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28 results on '"Jérôme Laurencin"'

1. Particle-based model for functional and diffusion layers of solid oxide cells electrodes

Author

Johan Debayle, Jérôme Laurencin, Yann Gavet, Peter Cloetens, Hamza Moussaoui, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire Georges Friedel (LGF-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Département Procédés de Mise en oeuvre des Milieux Granulaires (PMMG-ENSMSE), Centre Sciences des Processus Industriels et Naturels (SPIN-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), European Synchrotron Radiation Facility (ESRF), Université Grenoble Alpes – CEA/LITEN, and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, General Chemical Engineering, microstructure, 02 engineering and technology, law.invention, [INFO.INFO-TS]Computer Science [cs]/Signal and Image Processing, 020401 chemical engineering, law, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, SOFC, 0204 chemical engineering, Diffusion (business), Parametric statistics, macroporosity, [INFO.INFO-CV]Computer Science [cs]/Computer Vision and Pattern Recognition [cs.CV], 021001 nanoscience & nanotechnology, Microstructure, [INFO.INFO-MO]Computer Science [cs]/Modeling and Simulation, Ellipsoid, Synchrotron, Metric (mathematics), Electrode, particle-based model, Particle, electrode modeling, SOEC, 0210 nano-technology, Biological system, X-ray tomography
Abstract

International audience; A novel particle-based model is proposed to generate synthetic yet representative 3D microstructures of typical SOC electrodes. The model steps can be related to the real electrode manufacturing routes, classically via powders processing, making it a practical tool for electrodes design optimization. The representativeness of the synthetic microstructures is checked on several two-phase (LSCF, LSC) and three-phase (Ni-YSZ) electrodes reconstructed by synchrotron X-ray and FIB-SEM tomography. The validation shows a very good agreement between the real and synthetic media in terms of metric, topological and physical properties. Furthermore, the model is adapted to simulate the microstructure of a typical Ni-YSZ current collecting layer by taking into account a bimodal pore-size-distribution. In this objective, the macro-pores resulting from the burning-off of specific pore-formers are morphologically separated in the reconstruction from the micro-porosity network. Finally, the geometrical features of the macro-pores are meticulously characterized and successfully emulated by using parametric ellipsoids.

Published
2020
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2. Linear sweep and cyclic voltammetry of porous mixed conducting oxygen electrode: Formal study of insertion, diffusion and chemical reaction model

Author

C. Montella, Jérôme Laurencin, V. Tezyk, E. Effori, E. Siebert, Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI), Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Matériaux Interfaces ELectrochimie (MIEL), Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Cyclic voltammetry, Thermodynamics, Solid-state diffusion, 02 engineering and technology, Linear sweep voltammetry, 010402 general chemistry, 01 natural sciences, Chemical reaction, Mixed conductor, law.invention, Zone diagram, [SPI]Engineering Sciences [physics], Reaction rate constant, Oxygen electrode, law, [CHIM]Chemical Sciences, General Materials Science, Clark electrode, Chemical reaction model, General Chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Electrode, 0210 nano-technology, Dimensionless quantity
Abstract

International audience; The classical 1D continuum model of oxygen exchange in a porous mixed conductor (bulk path) is presented in terms of Linear Sweep Voltammetry (LSV) and Cyclic Voltammetry (CV). We show that, from a formal point of view, it corresponds to an insertion, diffusion and chemical reaction mechanism. Some general rules for LSV/CV curves are established. Using a dimensionless description, we evidence eight different limiting behaviors of the electrochemical model, which depend on four dimensionless parameters. For an almost full insertion level at equilibrium, these parameters can be reduced to only two, i.e. the dimensionless electrode thickness L and the dimensionless chemical rate constant Lambda. We show that the resulting zone diagram, plotted using the representation log L versus log Lambda, is useful to predict the possible sequences of model behaviors as a function of the potential sweep rate and the electrode thickness. This theoretical analysis is applied to a porous LSCF oxygen electrode under air at high temperature.

Published
2021
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3. An elementary kinetic model for the LSCF and LSCF-CGO electrodes of solid oxide cells: impact of operating conditions and degradation on the electrode response

Author

M. Petitjean, Maxime Hubert, Jérôme Laurencin, Gregory Geneste, E. Siebert, Laurent Dessemond, E. Da Rosa Silva, T. David, E. Effori, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), DAM Île-de-France (DAM/DIF), Direction des Applications Militaires (DAM), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Matériaux Interfaces ELectrochimie (MIEL), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI), Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, LSCF, Oxide, 02 engineering and technology, 010402 general chemistry, 7. Clean energy, 01 natural sciences, chemistry.chemical_compound, Physics::Plasma Physics, Materials Chemistry, Electrochemistry, SOFC, Kinetic model, Renewable Energy, Sustainability and the Environment, LSCF-CGO, modeling, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, chemistry, Chemical engineering, Electrode, oxygen electrode, Degradation (geology), SOEC, 0210 nano-technology, [CHIM.OTHE]Chemical Sciences/Other, Electrochemical impedance spectroscopy
Abstract

International audience; An elementary kinetic model was developed to predict the electrochemical response of porous LSCF and LSCF-CGO electrodes. The model was validated thanks to experiments performed on symmetrical cells using a three-electrode setup. After the model calibration on polarization curves, it has been shown that the model is able to simulate accurately the experimental impedance diagram at OCP and under polarization without additional fitting. Moreover, the evolution of the electrode polarization resistance with the oxygen partial pressure is well reproduced by the model. The electrodes reaction mechanism was thoroughly analyzed and it has been shown that the transition from the bulk path to the surface path depends on the temperature, the polarization and the oxygen partial pressure. The rate-determining steps for the LSCF electrode have been identified at OCP as function of the oxygen partial pressure. Finally, a sensitivity analysis has been performed to study the impact of LSCF demixing on the electrode performances. For a given decomposition, it has been highlighted that the surface passivation would be more impacting than the decrease of the ionic conductivity. Moreover, the impact of the LSCF decomposition would be more detrimental for the electrode performances evaluated in electrolysis mode.

