] Chemical Sciences/Catalysis, [CHIM.CATA]Chemical Sciences/Catalysis, [SDE.ES] Environmental Sciences/Environmental and Society, [SDE.ES]Environmental Sciences/Environmental and Society
Abstract

MICROSCOPIE+MEME+EEH:FCA:LBU:TEP; International audience; Systems of self-organized nanoparticles (NPs) are useful in many domains such as, for instance, optics, nanostructure growth and, the domain of most interest in our case, catalysis. It is indeed a way to control the classic characteristics of catalysts (size, dispersion, chemical phase, …) and add a new tunable parameter, often poorly controlled, which is the long-distance ordering and, thus, the inter-nanoparticle distance. Well-controlled physicochemical properties of the catalysts lead to better correlation between these properties, their possible evolution, and their catalytic performance (activity, selectivity, stability). Among self-assembly techniques, the use of di-block copolymer method, where an amphiphilic di-block copolymer dissolved in toluene yields a system of inverse micelles, is a rather simple method to obtain well controlled supported NPs which can be used as supported metallic catalysts on both flat (model catalysts) and powder (realistic catalysts) supports [1]. After formation of the micellar solution, we can indeed charge the core with metal salts that can then be deposited on flat surfaces by dip or spin coating for instance. Our main interest deals with applications of bimetallic catalysts that we study in the form of both realistic catalysts [2] and extended catalytic surfaces [3]; self-organized NPs on flat surfaces is an intermediate configuration between these two approaches which is useful to better extrapolate results between model and realistic systems. With this in mind we have extended the di-block copolymer method to the synthesis of bimetallic catalysts [4]. For these systems composed of metals with different characteristics, several questions remain unanswered such as the evolution of the pre-formed bimetallic seeds (Fig. 1b-d) with temperature, the temperature formation of unique NPs at the micellar core or the stability of the network of bimetallic NPs (Fig. 1a) at high temperature in presence of reactive gases.An objective lens aberration-corrected Environmental TEM (Titan ETEM G2 from FEI/ThermoFisher Scientific), operated at 300kV and capable of gas pressure up to 20 mbar, is a well-adapted tool to study those phenomena. An Au-rich AuPd core-metallized PS-b-P2VP micellar solution was synthesized and deposited by spin-coating on dedicated heating microchips containing a silicon nitride electron transparent (discrete) film capable of reaching temperatures up to 1300°C within a WildFire support holder (DENS solutions). Special care was taken to minimize/prevent any influence of the electron beam on the observed events. In order to observe both the formation of the individual NPs, together with the elimination of the copolymer, and the high-temperature stability of the network we have worked under oxygen pressure (up to 2 mbar). We observed that the seeds within the micellar cores (Fig. 2a-left) begin to sinter around 350°C (Fig. 2a-center) which is consistent with the temperature onset at which the copolymer (associated to a metal) begins to decompose [5]; unique NPs are formed around 500°C (Fig. 2a-right), when the copolymer is almost completely gasified [5]. The network is remarkably stable up to 900°C (Fig. 2b); finally, around 1000°C, close to the melting temperature of Au (1064°C), the NPs begin to decompose (Fig. 2b). At 1100° C, unique Au-rich NPs (Fig. 3a) begin to shrink and yield smaller satellite NPs (Fig. 3b); then the facetted NP (Fig. 3c) becomes spherical (Fig. 3d) and finally disappears to leave only the satellite NPs that grow on the surface (Fig. 3e). The volume ratio between the satellite NPs and the initial Au-rich NP indicate that only the Au within the NP has disappeared and that the remaining satellite NPs are pure Pd. The stability of the network seems to depend only on the intrinsic properties of the chosen metals [6].References:[1] B Roldan Cuenya, Accounts of Chemical Research 46 (2013) 1682.[2] B Pongthawornsakun et al, Applied Catalysis A: General 549 (2018) 1.[3] MC Saint-Lager et al, ACS Catalysis 9 (2019) 4448.[4] E Ehret et al, Nanoscale 7 (2015) 13239.[5] T Orhan Lekesiz et al, Journal of Analytical and Applied Pyrolysis 106 (2014) 81.[6] The authors acknowledge the French Microscopy and Atom probe network (METSA) and the Consortium Lyon – St-Etienne de Microscopie (CLYM) for supporting this work.

Published
2021

16. Interplay between local structure and magnetic properties of graded exchange-coupled Co@FePt nanocomposite films

Author

Fabrice Wilhelm, Andrei Rogalev, Véronique Dupuis, Matthieu Bugnet, Charles Paleo, Olivier Proux, O. Boisron, Isabelle Kieffer, Damien Le Roy, Thierry Epicier, Nanostructures magnétiques (MAGNETIQUES), Institut Lumière Matière [Villeurbanne] (ILM), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), European Synchrotron Radiation Facility (ESRF), Observatoire des Sciences de l'Univers de Grenoble (OSUG ), Institut national des sciences de l'Univers (INSU - CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Université Grenoble Alpes (UGA), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), ANR-16-CE09-0019,SHAMAN,Nanocomposites magnétique de type doux-dans-dur(2016), Institut National des Sciences Appliquées de Lyon (INSA Lyon), Institut National des Sciences Appliquées (INSA)-Université de Lyon, and Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS]Physics [physics], Nanocomposite, Materials science, Physics::Optics, Nanotechnology, 02 engineering and technology, 021001 nanoscience & nanotechnology, Microstructure, 01 natural sciences, Evaporation (deposition), Condensed Matter::Materials Science, Nanolithography, Magnet, 0103 physical sciences, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Cluster (physics), Nanometre, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], 010306 general physics, 0210 nano-technology, Absorption (electromagnetic radiation)
Abstract

International audience; Magnetically-hard nanocomposites are attractive materials for integration in various microsys-tems and for building next generation permanent magnets. However, exploiting their full potential requires to control their microstructure at the nanometre scale. Studying these materials in model systems synthesised by nanofabrication routes gives interesting insights about the interplay between the microstructure and the magnetic performances. Here, by using a combination of mass-selected low energy cluster beam deposition and electron-beam evaporation, we have prepared nanocomposite films where Co nanoinclusions are integrated in a hard magnetic FePt matrix. Local atomic structures and element selective magnetic properties of such nanocomposites have been thoroughly investigated using polarisation dependent hard X-ray absorption spectroscopies. These results demonstrate that magnetically soft inclusions are stabilised at room temperature, emphasising the role of the interdiffusion in the preparation of nanocomposites.

Published
2020
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17. Accurate post-mortem alignment for Focused Ion Beam and Scanning Electron Microscopy (FIB-SEM) tomography

Author

Thierry Epicier, B. Van de Moortèle, Hui Yuan, IRCELYON-Microscopie (MICROSCOPIE), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Epicier, Thierry, and IRCELYON-Méthodologies En Microscopie Environnementale (MEME)

Subjects
Image Series, drifts, Materials science, [SPI] Engineering Sciences [physics], Scanning electron microscope, 02 engineering and technology, 01 natural sciences, Focused ion beam, post-mortem alignment, [SPI]Engineering Sciences [physics], Optics, 0103 physical sciences, Fib sem tomography, FIB-SEM tomography, Instrumentation, 010302 applied physics, Cross-correlation, business.industry, reference markers, [CHIM.CATA]Chemical Sciences/Catalysis, surface topography, 021001 nanoscience & nanotechnology, Microstructure, [SDE.ES]Environmental Sciences/Environmental and Society, Sample (graphics), Atomic and Molecular Physics, and Optics, Electronic, Optical and Magnetic Materials, crosscorrelation, Tomography, 0210 nano-technology, business
Abstract

Drifts in the three directions (X, Y, Z) during the FIB-SEM slice-and-view tomography is an important issue in 3D-FIB experiments which may induce significant inaccuracies in the subsequent volume reconstruction and further quantification of morphological volume parameters of the sample microstructure. Cross-correlation is frequently applied directly to the cross-section image series for aligning FIB sliced images. This solution is hazardous and can be flawed as it has been easily demonstrated by a dedicated test experiment. As a result, a novel aligning procedure based on the quantification of the topography of the sample surface has been developed. This new approach will be compared to the common cross-correlation methods, as well as another approach consisting in using an artificial reference marker fabricated during the FIB procedure. All these methods will then be discussed in terms of accuracy and liability.

Published
2020
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18. Electron Tomography of Plasmonic Au Nanoparticles Dispersed in a TiO2 Dielectric Matrix

Author

Nicolas Martin, Filipe Vaz, Siddardha Koneti, Lucian Roiban, Thierry Epicier, Joel Nuno Pinto Borges, Marcos Rodrigues, Philippe Steyer, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Departamento de Física [Minho] (DFUM), Universidade do Minho, Franche-Comté Électronique Mécanique, Thermique et Optique - Sciences et Technologies (UMR 6174) (FEMTO-ST), Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS), and ANR-05-PADD-0003,TRANS,Transformations de l'élevage et dynamiques des espaces(2005)

Subjects
Materials science, Ciências Naturais::Ciências Físicas, Thin films, Ciências Físicas [Ciências Naturais], Nanoparticle, TiO matrix 2, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Reactive magnetron sputtering, [SPI.MAT]Engineering Sciences [physics]/Materials, law.invention, law, Sputtering, STEM (scanning transmission electron microscopy), General Materials Science, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, Thin film, Surface plasmon resonance, Plasmon, [SPI.ACOU]Engineering Sciences [physics]/Acoustics [physics.class-ph], Science & Technology, business.industry, Localized surface plasmon resonance, 021001 nanoscience & nanotechnology, TiO2 matrix, 0104 chemical sciences, 3. Good health, Electron tomography, Transmission electron microscopy, Optoelectronics, Electron microscope, Au nanoparticles, 0210 nano-technology, business
Abstract

Plasmonic Au nanoparticles (AuNPs) embedded into a TiO2 dielectric matrix were analyzed by combining two-dimensional and three-dimensional electron microscopy techniques. The preparation method was reactive magnetron sputtering, followed by thermal annealing treatments at 400 and 600 degrees C. The goal was to assess the nanostructural characteristics and correlate them with the optical properties of the AuNPs, particularly the localized surface plasmon resonance (LSPR) behavior. High-angle annular dark field scanning transmission electron microscopy results showed the presence of small-sized AuNPs (quantum size regime) in the as-deposited Au-TiO2 film, resulting in a negligible LSPR response. The in-vacuum thermal annealing at 400 degrees C induced the formation of intermediate-sized nanoparticles (NPs), in the range of 10-40 nm, which led to the appearance of a well-defined LSPR band, positioned at 636 nm. Electron tomography revealed that most of the NPs are small-sized and are embedded into the TiO2 matrix, whereas the larger NPs are located at the surface. Annealing at 600 degrees C promotes a bimodal size distribution with intermediate-sized NPs embedded in the matrix and big sized NPs, up to 100 nm, appearing at the surface. The latter are responsible for a broadening and a redshift, to 645 nm, in the LSPR band because of increase of scattering-to-absorption ratio. Beyond differentiating and quantifying the surface and embedded NPs, electron tomography also provided the identification of "hot-spots". The presence of NPs at the surface, individual or in dimers, permits adsorption sites for LSPR sensing and for surface-enhanced spectroscopies, such as surface enhanced Raman scattering., The authors thank the METSA network (FR3507 CNRS) for the financial support for this work, the Clym consortium for granting access to the Jeol 2010F and TITAN 80-300 keV ETEM. S.K. thanks the French Ministry of Higher Education and Research for the financial support during his PhD which was also supported by the LABEX iMUST (ANR-10-LABX-0064) of Universite de Lyon, within the program "Investissements d'Avenir" (ANR-11-IDEX-0007) operated by the French National Research Agency (ANR). This research was partly supported by the 3Dclean ANR-15-CE09-0009 project granted by the ANR. This research was also sponsored by the Portuguese Foundation for Science and Technology (FCT) in the framework of the Strategic Funding UID/FIS/04650/2013 and FCT Project 9471-RIDTI, co-funded by FEDER and with reference PTDC/FIS-NAN/1154/2014. J.B. acknowledges FCT for his Postdoc Grant (SFRH/BPD/117010/2016) and M.S.R. acknowledges FCT for his PhD Grant (SFRH/BD/118684/2016)., info:eu-repo/semantics/publishedVersion

Published
2018
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19. A Machine Learning pipeline to track the dynamics of a population of nanoparticles during in situ Environmental Transmission Electron Microscopy in gases

Author

Thierry Epicier, Khuram Faraz, Christophe Ducottet, and Thomas Grenier

Subjects
In situ, education.field_of_study, Materials science, business.industry, Transmission electron microscopy, Track (disk drive), Pipeline (computing), Population, Nanoparticle, Aerospace engineering, business, education, Instrumentation
Published
2021
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20. Direct Visualization and Control of Atomic Mobility at {100} Surfaces of Ceria in the Environmental Transmission Electron Microscope

Author

Thierry Epicier, Matthieu Bugnet, Zili Wu, Steven H. Overbury, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), and Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Nanocubes, Atoms, Cerium compounds, Catalyst support, Ultra-high vacuum, chemistry.chemical_element, High resolution transmission electron microscopy, Electrons, Bioengineering, Nanotechnology, 02 engineering and technology, 010402 general chemistry, Heterogeneous catalysis, 01 natural sciences, Catalysis, [SPI.MAT]Engineering Sciences [physics]/Materials, law.invention, law, Environmental Transmission Electron Microscope, Electron microscopy, General Materials Science, High-resolution transmission electron microscopy, Visualization, Temporal evolution, Catalysts, Catalytic mechanisms, Chemistry, Environmental transmission electron microscopy, Mechanical Engineering, General Chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Surfaces, Cerium, Carbon dioxide, Atomic mobility, facet, Electron microscope, 0210 nano-technology, Direct visualization, Environmental transmission electron microscopes
Abstract

cited By 0; International audience; Ceria is one of the world's most prominent material for applications in heterogeneous catalysis, as catalyst support or catalyst itself. Despite an exhaustive literature on the structure of reactive facets of CeO2 in line with its catalytic mechanisms, the temporal evolution of the atomic surface structure exposed to realistic redox conditions remains elusive. Here, we provide a direct visualization of the atomic mobility of cerium atoms on 100 surfaces of CeO2 nanocubes at room temperature in high vacuum, O2, and CO2 atmospheres in an environmental transmission electron microscope. Through quantification of the cationic mobility, we demonstrate the control of the surface dynamics under exposure to O2 and CO2 atmospheres, providing opportunities for a better understanding of the intimate catalytic mechanisms. © 2017 American Chemical Society.

Published
2017
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21. Tuning the Structure of Platinum Particles on Ceria In Situ for Enhancing the Catalytic Performance of Exhaust Gas Catalysts

Author

Benjamin Betz, Andreas M. Gänzler, Philippe Vernoux, Jan-Dierk Grunwaldt, Stéphane Loridant, Francisco J. Cadete Santos Aires, Rüdiger Dr. Hoyer, Maria Casapu, Thierry Epicier, Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), and Karlsruhe Inst Technol, Inst Chem Technol & Polymer Chem, Engesserstr 20, D-76131 Karlsruhe, Germany

Subjects
Materials science, 010405 organic chemistry, Inorganic chemistry, Exhaust gas, chemistry.chemical_element, 02 engineering and technology, General Chemistry, General Medicine, engineering.material, 021001 nanoscience & nanotechnology, Heterogeneous catalysis, 010402 general chemistry, 01 natural sciences, Catalysis, 0104 chemical sciences, chemistry, Transmission electron microscopy, Oxidizing agent, engineering, Noble metal, 0210 nano-technology, Dispersion (chemistry), Platinum, ComputingMilieux_MISCELLANEOUS
Abstract

A dynamic structural behavior of Pt nanoparticles on the ceria surface under reducing/oxidizing conditions was found at moderate temperatures ( H2>C3H6). This dynamic nature of Pt on ceria at such low temperatures (250–500 °C) was additionally confirmed by in situ environmental transmission electron microscopy. A general concept is proposed to adjust the noble metal dispersion (size, structure), for example, during operation of an exhaust gas catalyst.

Published
2017
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22. Fast ‘Operando ’ electron nanotomography

Author

Lucian Roiban, Alain Tuel, Thierry Epicier, S. Li, David Farrusseng, and Mimoun Aouine

Subjects
chemistry.chemical_classification, Histology, Materials science, Nanotechnology, 02 engineering and technology, Electron, Polymer, 010402 general chemistry, 021001 nanoscience & nanotechnology, Heterogeneous catalysis, 01 natural sciences, Silver nanoparticle, 0104 chemical sciences, Pathology and Forensic Medicine, law.invention, Electron tomography, chemistry, law, Transmission electron microscopy, Calcination, 0210 nano-technology, Nanoscopic scale
Abstract

Electron tomography in transmission electron microscopy provides valuable three-dimensional structural, morphological and chemical information of condensed matter at nanoscale. Current image acquisitions require at least tens of minutes, which prohibits the analysis of nano-objects evolving rapidly such as under dynamic environmental conditions. Reducing the acquisition duration to tens of seconds or less permits to follow in 3D the same object during its evolution under varying temperatures and pressures. We report Operando Electron nanotomography using image series acquired in less than 230 seconds instead of typically 15 min in the best cases so far. The in situ calcination of silica zeolites encaging silver nanoparticles, a catalytic nanosystem of potential interest for, e.g., nuclear waste treatments or selective heterogeneous catalysis, was successfully studied. Kinetic environmental Operando 3D electron microscopy becomes possible, as well as real time observation of beam sensitive samples (polymers, biological objects) without prior preparation, which reduces their contrast and reactivity.