Published
2021
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4. Durability of nanostructured LaPrNiO4+δ electrode for solid oxide cells: Electrochemical, microstructural, and structural investigation

Author

Dario Ferreira Sanchez, Nur Istiqomah Khamidy, Elisabeth Djurado, Frédéric Charlot, F. Monaco, Jérôme Laurencin, Matériaux Interfaces ELectrochimie (MIEL), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI), Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), 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), Consortium des Moyens Technologiques Communs (CMTC), Institut National Polytechnique de Grenoble (INPG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Oxide, Energy Engineering and Power Technology, 02 engineering and technology, 010402 general chemistry, Electrochemistry, 01 natural sciences, law.invention, chemistry.chemical_compound, law, Phase (matter), Electrical and Electronic Engineering, Physical and Theoretical Chemistry, Clark electrode, ComputingMilieux_MISCELLANEOUS, Electrolysis, Renewable Energy, Sustainability and the Environment, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Microstructure, 0104 chemical sciences, Anode, chemistry, Chemical engineering, Electrode, 0210 nano-technology
Abstract

This work reports a durability study in galvanostatic mode at 700 °C for 900–960 h related to structural and microstructural evolution of LaPrNiO4+δ (LPNO) oxygen electrode. The performances of the electrode, deposited by electrostatic spray deposition (ESD) and screen printing (SP), are not changed when operated under electrolysis current whereas a degradation is observed in fuel cell mode. Small quantities of secondary phases (La,Pr)3Ni2O7-δ in the fine ESD microstructure and Pr6O11 on both ESD and SP layers are detected in the pristine electrode by synchrotron μ-X-ray diffraction and fluorescence. The destabilization of LPNO electrode, which slightly occurs in the ESD layer after thermal aging in air, is strongly accelerated under anodic and cathodic currents. Indeed, the formation of a new phase (La,Pr)4Ni3O10-δ on both ESD and SP layers occurs with the extension of (La,Pr)3Ni2O7-δ in the SP layer, and a significant increase in the amount Pr6O11 at high current density. Nevertheless, the electrode microstructure, determined by FIB-SEM tomography, remains stable under current whereas severe delamination is observed after aging in fuel cell mode. Based on these characterizations, the mechanisms of electrode aging have been discussed to explain the different behavior in fuel cell and electrolysis modes.

Published
2020
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5. Differential analysis of SOFC current-voltage characteristics

Author

Dario Montinaro, G. Raikova, Patric Szabo, Günter Schiller, Daria Vladikova, Zdravko Stoynov, Jérôme Laurencin, and Blagoy Burdin

Subjects
Work (thermodynamics), Materials science, 020209 energy, 02 engineering and technology, Temperature cycling, Solid oxide fuel cells, Management, Monitoring, Policy and Law, 7. Clean energy, Automotive engineering, law.invention, increased sensitivity, Differential analysis of current-voltage characteristics, Stack (abstract data type), law, 0202 electrical engineering, electronic engineering, information engineering, Sensitivity (control systems), new performance indicators, degradation, Electrolysis, Elektrochemische Energietechnik, Mechanical Engineering, Building and Construction, 021001 nanoscience & nanotechnology, Durability, General Energy, Constant current, 0210 nano-technology, Voltage
Abstract

Solid Oxide Fuel Cells (SOFCs) are regarded as a promising technology for economic power generation due to their high efficiency and large fuel flexibility. Durability is a severe hurdle towards their deployment. The near future targets in respect to Degradation Rate (DR) are about 0.1% kh−1, which needs improved monitoring and diagnostics. This work aims at introducing a new approach based on Differential Analysis of the i-V curves, named DiVA. It operates with the Differential Resistance Rd and its evolution during long term testing. Two new performance indicators are introduced. Since derivatives are more sensitive to small deviations, the Differential Resistance Analysis (DRA) ensures increased sensitivity and information capability in respect to degradation monitoring and diagnostics, which is demonstrated on a small stack during thermal cycling conditions – before and after the first thermal cycle, on button cells tested up to 9000 h, as well as on button cells operating in fuel cell and in electrolysis mode. The results show that DRA is several times more sensitive in comparison with the classical DR evaluation based on registration of the voltage decrease at constant current.

Published
2018
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6. Stochastic geometrical modeling of solid oxide cells electrodes validated on 3D reconstructions

Author

T. Le Bihan, Yann Gavet, Peter Cloetens, Johan Debayle, Gérard Delette, Maxime Hubert, Jérôme Laurencin, Hamza Moussaoui, Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Centre Sciences des Processus Industriels et Naturels (SPIN-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Laboratoire Georges Friedel (LGF-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), European Synchrotron Radiation Facility (ESRF), CEA Le Ripault (CEA Le Ripault), Direction des Applications Militaires (DAM), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Université Grenoble Alpes – CEA/LITEN, CEA, DAM, and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, General Computer Science, Stochastic modelling, Analytical chemistry, Phase (waves), General Physics and Astronomy, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Electrode design, law.invention, Truncated plurigaussian random fields, [INFO.INFO-TS]Computer Science [cs]/Signal and Image Processing, law, Position (vector), 3D microstructure model, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, General Materials Science, Random field, [INFO.INFO-CV]Computer Science [cs]/Computer Vision and Pattern Recognition [cs.CV], General Chemistry, 021001 nanoscience & nanotechnology, Microstructure, [INFO.INFO-MO]Computer Science [cs]/Modeling and Simulation, Thresholding, Synchrotron, 0104 chemical sciences, Solid oxide cell, Computational Mathematics, Mechanics of Materials, Electrode, 0210 nano-technology, Biological system, X-ray tomography
Abstract

International audience; An original 3D stochastic model, based on the truncated plurigaussian random fields, has been adapted to simulate the complex microstructure of SOC electrodes. The representativeness of the virtual microstructures has been checked on several synchrotron X-ray and FIB-SEM tomographic reconstructions obtained on typical LSCF, LSC and Ni-YSZ electrodes. The validation step has been carried out by comparing numbers of electrode morphological properties as well as the phase effective diffusivities. This analysis has shown that the synthetic media mimic accurately the complex microstructure of typical SOC electrodes. The model capability to simulate different types of promising electrode architectures has also been investigated. It has been shown that the model is able to generate virtual electrode prepared by infiltration resulting in a uniform and continuous thin layer covering a scaffold. With a local thresholding depending on the position, continuous graded electrodes can be also produced. Finally, the model offers the possibility to introduce different correlation lengths for each phase in order to control the local topology of the interfaces. All these cases illustrate the model flexibility to generate various SOC microstructures. This validated and flexible model can be used for further numerical microstructural optimizations to improve the SOC performances.

Published
2018
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7. Differential Resistance Analysis – a New Tool for Evaluation of Solid Oxide Fuel Cells Degradation

Author

Arata Nakajo, Dario Montinaro, Blagoy Burdin, Roberto Spotorno, Anthony Chesnaud, Alain Thorel, Daria Vladikova, Maxime Hubert, Zdravko Stoynov, Paolo Piccardo, and Jérôme Laurencin

Subjects
Work (thermodynamics), Materials science, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, 7. Clean energy, Energy storage, General Materials Science, Sensitivity (control systems), Process engineering, energy storage, business.industry, Mechanical Engineering, electrical properties, energy generation, energy storage, ionic conductor, 021001 nanoscience & nanotechnology, Condensed Matter Physics, ionic conductor, Durability, 0104 chemical sciences, Electricity generation, energy generation, Mechanics of Materials, electrical properties, Degradation (geology), Constant current, 0210 nano-technology, business, Voltage
Abstract

Solid Oxide Fuel Cells (SOFCs) are a promising technology that can provide efficient and clean energy production. The general barriers hindering their market entry are durability, i.e. resistance to aging, and costs. In parallel to the deeper insight into the different degradation sources and improved understanding of ageing factors and their interactions, work towards higher accuracy for the assessment and monitoring of real-world fuel cell ageing in necessary. The requirements for operational stability formulate the parameter “degradation rate” (DR). Most often long term durability tests are performed at constant current load and the decrease of the voltage is used for its definition. In this work a new approach based on analysis of the volt-ampere characteristics, named Differential Resistance Analysis (DRA), is presented. It operates with the differential resistance, i.e. with the derivative of the voltage in respect to the current (dU/dI = Rd) which is more sensitive to small deviations and thus increases the sensitivity of the analysis. Two performance indicators are derived (Rd, min and ∆U*) with differing selectivity: ∆U* is more sensitive to activation losses and Rd, min - to transport hindrances. The application of the DRA is demonstrated on examples from measurements in fuel cell and in reverse (fuel cell/electrolyzer) mode, as well as on modeling data. The results show that the method is at least 10 times more sensitive to DR evaluation in comparison with the classical approach.

Published
2017
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8. Degradation mechanism of La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ /Gd 0.1 Ce 0.9 O 2-δ composite electrode operated under solid oxide electrolysis and fuel cell conditions

Author

Alex Morata, Maxime Hubert, Sergii Pylypko, D. Ferreira Sanchez, Bertrand Morel, Dario Montinaro, E. Siebert, Jérôme Laurencin, María Fernanda Batista Morales, and F. Lefebvre-Joud

Subjects
Electrolysis, Electrolysis operation, Materials science, 020209 energy, General Chemical Engineering, Oxide, chemistry.chemical_element, 02 engineering and technology, 021001 nanoscience & nanotechnology, Oxygen, law.invention, chemistry.chemical_compound, chemistry, Chemical engineering, law, Composite electrode, 0202 electrical engineering, electronic engineering, information engineering, Electrochemistry, Fuel cells, 0210 nano-technology, Polarization (electrochemistry), Yttria-stabilized zirconia
Abstract

A set of long-term tests (t ≥ 1000 h) have been carried out in fuel cell and electrolysis modes on typical Ni-YSZ//YSZ//LSCF-CGO cells. The degradation rates were found to be higher in electrolysis than in fuel cell operation. Post-test analyses have revealed that Sr diffusion and formation of SrZrO3 at YSZ/CGO interface occur mainly during electrolysis operation, whereas the process is very limited in fuel cell mode. As a consequence, LSCF destabilization is found to be not involved in the degradation of cell performances during fuel cell operation while it could explain the highest degradation rates recorded in electrolysis mode. An in-house multi-scale model has been used to interpret the role of the cell operating mode on the LSCF demixing mechanism. The simulations have shown that the electrolysis operation leads to a strong depletion of oxygen vacancies in LSCF material (while the fuel cell condition results in an increase in the concentration of oxygen vacancies). It has been proposed that the depletion in oxygen vacancies under electrolysis polarization could drive the Sr release from the structure, and in turn, could explain the experimental results. Based on this proposition, a possible mechanism for the LSCF destabilization and SrZrO3 formation is detailed.