Published
2017
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23. Spatial Distribution of the Vanadium Atomic Species in MoVTeO and MoVTeNbO Oxide Catalysts as Revealed by High-Angle Annular Dark-Field Scanning Transmission Electron Microscopy

Author

Mimoun Aouine, Jean-Marc M. Millet, Thierry Epicier, Thi Thao Nguyen, IRCELYON-Microscopie (MICROSCOPIE), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), and IRCELYON-Catalyse Hétérogène pour la Transition Energétique (CATREN)

Subjects
Materials science, Inorganic chemistry, Niobium, Analytical chemistry, Oxide, chemistry.chemical_element, Vanadium, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Catalysis, law.invention, Inorganic Chemistry, chemistry.chemical_compound, law, Scanning transmission electron microscopy, Physical and Theoretical Chemistry, Organic Chemistry, Doping, [CHIM.CATA]Chemical Sciences/Catalysis, 021001 nanoscience & nanotechnology, [SDE.ES]Environmental Sciences/Environmental and Society, Dark field microscopy, 0104 chemical sciences, chemistry, Electron microscope, 0210 nano-technology
Abstract

STEM-HAADF has been used to characterize a light alkanes mild oxidation catalysts corresponding to two different MoVTe(Nb)O M1 phases. For that purpose a semi-automatic integration routine allowing the analysis of several hundreds atomic columns with a normalization procedure has been developed to determine quantitatively the vanadium content of mixed (V, Mo) crystallographic sites with a low statistical variability. The results obtained have been compared to previous data obtained on other M1 phases with also different compositions. The comparison showed that the V distribution over the sites was not strongly influenced by the presence or not of niobium, the method of synthesis used or the nature of the Te or Sb cations in the hexagonal channels but depended mainly of the total V content of the phases. Extrapolation of low V content allowed discussing the possible location of the vanadium active sites

Published
2017
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24. Highly ductile amorphous oxide at room temperature and high strain rate

Author

Janne Kalikka, Erkki Levänen, Thierry Epicier, Lucile Joly-Pottuz, Lucian Roiban, Fabio Di Fonzo, Mikko Hokka, Douglas Stauffer, Siddardha Koneti, Megan J. Cordill, Matteo Vanazzi, Erkka Frankberg, Jaakko Akola, Francisco García Ferré, Patrice Kreiml, Thierry Douillard, Turkka Salminen, Karine Masenelli-Varlot, Bérangère Le Saint, Jouko Hintikka, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Laboratory of Photonics, University of Tampere [Finland], Tampere University of Technology [Tampere] (TUT), Bruker Nano, Physics Department, Norwegian University of Science and Technology, Norwegian University of Science and Technology [Trondheim] (NTNU), Norwegian University of Science and Technology (NTNU)-Norwegian University of Science and Technology (NTNU), Center for Nano Science and Technology@PoliMi, Instituto Italiano di Tecnologia, Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), Tampere University, Materials Science and Environmental Engineering, Physics, Research group: Nanophotonics, École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM)

Subjects
Materials science, aluminium oxide, Oxide, 02 engineering and technology, Flow stress, 01 natural sciences, chemistry.chemical_compound, [SPI]Engineering Sciences [physics], Brittleness, 0103 physical sciences, Composite material, Ductility, ComputingMilieux_MISCELLANEOUS, glass, 010302 applied physics, Multidisciplinary, 218 Environmental engineering, 221 Nanotechnology, ductile, food and beverages, 021001 nanoscience & nanotechnology, Amorphous solid, Creep, chemistry, 216 Materials engineering, Fracture (geology), room temperature, Elongation, 0210 nano-technology
Abstract

A glass that won't break Oxide glasses are important for applications ranging from smartphone screens to window panes. One familiar feature of glass is that it fractures and shatters when rapidly deformed, limiting the number of potential uses. However, Frankberg et al. found that they could deform thin films of glassy alumina (Al 2 O 3 ) with high strain rates at room temperature (see the Perspective by Wondraczek). This surprising observation is supported by simulations of the material that show that dense and flawless glassy alumina samples can deform this way. The discovery provides important insight into designing new glasses that might be more fracture resistant. Science , this issue p. 864 ; see also p. 804

Published
2019
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25. Fast electron tomography: Applications to beam sensitive samples and in situ TEM or operando environmental TEM studies

Author

Siddardha Koneti, Lucian Roiban, Florent Dalmas, Cyril Langlois, Anne-Sophie Gay, Amandine Cabiac, Thomas Grenier, Hussein Banjak, Voichiţa Maxim, Thierry Epicier, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), IFP Energies nouvelles (IFPEN), Images et Modèles, Centre de Recherche en Acquisition et Traitement de l'Image pour la Santé (CREATIS), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Imagerie Tomographique et Radiothérapie, ANR-15-CE09-0009,3DCLEAN,Tri-Dimensionnel Nano-laboratoire catalytique environnemental(2015), ANR-10-LABX-0064,Imust,Institut for Multiscale Science and Technology : from Fundamental Physics and Chemistry to Engineering in New Material and Processes and Ecotechnologies(2010), ANR-11-IDEX-0007,Avenir L.S.E.,PROJET AVENIR LYON SAINT-ETIENNE(2011), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet - Saint-Étienne (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet - Saint-Étienne (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), CCSD, Accord Elsevier, Tri-Dimensionnel Nano-laboratoire catalytique environnemental - - 3DCLEAN2015 - ANR-15-CE09-0009 - AAPG2015 - VALID, Institut for Multiscale Science and Technology : from Fundamental Physics and Chemistry to Engineering in New Material and Processes and Ecotechnologies - - Imust2010 - ANR-10-LABX-0064 - LABX - VALID, and PROJET AVENIR LYON SAINT-ETIENNE - - Avenir L.S.E.2011 - ANR-11-IDEX-0007 - IDEX - VALID

Subjects
Materials science, Polymer nanocomposite, Nanotechnology, 02 engineering and technology, [SPI.MAT] Engineering Sciences [physics]/Materials, 01 natural sciences, Nanomaterials, [SPI.MAT]Engineering Sciences [physics]/Materials, Data acquisition, Environmental Transmission Electron Microscope, Pd-Al2O3, 0103 physical sciences, Nano, General Materials Science, 010302 applied physics, Tomographic reconstruction, Pd-SiO2, Mechanical Engineering, Environmental Transmission Electron Microscopy (ETEM), 021001 nanoscience & nanotechnology, Condensed Matter Physics, Fast operando Electron Tomography, Tilt (optics), Electron tomography, Mechanics of Materials, 0210 nano-technology, Nanocatalysts
Abstract

International audience; Electron Tomography (ET) is of greatest interest in studying nano- and biological materials since it gives access to 3D morphological, chemical and physical features. Even though ET techniques have been continuously improved in the last decades, they are still limited: lengthy time scales (tens of minutes) are generally needed for the tilt series acquisition prior to the volume reconstruction step. Such long exposures to a relatively intense electron beam lead to large electron doses received by the sample. This may promote extensive irradiation damage in the case of soft materials like polymers and bio-materials when they are not protected through dedicated sample preparation methods, and any tomographic reconstruction will then be meaningless. More importantly, the time constraints drastically limit 3D investigations during dynamic in-situ experiments where the sample rapidly evolves during the acquisition.We present here developments for acquiring tilt series of projections in very short time scales, readily down to a few seconds. After an outlook of possible ways to speed up the data acquisition in the bright field imaging mode (BF-TEM), strategies for the fastest methods in ‘step-by-step’ and ‘continuous tilt’ ET will be described. Applications of these procedures are presented on various systems, including metallic Pd nanoparticles deposited on alumina, and soft materials like polymer nanocomposites and biological matter. A special reference is made to fast operando nano-tomography performed on nanomaterials during their dynamic evolution. The feasibility of fast ET is exemplified by a calcination study of Pd catalysts supported by SiO2 at 400 °C and 500 °C under 4 mbar H2 in a dedicated Environmental Transmission Electron Microscope (ETEM).

Published
2019
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26. Mechanical response of gasoline soot nanoparticles under compression: An in situ TEM study

Author

Arash Khajeh, Istvan Zoltan Jenei, Ashlie Martini, Hamed Ghaednia, Fabrice Dassenoy, Arup Gangopadhyay, Thierry Epicier, Dairene Uy, Laboratoire de Tribologie et Dynamique des Systèmes (LTDS), École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Ecole Nationale d'Ingénieurs de Saint Etienne (ENISE)-Centre National de la Recherche Scientifique (CNRS), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), University of California [Merced] (UC Merced), University of California (UC), Ford Motor Company, Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Ecole Nationale d'Ingénieurs de Saint Etienne-Centre National de la Recherche Scientifique (CNRS), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), University of California [Merced], and University of California

Subjects
In situ, Materials science, Nanoparticle, Modulus, 02 engineering and technology, Molecular dynamics, medicine.disease_cause, [SPI.MAT]Engineering Sciences [physics]/Materials, Diesel fuel, 0203 mechanical engineering, In situ TEM, medicine, Gasoline, Composite material, Mechanical Engineering, Compression, Soot nanoparticle, Surfaces and Interfaces, 021001 nanoscience & nanotechnology, Compression (physics), Soot, Surfaces, Coatings and Films, 020303 mechanical engineering & transports, Mechanics of Materials, Transmission electron microscopy, 0210 nano-technology
Abstract

International audience; Gasoline soot nanoparticles (SNPs) were studied by performing in situ compression tests on individual nanoparticles inside a transmission electron microscope. After consecutive compressions, the SNPs exhibited an elasto-plastic behavior, and an increasing trend in Young's modulus and hardness values. Molecular dynamics were used to simulate compression cycles, the results of which confirmed the observations made during the experiments. The simulations were used to investigate how the different structural components of the nanoparticles affect their elastic and plastic response. By comparing the behavior of gasoline and diesel SNPs under compression, differences were observed both experimentally and in the simulations: the former were found to be more elastic and less prone to become hard under compression compared to the latter.