Published
2017
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9. Degradation of Ni-YSZ Electrodes in Solid Oxide Cells: Impact of Polarization and Initial Microstructure on the Ni Evolution

Author

F. Lefebvre-Joud, Dario Montinaro, Paolo Piccardo, Julien Vulliet, Jérôme Laurencin, Peter Cloetens, F. Monaco, J. P. Ouweltjes, Maxime Hubert, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), European Synchrotron Radiation Facility (ESRF), CEA Le Ripault (CEA Le Ripault), Direction des Applications Militaires (DAM), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), SOLIDPower SpA, Dipartimento di chimica e chimica industriale, Università di Genova, Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), and Università degli studi di Genova = University of Genoa (UniGe)

Subjects
Ni electrodes, Materials science, Renewable Energy, Sustainability and the Environment, 020209 energy, anodes, Oxide, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Microstructure, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, chemistry.chemical_compound, SOFC, Ni electrodes, anodes, Chemical engineering, chemistry, Electrode, 0202 electrical engineering, electronic engineering, information engineering, Materials Chemistry, Electrochemistry, SOFC, 0210 nano-technology, Polarization (electrochemistry), Yttria-stabilized zirconia
Abstract

International audience; Two types of solid oxide cells with different Ni-YSZ cermet microstructures have been aged in electrolysis and fuel cell modes for operating times ranging from 1000 to 15000 hours. The pristine and aged cermets have been reconstructed by synchrotron X-ray holotomography. Nickel agglomeration has been observed in the bulk of the operated samples inducing a significant loss of triple phase boundary lengths. The inspection of the microstructural properties has confirmed the stabilizing role of YSZ on Ni coarsening. Furthermore, the gradients of properties quantified at the electrolyte interface have revealed a depletion of Ni only in the electrochemically active region of the electrode. The process is strongly promoted for a coarse cermet microstructure when operated under electrolysis current. The evolution of the microstructural properties has been implemented in an in-house multiscale model. The simulations have shown that the loss of performance is dominated by the depletion of Ni in case of a coarse microstructure. Thanks to the computations, it has been shown that the Ni depletion is controlled by the cathodic overpotential. To explain this dependency, it has been proposed that the accumulation of oxygen vacancies in the double layer could deteriorate the Ni/YSZ interface and trigger the Ni depletion.

Published
2019

10. Stochastic Geometrical and Microstructural Modeling for Solid Oxide Cell Electrodes

Author

Johan Debayle, Peter Cloetens, Hamza Moussaoui, Yann Gavet, Jérôme Laurencin, Gérard Delette, Rakesh Sharma, Maxime Hubert, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), European Synchrotron Radiation Facility (ESRF), Laboratoire Georges Friedel (LGF-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Département Procédés de Mise en oeuvre des Milieux Granulaires (PMMG-ENSMSE), Centre Sciences des Processus Industriels et Naturels (SPIN-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Université Grenoble Alpes – CEA/LITEN, Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Laboratoire d’Innovation pour les Technologies des Energies nouvelles et les Nanomatériaux (LITEN), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), and Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Random field, Materials science, Oxide, Solid Oxide Cell Electrodes, 02 engineering and technology, Image Analysis, 021001 nanoscience & nanotechnology, Microstructure, Microstruture Characterization, chemistry.chemical_compound, Sphere packing, 020401 chemical engineering, chemistry, Stochastic Geometry, Electrode, Particle-size distribution, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, 0204 chemical engineering, Composite material, 0210 nano-technology, Porosity, Triple phase boundary
Abstract

Chapter 11: Cell, Stack, and System Modeling and Simulation; International audience; As it plays a key role on the performances and durability of solid oxide cells, the electrode microstructure has to be finely characterized and modelled. In this frame, a plurigaussian random field model and an original sphere packing algorithm have been developed to simulate a large variety of electrode microstructures. The two stochastic geometrical models have been validated on various electrode reconstructions obtained by synchrotron X-ray holotomography including the microstructures of thin functional layers and a thick current collector. Afterwards, semi-analytical microstructural correlations have been proposed and validated on a large dataset of representative synthetic microstructures. These equations allow establishing the links between the microstructural properties controlling the performances (Triple Phase Boundary lengths density and specific surface areas) to the ‘basic’ geometric attributes of the electrode (composition, porosity and particle size distribution). These correlations have been used to model the loss of active TPBl due to the Ni agglomeration.

Published
2019
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11. Improving the electrochemical performance of LaPrNiO4+δ as an oxygen electrode for intermediate temperature solid oxide cells by varying the architectural design

Author

Elisabeth Djurado, Jérôme Laurencin, Nur Istiqomah Khamidy, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Matériaux Interfaces ELectrochimie (MIEL ), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), and Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)

Subjects
Electrostatic spray deposition, Scanning electron microscope, General Chemical Engineering, Oxide, 02 engineering and technology, Electrolyte, 010402 general chemistry, Electrochemistry, 01 natural sciences, 7. Clean energy, Intermediate temperature solid oxide cell, Analytical Chemistry, law.invention, chemistry.chemical_compound, Oxygen electrode, law, [CHIM]Chemical Sciences, Polarization (electrochemistry), Clark electrode, Chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Dielectric spectroscopy, Chemical engineering, Electrode, 0210 nano-technology, Electrochemical impedance spectroscopy, Rare-earth nickelates
Abstract

International audience; Rare earth nickelate, LaPrNiO4+δ (LPNO), is one of the most suitable oxygen electrode materials for Intermediate Temperature Solid Oxide Cells (IT-SOC). By using Electrostatic Spray Deposition (ESD) and Screen Printing (SP), various architectural designs of electrodes are fabricated on Ce0.9Gd0.1O2-δ (GDC) electrolyte. Three electrode configurations are investigated based on a single Active Functional Layer (AFL), a double layer of the same composition which is an AFL topped by a current collecting layer (CCL) and a triple layer which is mainly the double layer with an LPNO/GDC composite interface. For each configuration, the electrode response and properties are analyzed by using Electrochemical Impedance Spectroscopy (EIS), X-ray diffraction and Scanning Electron Microscopy (SEM). The electrochemical properties are discussed as a function of the electrode design, microstructure, and composition with the presence of a higher order nickelate such as (La,Pr)3Ni2O7-δ. The electrochemical performance is enhanced thanks to better adhesion of the electrode onto the electrolyte, the presence of an LPNO/GDC composite interface, a more homogeneous distribution of fine grains, and a flatter electrode surface. A significant decrease in the polarization resistance (Rpol) is measured from 0.72, 0.50, and down to 0.20 Ω cm2 at 600 °C from single to triple layer, respectively.

Published
2019
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12. Reaction Mechanism and Impact of Microstructure on Performances for the LSCF‐CGO Composite Electrode in Solid Oxide Cells

Author

E. Effori, Gérard Delette, Johan Debayle, Rakesh Sharma, J. Vulliet, G. Si Larbi, F. Monaco, Hamza Moussaoui, L. Dessemond, Jérôme Laurencin, E. Siebert, Yann Gavet, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Matériaux Interfaces ELectrochimie (MIEL ), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Ecole Nationale Supérieure des Mines de St Etienne (ENSM ST-ETIENNE), Département Procédés de Mise en oeuvre des Milieux Granulaires (PMMG-ENSMSE), Centre Sciences des Processus Industriels et Naturels (SPIN-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Laboratoire Georges Friedel (LGF-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), CEA Le Ripault (CEA Le Ripault), Direction des Applications Militaires (DAM), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), and Ecole Nationale Supérieure des Mines de St Etienne

Subjects
Materials science, Working electrode, Renewable Energy, Sustainability and the Environment, 020209 energy, Composite number, Energy Engineering and Power Technology, 02 engineering and technology, 021001 nanoscience & nanotechnology, Microstructure, Dielectric spectroscopy, Electrode, 0202 electrical engineering, electronic engineering, information engineering, [CHIM]Chemical Sciences, Composite material, 0210 nano-technology, Polarization (electrochemistry), Porosity, Microscale chemistry
Abstract

International audience; The reaction mechanism and the impact of microstructure on performances for a porous LSCF‐CGO composite used as O2 electrode in SOCs have been investigated. For this purpose, an integrated approach coupling (i) electrochemical testing, (ii) advanced 3D characterizations, and (iii) modeling was proposed. In this frame, a symmetrical cell was tested in a three‐electrode setup and the microstructure of the LSCF‐CGO working electrode was reconstructed by FIB‐SEM tomography. The experimental polarization curves and the impedance diagrams along with the extracted microstructural parameters were used to validate an in‐house microscale electrochemical model. This model considers two parallel reaction pathways with (i) an oxidation/reduction at TPBls (surface path) and (ii) an oxygen transfer at the gas/LSCF interface (bulk path). It was shown that the LSCF‐CGO electrode reaction mechanism is mostly controlled by the charge transfer at TPBls whatever the polarization. Finally, the impact of electrode composition, porosity and particles size on the cell polarization resistance was investigated by using the electrochemical model in combination with a large dataset of synthetic microstructures generated by a geometrical stochastic model. The effect of each microstructural parameter on the electrode performance was analyzed in order to provide useful guidelines for the cell manufacturing.

Published
2019
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13. Cyclic voltammetry and high-frequency series resistance of La0.6Sr0.4Co0.2Fe0.8O3-δ electrode deposited on GDC : effect of the electrode microstructure and the oxygen partial pressure

Author

E. Siebert, V. Tezyk, Elisabeth Djurado, N. Sergent, C. Rossignol, Jérôme Laurencin, Matériaux Interfaces ELectrochimie (MIEL ), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), ARC-Nucleart CEA Grenoble (NUCLEART), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut National de L'Energie Solaire (INES), and Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)

Subjects
Materials science, General Chemical Engineering, LSCF/GDC interface, microstructure, Analytical chemistry, chemistry.chemical_element, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Oxygen, Electrochemistry, [CHIM]Chemical Sciences, Gadolinium-doped ceria, high-frequency series resistance, Partial pressure, Atmospheric temperature range, 021001 nanoscience & nanotechnology, Microstructure, oxygen partial pressure, cyclic voltammetry, 0104 chemical sciences, Dielectric spectroscopy, chemistry, Electrode, Cyclic voltammetry, 0210 nano-technology
Abstract

International audience; La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) electrode deposited on Gadolinium Doped Ceria (GDC) has been characterized by cyclic voltammetry and impedance spectroscopy in the temperature range of 300 to 700 °C. We demonstrate that the LSCF microstructure has a strong influence on the shape of the voltammograms and on the variation of the series resistance, Rs, measured on the impedance diagrams as a function of the dc bias. LSCF was deposited with two different microstructures, either porous layer (~10 μm thick) by screen-printing (SP) or almost dense layer (~2 μm thick) by Electrostatic Spray Deposition (ESD). For the denser film, one cathodic peak and one reverse anodic peak were evidenced under air at 300 and 500°C. The Rs value was also found to increase with the dc cathodic bias. On the contrary, no peak was observed with the porous film under the same conditions and Rs was independent on the applied potential from 300 to 700°C. Decreasing the oxygen partial pressure allowed the peaks to be evidenced and Rs to vary. The results are discussed in terms of oxygen exchange rate at the LSCF/gas interface, which depends on the LSCF specific surface area and the oxygen partial pressure.

Published
2019
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14. A 2D and 3D X-ray μ-diffraction and μ-fluorescence study of a mixed ionic electronic conductor

Author

Daniel Grolimund, Dario Ferreira Sanchez, Maxime Hubert, Pierre Bleuet, and Jérôme Laurencin

Subjects
Materials science, Renewable Energy, Sustainability and the Environment, Analytical chemistry, Oxide, Energy Engineering and Power Technology, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 01 natural sciences, Cathode, 0104 chemical sciences, law.invention, Barrier layer, chemistry.chemical_compound, Fuel Technology, Lanthanum strontium cobalt ferrite, chemistry, law, Solid oxide fuel cell, 0210 nano-technology, Layer (electronics), Yttria-stabilized zirconia, Gadolinium-doped ceria
Abstract

Due to the mixed ionic electronic conductive properties of the Lanthanum Strontium Cobalt Ferrite (LSCF) La0.6Sr0.4Co0.2Fe0.8O3−δ compound, it is of great scientific and technological interest. Especially in the Solid Oxide Fuel Cell (SOFC) technology, this compound has receiving great attention as a cathode material. However, its chemical reactivity with the Yttria-stabilized Zirconia (YSZ) electrolyte still remains one of the main challenges, which demands a comprehension in the μm and sub-μm range. In order to address the reactivity issues locally in the micrometre scale range, 2D and 3D X-ray μ-diffraction and μ-fluorescence analysis have been performed on a pristine LSCF cathode layer. The cathode was deposited on a dense YSZ electrolyte substrate spaced by a thin Gadolinium doped Ceria Oxide (CGO) barrier layer in between LSCF and YSZ to limit the reactivity. The present approach offers a larger field of view in comparison to electron microscopy techniques. The method can provide a more representative information and may offer some insights on the reactivity distribution along the interfaces. The formation of micro SrZrO3 inclusions in LSCF layer is then indubitably identified, as well as in the CGO/YSZ interface.