Published
2019
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27. HAADF-STEM characterization and simulation of nanoparticle distributions in an inhomogeneous matrix

Author

Z. Liu, Guy Vitrant, Yaya Lefkir, Thierry Epicier, and Nathalie Destouches

Subjects
Accuracy and precision, Histology, Materials science, business.industry, Nanoparticle, Metamaterial, 02 engineering and technology, Image segmentation, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Dark field microscopy, 0104 chemical sciences, Pathology and Forensic Medicine, Characterization (materials science), Optics, Transmission electron microscopy, Microscopy, 0210 nano-technology, business
Abstract

Measuring with a high accuracy the size distribution of small metallic nanoparticles loaded in a mesoporous metal oxide matrix is of particular interest for many studies related to new generations of interesting metamaterials. Transmission electron microscopy (TEM) is a powerful tool to determine the nature and morphology of very small particles, but their reliable and automatic identification in an inhomogeneous environment where the nanoparticle/background contrast locally varies is not straightforward. Here, we present how a quantitative analysis of high-angle annular dark field scanning TEM (HAADF STEM) images, accounting for the chemical sensitivity of the technique, can improve the accuracy of semiautomatic segmentation methods based on morphological processing to calculate size histograms. The paper also provides an estimate of the reliability of this method through the analysis of numerically synthesized images. The latter are based on the simulation of HAADF STEM projections of a volume filled with titania, pores and silver particles, whose morphological features, such as dimensions, shapes and densities are evaluated from experimental measurements of real samples. The results obtained with synthesized images prove the performances of the quantitative analysis to suppress nonsilver nanoparticles from the statistics and allow to infer empirical rules to determine imaging parameters that ensure a good reliability of histograms. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society

Published
2017
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28. 2D & 3D in situ study of the calcination of Pd nanocatalysts supported on delta-Alumina in an Environmental Transmission Electron Microscope

Author

Thierry Epicier, Siddardha Koneti, Priscilla Avenier, Amandine Cabiac, Anne-Sophie Gay, Lucian Roiban, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), IFP Energies nouvelles (IFPEN), ANR-15-CE09-0009,3DCLEAN,Tri-Dimensionnel Nano-laboratoire catalytique environnemental(2015), and ANR-10-LABX-0064,Imust,Institut for Multiscale Science and Technology : from Fundamental Physics and Chemistry to Engineering in New Material and Processes and Ecotechnologies(2010)

Subjects
Ostwald ripening, Microscope, Materials science, Ultra-high vacuum, Nanotechnology, 02 engineering and technology, General Chemistry, [CHIM.CATA]Chemical Sciences/Catalysis, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Catalysis, Nanomaterial-based catalyst, 0104 chemical sciences, law.invention, symbols.namesake, Electron tomography, law, Transmission electron microscopy, Environmental Transmission Electron Microscope, symbols, Calcination, 0210 nano-technology
Abstract

International audience; The quality of metallic nanoparticles (NPs) used in heterogeneous catalysis relies through many aspects on their small size, on the homogeneity of their spatial distribution on their supports and on their ability to resist to sintering or coalescence. It is thus very important to quantify these parameters and understand the mechanisms controlling the growth of NPs during the genesis process of the catalyst. Whereas conventional Transmission Electron Microscopy (TEM) is currently used for these purposes, it most frequently remains a ‘static’ method where results are obtained in high vacuum and post mortem, i.e. after the typical drying, calcination and reduction steps without the possibility to follow directly the evolution of both NPs and supports during those treatments. Environmental TEM (ETEM) unlocks this blocking and allows elementary mechanisms, such as Ostwald Ripening and coalescence to be unravelled through direct in situ observations. We report here an ETEM study of the preparation of Pd-based narrow NPs, less than 5 nm in size, deposited on a δ-alumina support. We focused on 3 main objectives: (i) quantifying the sizes of NPs at each preparation step performed in situ under environmental (i.e. respectively oxygen or air and hydrogen atmospheres at working temperatures) and comparing them to post mortem measurements; (ii) identify the oxidation state of the NPs through an in situ High Resolution imaging study of their crystallographic structure; (iii) explore the possibilities of environmental tri-dimensional (3D) studies by tilt series based Electron Tomography. This last item represents a challenging breakthrough in the characterization of nanocatalysts; it will be demonstrated that the use of modern instruments (microscope and accessories) allows tomographic acquisitions to be performed very fast, within a few minutes and even seconds, which opens the way to the 3D tracking of microstructures almost in real time during their evolution under gas and at high temperature.

Published
2019
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30. PEALD of Pt nanoparticles: towards the development of single electron transistors and flexible strain sensors

Author

Etienne Puyoo, Daniel Thomas, Martine LE BERRE, Liviu Militaru, Christophe Malhaire, Siddardha Koneti, Solène Brottet, Rémi Rafael, Matthieu Bugnet, Annie Malchere, Thierry Epicier, Lucian Roiban, INL - Dispositifs Electroniques (INL - DE), Institut des Nanotechnologies de Lyon (INL), Centre National de la Recherche Scientifique (CNRS)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-École Centrale de Lyon (ECL), Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-École supérieure de Chimie Physique Electronique de Lyon (CPE)-Centre National de la Recherche Scientifique (CNRS)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-École supérieure de Chimie Physique Electronique de Lyon (CPE), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), INL - Plateforme Technologique Nanolyon (INL - Nanolyon), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), LE BERRE, Martine, École Centrale de Lyon (ECL), Université de Lyon-École Supérieure de Chimie Physique Électronique de Lyon (CPE)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-École Centrale de Lyon (ECL), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM)

Subjects
[SPI.NANO] Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018

31. Elastic Properties of Cerium Oxide Nanocubes from In Situ TEM Compression Tests and DFT+U Simulations

Author

Lucile Joly-Pottuz, Manuel Cobian, Tristan Albaret, Douglas Stauffer, Karine Masenelli-Varlot, Thierry Epicier, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), Institut Lumière Matière [Villeurbanne] (ILM), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Tribologie et Dynamique des Systèmes (LTDS), École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Ecole Nationale d'Ingénieurs de Saint Etienne-Centre National de la Recherche Scientifique (CNRS), Bruker Nano, Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM), and Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Ecole Nationale d'Ingénieurs de Saint Etienne (ENISE)-Centre National de la Recherche Scientifique (CNRS)

Subjects
In situ, Cerium oxide, Materials science, 02 engineering and technology, 021001 nanoscience & nanotechnology, Compression (physics), 01 natural sciences, 0103 physical sciences, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Composite material, 010306 general physics, 0210 nano-technology, Instrumentation, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018
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32. Correlative HAADF-STEM and EDX-STEM Tomography for the 3D Morphological and Elemental Analysis of FinFET Semiconductor Devices

Author

Martin Jacob, Rafael Bortolin Pinheiro, Zineb Saghi, Frédéric Mazen, Thierry Epicier, Julien Sorel, Toby Sanders, Adeline Grenier, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Institut National des Sciences Appliquées (INSA), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon, School of Mathematical and Statistical Sciences (Arizona, Tempe), Arizona State University [Tempe] (ASU), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
010302 applied physics, Correlative, Materials science, Nanotechnology, 02 engineering and technology, STEM Tomography, Semiconductor device, 021001 nanoscience & nanotechnology, 01 natural sciences, Elemental analysis, 0103 physical sciences, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, Instrumentation, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018
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33. Very Fast Tomography in the (E)TEM to Probe Dynamics in Materials during Operando and In Situ Experiments

Author

Thierry Epicier, Hussein Banjak, Anne-Sophie Gay, Thomas Grenier, Sid Koneti, Voichita Maxim, Lucian Roiban, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Imagerie Tomographique et Radiothérapie, Centre de Recherche en Acquisition et Traitement de l'Image pour la Santé (CREATIS), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), IFP Energies nouvelles (IFPEN), Images et Modèles, ANR-15-CE09-0009,3DCLEAN,Tri-Dimensionnel Nano-laboratoire catalytique environnemental(2015), Epicier, Thierry, Tri-Dimensionnel Nano-laboratoire catalytique environnemental - - 3DCLEAN2015 - ANR-15-CE09-0009 - AAPG2015 - VALID, Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet - Saint-Étienne (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet - Saint-Étienne (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
0301 basic medicine, In situ, Materials science, Dynamics (mechanics), 02 engineering and technology, 021001 nanoscience & nanotechnology, [PHYS.COND.CM-MS] Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 03 medical and health sciences, 030104 developmental biology, Chemical physics, Environmental TEM, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Tomography, 0210 nano-technology, Instrumentation, Transmission Electron Microscopy TEM, ComputingMilieux_MISCELLANEOUS, Operando TEM
Abstract