Published
2017
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15. State-of-the-Art Three-Dimensional Chemical Characterization of Solid Oxide Fuel Cell Using Focused Ion Beam Time-of-Flight Secondary Ion Mass Spectrometry Tomography

Author

Dario Montinaro, Jean-Paul Barnes, Agnieszka Priebe, Pierre Bleuet, Jérôme Laurencin, and Gael Goret

Subjects
010302 applied physics, Static secondary-ion mass spectrometry, Materials science, Analytical chemistry, 02 engineering and technology, 021001 nanoscience & nanotechnology, 01 natural sciences, Focused ion beam, Ion source, Secondary ion mass spectrometry, Time of flight, Ion beam deposition, Elemental analysis, 0103 physical sciences, Solid oxide fuel cell, 0210 nano-technology, Instrumentation
Abstract

In this paper the potential of time-of-flight secondary ion mass spectroscopy combined with focused ion beam technology to characterize the composition of a solid oxide fuel cell (SOFC) in three-dimension is demonstrated. The very high sensitivity of this method allows even very small amounts of elements/compounds to be detected and localized. Therefore, interlayer diffusion of elements between porous electrodes and presence of pollutants can be analyzed with a spatial resolution of the order of 100 nm. However, proper element recognition and mass interference still remain important issues. Here, we present a complete elemental analysis of the SOFC as well as techniques that help to validate the reliability of obtained results. A discussion on origins of probable artifacts is provided.

Published
2016
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16. 3D correlative morphological and elemental characterization of materials at the deep submicrometre scale

Author

Agnieszka Priebe, Jérôme Laurencin, Jean-Paul Barnes, Pierre Bleuet, Gael Goret, and G. Audoit

Subjects
010302 applied physics, Histology, Materials science, Nanotechnology, 02 engineering and technology, Orders of magnitude (numbers), 021001 nanoscience & nanotechnology, 01 natural sciences, Focused ion beam, Pathology and Forensic Medicine, Characterization (materials science), Secondary ion mass spectrometry, 0103 physical sciences, Nanometre, Sample preparation, Solid oxide fuel cell, 0210 nano-technology, Porosity
Abstract

This paper shows how X-ray computed nanotomography (CNT) can be correlated with focused ion beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) tomography on the same sample to investigate both the morphological and elemental structure. This methodology is applicable to relatively large specimens with dimensions of several tens of microns whilst maintaining a high spatial resolution of the order of 100 nm. However, combining X-ray CNT and FIB-TOF-SIMS tomography requires innovative sample preparation protocols to allow both experiments to be conducted on exactly the same sample without chemically or structurally modifying the sample between measurements. Moreover, dedicated algorithms have been developed for effective data fusion that is biased with nine degrees of freedom. This methodology has been tested using a porous and heterogeneous solid oxide fuel cell (SOFC) that has features varying in size by three orders of magnitude - from hundreds of nanometre large pores and grains to tens of micron wide functional layers.

Published
2016
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17. 3D geometrical characterization and modelling of solid oxide cells electrodes microstructure by image analysis

Author

Gérard Delette, Johan Debayle, Hamza Moussaoui, Yann Gavet, Peter Cloetens, Maxime Hubert, Jérôme Laurencin, Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire Georges Friedel (LGF-ENSMSE), Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Centre Sciences des Processus Industriels et Naturels (SPIN-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Département Procédés de Mise en oeuvre des Milieux Granulaires (PMMG-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), European Synchrotron Radiation Facility (ESRF), Chuo University, Hajime Nagahara, Kazunori Umeda, Atsushi Yamashita, Université Grenoble Alpes (France), LITEN-CEA, Grenoble (France), ESRF - The European Synchrotron (France), and Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)

Subjects
3D microstructuring, Materials science, Analytical chemistry, Oxide, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Tortuosity, Image analysis, law.invention, chemistry.chemical_compound, [INFO.INFO-TS]Computer Science [cs]/Signal and Image Processing, law, X-rays, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Composite material, Porosity, Tomography, Electrodes, Electrolysis, Synchrotron radiation, Modeling, [INFO.INFO-CV]Computer Science [cs]/Computer Vision and Pattern Recognition [cs.CV], Oxides, 021001 nanoscience & nanotechnology, Microstructure, 0104 chemical sciences, Characterization (materials science), Oxygen, chemistry, Electrode, 0210 nano-technology, Porous medium, Hydrogen
Abstract

Session 1:Image Analysis - SPIE : Society of Photo-Optical Instrumentation Engineers; International audience; A strong correlation exists between the performance of Solid Oxide Cells (SOCs), working either in fuel cell or electrolysis mode, and their electrodes microstructure. However, the basic relationships between the three-dimensional characteristics of the microstructure and the electrode properties are not still precisely understood. Thus, several studies have been recently proposed in an attempt to improve the knowledge of such relations, which are essential before optimizing the microstructure, and hence, designing more efficient SOC electrodes. In that frame, an original model has been adapted to generate virtual 3D microstructures of typical SOCs electrodes. Both the oxygen electrode, which is made of porous LSCF, and the hydrogen electrodes, made of porous Ni-YSZ, have been studied. In this work, the synthetic microstructures are generated by the so-called 3D Gaussian ‘Random Field model’. The morphological representativeness of the virtual porous media have been validated on real 3D electrode microstructures of a commercial cell, obtained by X-ray nano-tomography at the European Synchrotron Radiation Facility (ESRF). This validation step includes the comparison of the morphological parameters like the phase covariance function and granulometry as well as the physical parameters like the ‘apparent tortuosity’. Finally, this validated tool will be used, in forthcoming studies, to identify the optimal microstructure of SOCs.

Published
2017
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18. Effects of Pressure on High Temperature Steam and Carbon Dioxide Co-electrolysis

Author

Fabrice Mauvy, Guilhem Roux, Lucile Bernadet, Dario Montinaro, Jérôme Laurencin, Magali Reytier, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), SOLIDpower S.p.A., Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université de Bordeaux (UB), the European Union's Seventh Framework Programme (FP7/2007-2013) Fuel Cells and Hydrogen Joint Undertaking (FCH-JU-2013-1) under grant agreement n° 621173 (SOPHIA project). It has also received funding from European Horizon 2020 − Research and Innovation Framework Programme (H2020-JTI-FCH-2015-1) under grant agreement n° 699892 (ECO project). The work has also been partially supported by the 'Région Aquitaine'., and Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
020209 energy, General Chemical Engineering, Analytical chemistry, 02 engineering and technology, Electrochemistry, 7. Clean energy, Chemical reaction, Modelling, Methane, law.invention, Experiment, chemistry.chemical_compound, law, Mass transfer, Pressure, 0202 electrical engineering, electronic engineering, information engineering, Polarization (electrochemistry), Yttria-stabilized zirconia, Electrolysis, Chemistry, Co-electrolysis, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 13. Climate action, SOEC, 0210 nano-technology, Syngas
Abstract

International audience; Experiments have been performed in pressurized co-electrolysis mode at 800 °C on a typical Ni-YSZ//YSZ//CGO-LSCF cell. The polarization curves and the composition of the produced syngas have been measured at 1 bar and 10 bar. It has been found that the cell performances are improved under pressure at 1.3 V. The gas analyses have revealed that the methane formation is only activated under polarization and pressure. These experimental results have been used to validate a model which encompasses a chemical and electrochemical description of the co-electrolyser combined with a mass transport module. It has been found that the model is able to predict accurately the polarization curves as well as the syngas compositions at the cell outlet. Once validated, the model has been used to analyze the operating mechanisms in pressurized co-electrolysis. The impact of pressure on the mass transfer, the electrochemical and chemical reactions has been discussed. The close interaction between the electrochemical and chemical reactions for the internal production of CH4 has been specifically highlighted. Finally, operating maps have been computed at 10 bar from 700 °C to 800 °C. These simulations have shown that formation of CH4 in the co-electrolyser remains limited at 700 °C.

Published
2017
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19. Role of microstructure on electrode operating mechanisms for mixed ionic electronic conductors: From synchrotron-based 3D reconstruction to electrochemical modeling

Author

Maxime Hubert, J. C. da Silva, E. Siebert, Arata Nakajo, Peter Cloetens, Pierre Bleuet, F. Lefebvre-Joud, Jérôme Laurencin, Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), European Synchroton Radiation Facility [Grenoble] (ESRF), ARC-Nucleart CEA Grenoble (NUCLEART), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), 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), Ecole Polytechnique Fédérale de Lausanne (EPFL), Electrochimie Interfaciale et Procédés (EIP ), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), and Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])

Subjects
Materials science, 020209 energy, LSCF, Analytical chemistry, Synchrotron radiation, Impedance spectroscopy, 02 engineering and technology, Cathodic protection, law.invention, law, 0202 electrical engineering, electronic engineering, information engineering, General Materials Science, SOC, SOFC, Composite material, Polarization (electrochemistry), Tomography, LSCF-CGO, Modeling, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Microstructure, Synchrotron, Anode, Dielectric spectroscopy, Electrode, SOEC, 0210 nano-technology, [CHIM.OTHE]Chemical Sciences/Other
Abstract

A typical La0.6Sr0.4Co0.2Fe0.8O3-delta (LSCF) electrode was reconstructed by X-ray nanotomography. The new Nano Imaging beamline ID16A-NI of the European Synchrotron Radiation Facility (ESRF) was used to conduct the investigation. Particular attention was paid to prepare samples with a well-adapted shape for the tomographic experiments. The optimized sample preparation and new experimental set-up enables an improved spatial resolution of about 50 nm to be obtained in the electrode reconstruction of 51.2 x 25.6(2) x pi mu m(3). The LSCF microstructural properties were quantified in the 3D volume and used as input data in a dynamic micro scale electrochemical model. The numerical tool includes two parallel reaction pathways with an oxygen exchange at the LSCF/gas surface and a charge transfer at the electrode TPB. Electrochemical impedances were computed in the time domain at OCP, as well as under anodic and cathodic polarizations. Simulations allowed the microstructural parameters to be linked to the basic mechanisms of electrode operation according to the electrode polarization. A microstructural sensitivity analysis was performed on the single-phase LSCF and LSCF-CGO composite electrodes in order to identify the parameters that impact most the electrode response. It was found that the LSCF-CGO composite presents much higher performances compared to the LSCF single phase electrode especially in anodic polarization. (C) 2016 Elsevier B.V. All rights reserved.