International audience

Published
2018
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34. Visualizing and Quantifying the Cationic Mobility at {100} Surfaces of Ceria: Application to CO2 Adsorption/Desorption Phenomena in the Environmental Transmission Electron Microscope

Author

Matthieu Bugnet, Steven H. Overbury, Frederic Meunier, Francisco J. Cadete Santos Aires, Zili Wu, Thierry Epicier, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), IRCELYON-Approches thermodynamiques, analytiques et réactionnelles intégrées (ATARI), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRCELYON-Ingéniérie, du matériau au réacteur (ING), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM), Institut Pprime (PPRIME), Université de Poitiers-ENSMA-Centre National de la Recherche Scientifique (CNRS), Oak Ridge National Laboratory [Oak Ridge] (ORNL), UT-Battelle, LLC, Internal Medicine Research Unit (IMRU - BUENOS AIRES), Hospital Italiano - BUENOS AIRES (Hop It - BUENOS AIRES), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon, and Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, 020502 materials, Cationic polymerization, 02 engineering and technology, [CHIM.CATA]Chemical Sciences/Catalysis, 021001 nanoscience & nanotechnology, Co2 adsorption, 0205 materials engineering, Chemical engineering, Desorption, Environmental Transmission Electron Microscope, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM]Chemical Sciences, 0210 nano-technology, Instrumentation, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018
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35. Contribution of Local Analysis Techniques for the Characterization of Iron and Alloying Elements in Nitrides: Consequences on the Precipitation Process in Fe⁻Si and Fe⁻Cr Nitrided Alloys

Author

Hugo P, Van Landeghem, Raphaële, Danoix, Mohamed, Gouné, Sylvie, Bordère, Andrius, Martinavičius, Peter, Jessner, Thierry, Epicier, Béatrice, Hannoyer, Frédéric, Danoix, and Abdelkrim, Redjaïmia

Subjects
clusters precipitation, APT and TEM characterization, excess nitrogen, Fe–Si and Fe–Cr nitrided alloys, Article
Abstract

Atom Probe Tomography (APT), Transmission Electron Microscopy (TEM), and 3D mechanical calculations in complex geometry and anisotropic strain fields were employed to study the role of minor elements in the precipitation process of silicon and chromium nitrides in nitrided Fe–Si and Fe–Cr alloys, respectively. In nitrided Fe–Si alloys, an original sequence of Si3N4 precipitation was highlighted. Al–N clusters form first and act as nucleation sites for amorphous Si3N4 nitrides. This novel example of particle-simulated nucleation opens a new way to control Si3N4 precipitation in Fe–Si alloys. In nitrided Fe–Cr alloys, both the presence of iron in chromium nitrides and excess nitrogen in the ferritic matrix are unquestionably proved. Only a certain part of the so-called excess nitrogen is shown to be explained by the elastic accommodation of the misfit between nitride and the ferritic matrix. The presence of immobile excess nitrogen trapped at interfaces can be highly suspected.

Published
2018

36. Uncovering the 3D Structure of Combustion-Synthesized Noble Metal-Ceria Nanocatalysts

Author

Lucian Roiban, Franck Morfin, Thierry Epicier, Pascale Mascunan, Mimoun Aouine, Siddardha Koneti, Laurent Piccolo, Thanh-Son Nguyen, IRCELYON-Ingéniérie, du matériau au réacteur (ING), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRCELYON-Analyse chimique, texture (ANALYSE), IRCELYON-Microscopie (MICROSCOPIE), IRCELYON-Catalyse Hétérogène pour la Transition Energétique (CATREN), and IRCELYON, ProductionsScientifiques

Subjects
Materials science, Scanning electron microscope, Nanoparticle, Nanotechnology, 02 engineering and technology, engineering.material, 010402 general chemistry, Platinum nanoparticles, Heterogeneous catalysis, 01 natural sciences, Catalysis, Inorganic Chemistry, Scanning transmission electron microscopy, Physical and Theoretical Chemistry, Organic Chemistry, [CHIM.CATA] Chemical Sciences/Catalysis, [CHIM.CATA]Chemical Sciences/Catalysis, 021001 nanoscience & nanotechnology, [SDE.ES]Environmental Sciences/Environmental and Society, Nanomaterial-based catalyst, 0104 chemical sciences, engineering, Noble metal, [SDE.ES] Environmental Sciences/Environmental and Society, 0210 nano-technology, Mesoporous material
Abstract

ANALYSE:MICROSCOPIE+ECI2D:ING+FMO:PMA:MAO:LPI; International audience; With its unique redox properties, ceria is an oxide with a range of applications, including automotive catalytic converters, which consist of platinum-group metal nanoparticles on ceria-containing supports. In this work, the 3D architecture of a ceria-based material synthesized by the widely employed glycine- nitrate solution combustion method [1,2] is revealed for the first time.Together with N2 adsorption volumetry, scanning transmission electron microscopy (STEM) and scanning electron microscopy (SEM), STEM tomography provides a comprehensive picture of the multimodal porous network of a pre-reduced Pt-CeO2 catalyst, from the nanometer to the micrometer scale. This material consists of ceria nanocrystallites forming 3D aggregates and puzzle-like 2D walls separating large roundish mesopores and macropores. The small voids between imperfectly assembled crystallites give rise to some microporosity. In addition, it is demonstrated that a significant proportion of platinum nanoparticles (3–4 nm) are not located at the ceria surface following the one-step synthesis process, i.e. about half of them are buried within ceria. This result is valid for another metal (Rh) and another fuel (oxalyl dihydrazide), and has important implications for heterogeneous catalysis [3].References[1]A. Varma, A.S. Mukasyan, A.S. Rogachev, K.V. Manukyan, Chemical Reviews 2016, 116, 14496-14586.[2]F. Morfin, T.S. Nguyen, J.L. Rousset, L. Piccolo, Applied Catalysis B: Environmental 2016, 197, 2-13.[3]L. Roiban, S. Koneti, F. Morfin, T.S. Nguyen, P. Mascunan, M. Aouine, T. Epicier, L. Piccolo, ChemCatChem 2017, 9, 4607-4613.

Published
2018

37. Evaluation of noise and blur effects with SIRT-FISTA-TV reconstruction algorithm: Application to fast environmental transmission electron tomography

Author

Hussein Banjak, Thomas Grenier, Thierry Epicier, Siddardha Koneti, Lucian Roiban, Anne-Sophie Gay, Isabelle Magnin, Françoise Peyrin, Voichita Maxim, Imagerie Tomographique et Radiothérapie, Centre de Recherche en Acquisition et Traitement de l'Image pour la Santé (CREATIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Hospices Civils de Lyon (HCL)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Images et Modèles, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), IFP Energies nouvelles (IFPEN), Imagerie et modélisation Vasculaires, Thoraciques et Cérébrales (MOTIVATE), European Synchrotron Radiation Facility (ESRF), ANR-15-CE09-0009,3DCLEAN,Tri-Dimensionnel Nano-laboratoire catalytique environnemental(2015), ANR-11-IDEX-0007,Avenir L.S.E.,PROJET AVENIR LYON SAINT-ETIENNE(2011), ANR-11-LABX-0063,PRIMES,Physique, Radiobiologie, Imagerie Médicale et Simulation(2011), 4 - Imagerie Tomographique et Radiothérapie, Centre de Recherche en Acquisition et Traitement de l'Image pour la Santé ( CREATIS ), Hospices Civils de Lyon ( HCL ) -Université Jean Monnet [Saint-Étienne] ( UJM ) -Institut National de la Santé et de la Recherche Médicale ( INSERM ) -Centre National de la Recherche Scientifique ( CNRS ) -Université Claude Bernard Lyon 1 ( UCBL ), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon ( INSA Lyon ), Université de Lyon-Institut National des Sciences Appliquées ( INSA ) -Institut National des Sciences Appliquées ( INSA ) -Hospices Civils de Lyon ( HCL ) -Université Jean Monnet [Saint-Étienne] ( UJM ) -Institut National de la Santé et de la Recherche Médicale ( INSERM ) -Centre National de la Recherche Scientifique ( CNRS ) -Université Claude Bernard Lyon 1 ( UCBL ), Université de Lyon-Institut National des Sciences Appliquées ( INSA ) -Institut National des Sciences Appliquées ( INSA ), 2 - Images et Modèles, Matériaux, ingénierie et science [Villeurbanne] ( MATEIS ), Université Claude Bernard Lyon 1 ( UCBL ), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique ( CNRS ) -Institut National des Sciences Appliquées de Lyon ( INSA Lyon ), IFP Energies nouvelles ( IFPEN ), 1 - Imagerie et modélisation Vasculaires, Thoraciques et Cérébrales ( MOTIVATE ), and European Synchrotron Radiation Facility ( ESRF )

Subjects
[ INFO.INFO-TS ] Computer Science [cs]/Signal and Image Processing, Computer science, ComputingMethodologies_IMAGEPROCESSINGANDCOMPUTERVISION, 02 engineering and technology, Iterative reconstruction, 01 natural sciences, Poor quality, [INFO.INFO-TS]Computer Science [cs]/Signal and Image Processing, Robustness (computer science), Environmental TEM, Fast acquisition, 0103 physical sciences, [INFO.INFO-IM]Computer Science [cs]/Medical Imaging, Computer vision, Segmentation, Instrumentation, Tilt series, 010302 applied physics, [ INFO.INFO-IM ] Computer Science [cs]/Medical Imaging, business.industry, Reconstruction algorithm, 021001 nanoscience & nanotechnology, Atomic and Molecular Physics, and Optics, Electronic, Optical and Magnetic Materials, Electron tomography, Artificial intelligence, Tomography, 0210 nano-technology, business, Nanocatalysts
Abstract

International audience; Highlights The proposed SIRT-FISTA-TV algorithm is adapted to tomography reconstruction from tilt series of images such as recorded in Transmission Electron Microscopy. It produces reconstructed volumes with clear and sharp edges, and thus, the segmentation step was quite easy to perform after 3D reconstruction.SIRT-FISTA-TV can suppress noise artifacts without affecting spatial resolution.SIRT-FISTA-TV is robust to blurred data and gives better results than conventional reconstruction algorithms.SIRT-FISTA-TV is very well adapted to 3D reconstruction of experimental data (i.e. tilt series of projections) collected during very rapid tilt series acquisitions (down to 5 seconds) in situ or operando environmental TEM for studying dynamics of nanomaterials such as nanocatalysts.Fast tomography in Environmental Transmission Electron Microscopy (ETEM) is of a great interest for in situ experiments where it allows to observe 3D real-time evolution of nanomaterials under operating conditions. In this context, we are working on speeding up the acquisition step to a few seconds mainly with applications on nanocatalysts. In order to accomplish such rapid acquisitions of the required tilt series of projections, a modern 4K high-speed camera is used, that can capture up to 100 images per second in a 2K binning mode. However, due to the fast rotation of the sample during the tilt procedure, noise and blur effects may occur in many projections which in turn would lead to poor quality reconstructions. Blurred projections make classical reconstruction algorithms inappropriate and require the use of prior information. In this work, a regularized algebraic reconstruction algorithm named SIRT-FISTA-TV is proposed. The performance of this algorithm using blurred data is studied by means of a numerical blur introduced into simulated images series to mimic possible mechanical instabilities/drifts during fast acquisitions. We also present reconstruction results from noisy data to show the robustness of the algorithm to noise. Finally, we show reconstructions with experimental datasets and we demonstrate the interest of fast tomography with an ultra-fast acquisition performed under environmental conditions, i.e. gas and temperature, in the ETEM. Compared to classically used SIRT and SART approaches, our proposed SIRT-FISTA-TV reconstruction algorithm provides higher quality tomograms allowing easier segmentation of the reconstructed volume for a better final processing and analysis.

Published
2018
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38. Can the environmental TEM confirm atomistic models of adsorbed molecules at surfaces of solids?

Author

Thierry Epicier, Matthieu Bugnet, Olivier Matz, Ihor Pershukov, Monica Calatayud, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de chimie théorique (LCT), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Universitaire de France (IUF), and Ministère de l'Education nationale, de l’Enseignement supérieur et de la Recherche (M.E.N.E.S.R.)

Subjects
Adsorption, Materials science, 010405 organic chemistry, Chemical physics, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Molecule, [CHIM.CATA]Chemical Sciences/Catalysis, 02 engineering and technology, 021001 nanoscience & nanotechnology, 0210 nano-technology, 01 natural sciences, Instrumentation, 0104 chemical sciences
Abstract

International audience; It is well established that enhanced atomic mobility exists at ceria (CeO 2) surfaces in high vacuum (HV) conditions within the TEM, owing to beam-induced reduction effects. Controlling the atmosphere surrounding the specimen within an aberration-corrected environmental TEM (ETEM) allows to monitor the atomic mobility at {100} surfaces, and to directly visualize the projected atomic structure of the top surface of ceria nanocubes through high resolution TEM (HRTEM) imaging [1]. Therefore, it is pertinent to investigate the current capabilities of the ETEM to validate atomistic models of adsorbed molecules at the surface of materials. However, it is only possible to conclude about the nature of the contrasts at the surface by comparing the experimental HRTEM images to image simulations.

Published
2019
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39. Understanding the Growth Mechanisms of Ag Nanoparticles Controlled by Plasmon-Induced Charge Transfers in Ag-TiO2 Films

Author

Thierry Epicier, B. Bandyopadhyay, Yaya Lefkir, Nathalie Destouches, Said Bakhti, Francis Vocanson, Z. Liu, Musahid Ahmed, Yigang Fang, and Guy Vitrant

Subjects
Materials science, Doping, Nanotechnology, Laser, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, law.invention, General Energy, Chemical physics, law, Laser power scaling, Physical and Theoretical Chemistry, Surface plasmon resonance, Thin film, Excitation, Plasmon, Visible spectrum
Abstract

Mesoporous thin films of TiO2 doped with silver can undergo spectacular microstructural modifications upon laser scanning at visible wavelengths through the excitation of a localized surface plasmon resonance in Ag nanoparticles (NPs). The latter can result in competitive physicochemical mechanisms, leading either to the shrinkage or to the growth of NPs depending on the exposure conditions. Contrary to intuition, we provide evidence that the speed of the laser scan controls the size of NPs as follows: low speeds lead to silver oxidation and a decrease in the NP size, whereas high speeds induce rapid temperature rises and a spectacular growth of NPs. Both regimes are separated by a speed threshold that depends on extrinsic and intrinsic parameters such as laser power, beam diameter, and initial size of Ag NPs. We propose here a comprehensive model based on a set of coupled differential equations describing the transformations of silver under laser excitation between the Ag0, Ag+, and metallic NP states, w...

Published
2015
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40. Electron Tomography of Plasmonic Au Nanoparticles Dispersed in a TiO2 Dielectric Matrix

Author

Borges, Joel, Martin, Nicolas, Rodrigues, Marco Sampaio, Thierry, Epicier, Vaz, Filipe, Steyer, P, Siddardha, Koneti, Lucian, Roiban, Departamento de Física [Minho] (DFUM), Universidade do Minho, Franche-Comté Électronique Mécanique, Thermique et Optique - Sciences et Technologies (UMR 6174) (FEMTO-ST), Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Centre National de la Recherche Scientifique (CNRS)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC), and Universidade do Minho (Centro de Física)

Subjects
[SPI.ACOU]Engineering Sciences [physics]/Acoustics [physics.class-ph], [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

International audience; Plasmonic Au nanoparticles (AuNPs) embedded into a TiO2 dielectric matrix were analyzed by combining two-dimensional and three-dimensional electron microscopy techniques. The preparation method was reactive magnetron sputtering, followed by thermal annealing treatments at 400 and 600 °C. The goal was to assess the nanostructural characteristics and correlate them with the optical properties of the AuNPs, particularly the localized surface plasmon resonance (LSPR) behavior. High-angle annular dark fieldscanning transmission electron microscopy results showed the presence of small-sized AuNPs (quantum size regime) in the as-deposited Au−TiO2 film, resulting in a negligible LSPR response. The in-vacuum thermal annealing at 400 °C induced the formation of intermediate-sized nanoparticles (NPs), in the range of 10−40 nm, which led to the appearance of a well-defined LSPR band, positioned at 636 nm. Electron tomography revealed that most of the NPs are small-sized and are embedded into the TiO2 matrix, whereas the larger NPs are located at the surface. Annealing at 600 °C promotes a bimodal size distribution with intermediate-sized NPs embedded in the matrix and bigsized NPs, up to 100 nm, appearing at the surface. The latter are responsible for a broadening and a redshift, to 645 nm, in the LSPR band because of increase of scattering-to-absorption ratio. Beyond differentiating and quantifying the surface and embedded NPs, electron tomography also provided the identification of “hot-spots”. The presence of NPs at the surface, individual or in dimers, permits adsorption sites for LSPR sensing and for surface-enhanced spectroscopies, such as surfaceenhanced Raman scattering.

Published
2018

41. Lateral growth of NiSi at the θ-Ni2Si/Si(100) interface: Experiments and modelling

Author

Federico Panciera, Thierry Epicier, M. El Kousseifi, Khalid Hoummada, Dominique Mangelinck, 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), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), and Université de Toulon (UTLN)-Centre National de la Recherche Scientifique (CNRS)-Aix Marseille Université (AMU)

Subjects
Silicides, Materials science, Thin films, Intermetallic, Nucleation, 02 engineering and technology, 01 natural sciences, Precipitates, [SPI.MAT]Engineering Sciences [physics]/Materials, Mechanical equilibrium, chemistry.chemical_compound, Microelectronics, Models, Phase (matter), 0103 physical sciences, Silicide, Lateral growth, Growth kinetics, Kinetics parameter, Large aspect ratio, Nickel compounds, Electrical and Electronic Engineering, Thin film, 010302 applied physics, Condensed matter physics, business.industry, Contact formation, Enzyme kinetics, Film thickness, Large diameter, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Aspect ratio (image), Aspect ratio, Atomic and Molecular Physics, and Optics, Surface energy, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Triple lines, chemistry, Interfacial energy, Film growth, 0210 nano-technology, business
Abstract

cited By 0; International audience; The nucleation and lateral growth are more and more important steps for the thin film growth of a phase (silicide, intermetallic…) when the thin film thickness is in the range or below 10 nm. It might become crucial for contact in microelectronics that are in this range of thickness for actual devices and affect the properties of contacts in different parts of the devices. For reaction between 10 nm Ni(10%Pt) and (100)Si, it was shown that NiSi grows by nucleation and lateral growth at the epitaxial θ-Ni2Si/Si interface and forms precipitates having a large aspect ratio (large diameter and small thickness) were observed. In this work, the precipitate shape as well as the shape of the different interfaces close to the triple line are reproduced by using the model of Pasichnyy and Gusak for θ-Ni2Si/Si interfaces that are either curved or straight. The deduced interfacial energies and kinetics parameters enabling to obtain the characteristics of the precipitates are discussed and compared to the ones obtained by the model of El Kousseifi et al. The conditions for mechanical equilibrium and the implication for the contact formation are discussed. © 2018 Elsevier B.V.

Published
2018
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42. Mechanical characterization of diesel soot nanoparticles: in situ compression in a transmission electron microscope and simulations

Author

Ashlie Martini, Dairene Uy, Thierry Epicier, Arash Khajeh, Arup Gangopadhyay, Fabrice Dassenoy, Istvan Zoltan Jenei, Hamed Ghaednia, Laboratoire de Tribologie et Dynamique des Systèmes ( LTDS ), École Centrale de Lyon ( ECL ), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État ( ENTPE ) -Ecole Nationale d'Ingénieurs de Saint Etienne-Centre National de la Recherche Scientifique ( CNRS ), Matériaux, ingénierie et science [Villeurbanne] ( MATEIS ), Université Claude Bernard Lyon 1 ( UCBL ), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique ( CNRS ) -Institut National des Sciences Appliquées de Lyon ( INSA Lyon ), Université de Lyon-Institut National des Sciences Appliquées ( INSA ) -Institut National des Sciences Appliquées ( INSA ), Stockholm University, Laboratoire de Tribologie et Dynamique des Systèmes (LTDS), École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Ecole Nationale d'Ingénieurs de Saint Etienne-Centre National de la Recherche Scientifique (CNRS), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), University of California [Merced], University of California, Ford Motor Company, Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Ecole Nationale d'Ingénieurs de Saint Etienne (ENISE)-Centre National de la Recherche Scientifique (CNRS), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM), University of California [Merced] (UC Merced), University of California (UC), and ANR-11-IDEX-0007,Avenir L.S.E.,PROJET AVENIR LYON SAINT-ETIENNE(2011)

Subjects
Materials science, soot nanoparticle, [ SPI.MAT ] Engineering Sciences [physics]/Materials, Modulus, Nanoparticle, Bioengineering, 02 engineering and technology, medicine.disease_cause, 7. Clean energy, in situ TEM, [SPI.MAT]Engineering Sciences [physics]/Materials, 0203 mechanical engineering, [SPI.MECA.MEMA]Engineering Sciences [physics]/Mechanics [physics.med-ph]/Mechanics of materials [physics.class-ph], medicine, General Materials Science, Electrical and Electronic Engineering, Lubricant, Composite material, Elastic modulus, ComputingMilieux_MISCELLANEOUS, Mechanical Engineering, Electron energy loss spectroscopy, General Chemistry, Nanoindentation, 021001 nanoscience & nanotechnology, compression, Soot, molecular dynamics, 020303 mechanical engineering & transports, Mechanics of Materials, Transmission electron microscopy, 0210 nano-technology
Abstract

International audience; Incomplete fuel burning inside an internal combustion engine results in the creation of soot in the form of nanoparticles. Some of these soot nanoparticles (SNP) become adsorbed into the lubricating oil film present on the cylinder walls, which adversely affects the tribological performance of the lubricant. In order to better understand the mechanisms underlying the wear caused by SNPs, it is important to understand the behavior of SNPs and to characterize potential changes in their mechanical properties (e.g. hardness) caused by (or during) mechanical stress. In this study, the behavior of individual SNPs originating from diesel engines was studied under compression. The experiments were performed in a transmission electron microscope using a nanoindentation device. The nanoparticles exhibited elasto-plastic behavior in response to consecutive compression cycles. From the experimental data, the Young's modulus and hardness of the SNPs were calculated. The Young's modulus and hardness of the nanoparticles increased with the number of compression cycles. Using an electron energy loss spectroscopy technique, it was shown that the sp(2)/sp(3) ratio within the compressed nanoparticle decreases, which is suggested to be the cause of the increase in elasticity and hardness. In order to corroborate the experimental findings, molecular dynamics simulations of a model SNP were performed. The SNP model was constructed using carbon and hydrogen atoms with morphology and composition comparable to those observed in the experiment. The model SNP was subjected to repeated compressions between two virtual rigid walls. During the simulation, the nanoparticle exhibited elasto-plastic behavior like that in the experiments. The results of the simulations confirm that the increase in the elastic modulus and hardness is associated with a decrease in the sp(2/)sp(3) ratio.

Published
2018
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43. Hollow Beta Zeolite Single Crystals for the Design of Selective Catalysts

Author

Lucian Roiban, Siddhardha Koneti, David Farrusseng, Thierry Epicier, Ana Rita Morgado Prates, Alain Tuel, Nicolas Bats, Frederic Meunier, Laurence Burel, Céline Pagis, Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IFP Energies nouvelles (IFPEN), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Chemical substance, Materials science, 010405 organic chemistry, technology, industry, and agriculture, General Chemistry, [CHIM.CATA]Chemical Sciences/Catalysis, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, Condensed Matter Physics, 01 natural sciences, 0104 chemical sciences, law.invention, Catalysis, Crystal, Metal, Chemical engineering, Electron tomography, Magazine, law, visual_art, visual_art.visual_art_medium, General Materials Science, Zeolite, Science, technology and society
Abstract

We present a Pt@Beta catalyst with a unique, well-controlled location of metal nanoparticles that allows more efficient use of this rare, expensive metal in catalysis. The zeolite crystal has an inner cavity, leaving a thin zeolite shell where the metal nanoparticles are encapsulated, thereby ensuring a relatively small diffusional path length and high selectivity. Hollow Beta is obtained by a controlled dissolution–recrystallization method. The location of the particles not only was revealed by electron tomography 3D reconstruction but was further confirmed by a model hydrogenation reaction of aromatics.

Published
2018
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44. Investigation of the in-plane and out-of-plane electrical properties of metallic nanoparticles in dielectric matrix thin films elaborated by atomic layer deposition

Author

Daniel Thomas, Lucian Roiban, A Malchère, L. Militaru, Etienne Puyoo, M. Le Berre, David Albertini, Thierry Epicier, Siddardha Koneti, Francis Calmon, Andrei Sabac, INL - Dispositifs Electroniques (INL - DE), Institut des Nanotechnologies de Lyon (INL), École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-École supérieure de Chimie Physique Electronique de Lyon (CPE)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), INL - Plateforme Technologique Nanolyon (INL - Nanolyon), and ANR-11-IDEX-0007,Avenir L.S.E.,PROJET AVENIR LYON SAINT-ETIENNE(2011)

Subjects
Electron mobility, Materials science, Analytical chemistry, Bioengineering, 02 engineering and technology, 01 natural sciences, Atomic layer deposition, Planar, 0103 physical sciences, General Materials Science, Electrical and Electronic Engineering, Thin film, 010302 applied physics, metallic nanoparticles, Condensed matter physics, Mechanical Engineering, [SPI.NRJ]Engineering Sciences [physics]/Electric power, shadow edge evaporation, General Chemistry, 021001 nanoscience & nanotechnology, Evaporation (deposition), Mechanics of Materials, atomic layer deposition, electrical properties, Electrode, 0210 nano-technology, Current density, Order of magnitude
Abstract

International audience; Pt nanoparticles in a Al2O3 dielectric matrix thin films are elaborated by means of atomic layer deposition. These nanostructured thin films are integrated in vertical and planar test structures in order to assess both their in-plane and out-of-plane electrical properties. A shadow edge evaporation process is used to develop planar devices with electrode separation distances in the range of 30 nm. Both vertical and planar test structures show a Poole–Frenkel conduction mechanism. Low trap energy levels (

Published
2017
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45. The Influence of Vanadium on Ferrite and Bainite Formation in a Medium Carbon Steel

Author

Frédéric Danoix, Sophie Cazottes, Francisca García Caballero, Carlos Garcia-Mateo, D. Milbourn, Thierry Epicier, Thomas Sourmail, Asco Industries CREAS, El Centro Nacional de Investigaciones Metalúrgicas (CENIM), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA), Groupe de physique des matériaux (GPM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU), Vanitec Ltd, Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), and Vanitec

Subjects
Materials science, Carbon steel, Bainite, Medium carbon forging steel, Nucleation, Vanadium, chemistry.chemical_element, 02 engineering and technology, Atom probe, engineering.material, 01 natural sciences, law.invention, law, Ferrite (iron), 0103 physical sciences, Influence transformation kinetics, ComputingMilieux_MISCELLANEOUS, 010302 applied physics, Metallurgy, Vanadium additions, Metals and Alloys, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Isothermal transformation diagram, chemistry, Mechanics of Materials, engineering, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, Solid solution
Abstract

The influence of vanadium additions on transformation kinetics has been investigated in a medium carbon forging steel. Using dilatometry to track transformation during continuous cooling or isothermal transformation, the impact of vanadium on both ferrite-pearlite and bainite has been quantified. Transmission electron microscopy and atom probe tomography have been used to establish whether vanadium was present in solid solution, or as clusters and precipitates. The results show that vanadium in solid solution has a pronounced retarding influence on ferrite-pearlite formation and that, unlike in the case of niobium, this effect can be exploited even during relatively slow cooling. The influence on bainite transformation was found to depend on temperature; an explanation in terms of the effect of vanadium on heterogeneous nucleation is tentatively proposed., The authors are grateful to Vanitec for financial support of the present work and to Kira J. Weissman for careful proofreading of the manuscript.

Published
2017
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46. Nanoparticles in The ETEM: From Gas-Surface Interactions of Single Objects to Collective Behavior of Nanocatalysts

Author

Thierry Epicier, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), and ANR-15-CE09-0009,3DCLEAN,Tri-Dimensionnel Nano-laboratoire catalytique environnemental(2015)

Subjects
Surface (mathematics), Collective behavior, Materials science, 010405 organic chemistry, Nanoparticle, Nanotechnology, 010402 general chemistry, 01 natural sciences, Instrumentation, Nanomaterial-based catalyst, ComputingMilieux_MISCELLANEOUS, 0104 chemical sciences, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

International audience

Published
2017
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47. Mechanical behavior law of ceramic nanoparticles from transmission electron microscopy in situ nano-compression tests

Author

Yves Jorand, J. B. Quirk, Sylvain Meille, Vincent Garnier, Jérôme Chevalier, Julien Réthoré, Emilie Calvié, Karine Masenelli-Varlot, Thierry Epicier, Lucile Joly-Pottuz, Claude Esnouf, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), Laboratoire de Mécanique des Contacts et des Structures [Villeurbanne] (LaMCoS), Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Mécanique Multiéchelle pour les solides (MIMESIS), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM)

Subjects
In situ, Ceramics, Materials science, Mechanical Engineering, Physics::Optics, Nanoparticle, Nanotechnology, Young's modulus, Condensed Matter Physics, Compression (physics), In situ testing, Finite element method, symbols.namesake, Mechanics of Materials, Transmission electron microscopy, visual_art, [SPI.MECA.MEMA]Engineering Sciences [physics]/Mechanics [physics.med-ph]/Mechanics of materials [physics.class-ph], Nano, visual_art.visual_art_medium, symbols, Nanoparticles, General Materials Science, Ceramic, Composite material
Abstract

International audience; A methodology has been developed to determine constitutive laws of nanoparticles from in situ nanocompression experiments in a transmission electron microscope. It is based on image analysis to obtain relevant load–displacement curves, followed by finite element analysis associated to an inverse method. A transition alumina, stable only at the nanometer size, has been characterized as an example. The Young modulus and yield strength of this transition alumina, not available for such crystallographic structure, have been obtained.

Published
2014
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48. Experimental Evidence for the Existence of an Iridium Sesquioxide Metastable Phase during ETEM Studies of Methane Steam Reforming on an Ir/Ce0.9Gd0.9O2-x Catalyst

Author

Thierry Epicier, Francisco J. Cadete Santos Aires, Patrick Gélin, L. Massin, Mimoun Aouine, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Institut de recherches sur la catalyse et l'environnement de Lyon (IRCELYON), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Application de la Chimie à l'Environnement (LACE), and Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, chemistry.chemical_element, [CHIM.CATA]Chemical Sciences/Catalysis, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 3. Good health, 0104 chemical sciences, Catalysis, Steam reforming, Sesquioxide, chemistry, Phase (matter), Metastability, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM]Chemical Sciences, Physical chemistry, Iridium, 0210 nano-technology, Instrumentation, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018
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49. Study of temperature and radiation induced microstructural changes in Xe-implanted UO2 by TEM, STEM, SIMS and positron spectroscopy

Author

Patrick Nedelec, Thierry Epicier, B. Marchand, Nikolay Djourelov, Y. Pipon, Hristo Marinov, Louis Raimbault, N. Bérerd, Nathalie Moncoffre, ACE, Institut de Physique des 2 Infinis de Lyon (IP2I Lyon), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Centre National de la Recherche Scientifique (CNRS), Institut de Physique Nucléaire de Lyon (IPNL), Laboratoire Pierre Süe (LPS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre de Géosciences (GEOSCIENCES), Mines Paris - PSL (École nationale supérieure des mines de Paris), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3), and MINES ParisTech - École nationale supérieure des mines de Paris

Subjects
Nuclear and High Energy Physics, Annealing (metallurgy), Analytical chemistry, chemistry.chemical_element, 02 engineering and technology, 01 natural sciences, 010305 fluids & plasmas, Positron, Xenon, 0103 physical sciences, Scanning transmission electron microscopy, General Materials Science, Irradiation, Spectroscopy, ComputingMilieux_MISCELLANEOUS, Chemistry, uranium dioxide, 021001 nanoscience & nanotechnology, Grain size, xenon, Nuclear Energy and Engineering, positron spectroscopy, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, SIMS, Doppler broadening
Abstract

Doppler broadening of annihilation gamma-line combined with a slow positron beam (SPB) was used to measure the momentum density distribution of annihilating pairs in a set of sintered UO 2 samples implantated with 800-keV 136 Xe 2+ at fluences of 1 × 10 15 and 1 × 10 16 Xe cm −2 . The effect of prolonged post-implantation annealing at 1673 and 1873 K, grain size, and 152-MeV Iodine irradiation were studied by analysis of S ( E ) profiles and S - W maps and discussed versus secondary ion mass spectroscopy (SIMS), scanning transmission electron microscopy results. Spectroscopy with SPB and SIMS is an excellent combination of complementary techniques for studying the formation and evolution of Xe-bubbles, and Xe retention.

Published
2013
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50. Xenon migration in UO2 under irradiation studied by SIMS profilometry

Author

C. Peaucelle, B. Marchand, Y. Pipon, Christine Delafoy, A. Perrat-Mabilon, Louis Raimbault, Philippe Sainsot, Nathalie Moncoffre, N. Bérerd, Clotilde Gaillard, C. Garnier, Thierry Epicier, M. Fraczkiewicz, N. Toulhoat, Institut de Physique Nucléaire de Lyon (IPNL), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3), AREVA TD, Université Claude Bernard Lyon 1 (UCBL), Université de Lyon, Centre de Géosciences (GEOSCIENCES), MINES ParisTech - École nationale supérieure des mines de Paris, Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL), Laboratoire de Mécanique des Contacts et des Structures [Villeurbanne] (LaMCoS), Institut National des Sciences Appliquées de Lyon (INSA Lyon), Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), and Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
010302 applied physics, Nuclear and High Energy Physics, Fission products, Nuclear fuel, Radiochemistry, Krypton, Pellets, chemistry.chemical_element, 02 engineering and technology, Atmospheric temperature range, 021001 nanoscience & nanotechnology, 01 natural sciences, 7. Clean energy, Secondary ion mass spectrometry, Xenon, Nuclear Energy and Engineering, chemistry, 0103 physical sciences, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], General Materials Science, Irradiation, 0210 nano-technology
Abstract

International audience; During Pressurized Water Reactor operation, around 25% of the created Fission Products (FP) are Xenon and Krypton. They have a low solubility in the nuclear fuel and can either (i) agglomerate into bubbles which induce mechanical stress in the fuel pellets or (ii) be released from the pellets, increasing the pressure within the cladding and decreasing the thermal conductivity of the gap between pellets and cladding. After fifty years of studies on the nuclear fuel, all mechanisms of Fission Gas Release (FGR) are still not fully understood. This paper aims at studying the FGR mechanisms by decoupling thermal and irradiation effects and by assessing the Xenon behavior for the first time by profilometry. Samples are first implanted with 136Xe at 800 keV corresponding to a projected range of 140 nm. They are then either annealed in the temperature range 1400-1600 °C, or irradiated with heavy energy ions (182 MeV Iodine) at Room Temperature (RT), 600 °C or 1000 °C. Depth profiles of implanted Xenon in UO2 are determined by Secondary Ion Mass Spectrometry (SIMS). It is shown that Xenon is mobile during irradiation at 1000 °C. In contrast, thermal treatments do not induce any Xenon migration process: these results are correlated to the formation of Xenon bubbles observed by Transmission Electron Microscopy

Published
2013
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