Published
2016
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20. Overstoichiometric oxides Ln2NiO4+δ (Ln = La, Pr or Nd) as oxygen anodic electrodes for solid oxide electrolysis application

Author

Tiphaine Ogier, Fabrice Mauvy, Jérôme Laurencin, Julie Mougin, Jean-Claude Grenier, Jean-Marc Bassat, Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université de Bordeaux (UB), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), ANR-05-PANH-0019,SEMI EHT,Stacks Expérimentaux et Modules Innovants pour EHT(2005), ANR-09-HPAC-0005,FIDELHYO,FIabilisation De l'ELectrolYse de l'eau à haute température pour la production d'Hydrogène(2009), and Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Electrolysis, Materials science, Renewable Energy, Sustainability and the Environment, Non-blocking I/O, Inorganic chemistry, Oxide, Energy Engineering and Power Technology, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, Overpotential, 010402 general chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Electrochemistry, 01 natural sciences, 0104 chemical sciences, law.invention, chemistry.chemical_compound, Fuel Technology, chemistry, law, Electrode, 0210 nano-technology, Polarization (electrochemistry), Clark electrode
Abstract

Improving the oxygen electrode performances of the single solid oxide electrolysis cell (SOEC) is of peculiar interest as it contributes to a large extent to the cell polarization resistance. The present study focuses on alternative oxygen electrode materials: the oxygen overstoichiometric rare-earth nickelate oxides Ln 2 NiO 4+δ (Ln = La, Pr or Nd). Their electrochemical properties are measured on three-electrode symmetrical half-cells under zero dc conditions and under anodic polarization. The electrochemical characteristics are compared to those of the usual perovskite La 0.6 Sr 0.4 Fe 0.8 Co 0.2 O 3-δ (LSFC) electrode. Under polarization, in the temperature range from 600 °C to 800 °C, the Pr 2 NiO 4+δ -based cells exhibit the highest performances. At the same anodic overpotential of 0.15 V/Pt/air, the current densities measured through Pr 2 NiO 4+δ nickelate-based cells are more than ten times larger than those obtained with a cell based on LSCF. The modeling of the anodic overpotential phenomena (activation and concentration terms) occurring at the oxygen electrode is achieved and discussed.

Published
2015
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21. Influence of pressure on solid oxide electrolysis cells investigated by experimental and modeling approach

Author

Fabrice Mauvy, G. Gousseau, A. Chatroux, Jérôme Laurencin, Lucile Bernadet, Magali Reytier, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), the European Fuel Cells and Hydrogen Joint Undertaking (FCH-JU-2013-1) under grant agreement n° 621173 (SOPHIA project). Région Aquitaine, ANR-10-HPAC-0001,APHRODITE,Architecture sous Pression d'evHt à suRface de cOntact maximale et DIstribution par et à Travers l'Electrode.(2010), and Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université de Bordeaux (UB)

Subjects
Hydrogen, 020209 energy, High-pressure electrolysis, Analytical chemistry, Energy Engineering and Power Technology, Thermodynamics, chemistry.chemical_element, 02 engineering and technology, Pressure effects, Overpotential, 7. Clean energy, Electrolysis, law.invention, HTSE, law, 0202 electrical engineering, electronic engineering, information engineering, Solid oxide technology, Hydrogen production, Renewable Energy, Sustainability and the Environment, Chemistry, Limiting current, Modeling, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Fuel Technology, 13. Climate action, High-temperature electrolysis, SOEC, 0210 nano-technology, Polymer electrolyte membrane electrolysis
Abstract

International audience; For many industrial applications, hydrogen must be pressurized before being used or stored. Because compressing liquid water is less energetic than the first levels of gaseous H2 compression, High Temperature Steam Electrolysis (HTSE) performed under pressure might represent an advantageous way for hydrogen production. With the goal of improving the electrolysis efficiency, an experimental and modeling approach has been adopted in order to better understand the basic underlying mechanisms of pressurized electrolysis operation. Experiments were carried on two different single commercial solid oxide cells at 800 °C in the pressure range of 1–10 bar. As a first result, according to the i–V curves, two main pressure effects have been observed. First, as expected, the Open Circuit Voltage is higher under pressure. Then, the limiting current density is increased with increasing the pressure, meaning that the hydrogen production can be improved. The electrochemical model, which has been adjusted on the experimental i–V curves obtained at atmospheric conditions, has been validated for the pressurized operation. Simulations have shown that the improvement of the limiting current is related to the decrease of cathode's concentration overpotential with pressure. Moreover, an optimal pressure can be defined depending on the cell polarization. Higher pressures than the optimal one lead to slightly decrease the hydrogen production rate, mainly due to Open Circuit Voltage increase that cannot be balanced enough by the cathode's concentration overpotential decrease. Finally, this study demonstrates that cell performances under pressure are less sensitive to the variation of cermet-support microstructural properties.

Published
2015
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22. Direct comparison between X-ray nanotomography and scanning electron microscopy for the microstructure characterization of a solid oxide fuel cell anode

Author

Peter Cloetens, Romain Quey, Pierre Bleuet, Heikki Suhonen, Jérôme Laurencin, Centre Science des Matériaux et des Structures (SMS-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Laboratoire Georges Friedel (LGF-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), PMM-ENSMSE- Département Physique et Mécanique des Matériaux, European Synchrotron Radiation Facility (ESRF), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), 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), and Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-École des Mines de Saint-Étienne (Mines Saint-Étienne MSE)

Subjects
Materials science, Registration, Scanning electron microscope, 020209 energy, Analytical chemistry, 02 engineering and technology, Substrate (electronics), Spatial resolution 3D RECONSTRUCTION, [SPI]Engineering Sciences [physics], SUBSTRATE, TOMOGRAPHY, 0202 electrical engineering, electronic engineering, information engineering, General Materials Science, SOFC, Porosity, Image resolution, Mechanical Engineering, QUANTIFICATION, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Microstructure, Characterization (materials science), Anode, Mechanics of Materials, Solid oxide fuel cell, Microstructures, 0210 nano-technology
Abstract

International audience; X-ray computed nanotomography (nano-CT) and scanning electron microscopy (SEM) have been applied to characterize the microstructure of a Solid Oxide Fuel Cell (SOFC) anode. A direct comparison between the results of both methods is conducted on the same region of the microstructure to assess the spatial resolution of the nano-CT microstructure, SEM being taken as a reference. A registration procedure is proposed to find out the position of the SEM image within the nano-CT volume. It involves a second SEM observation, which is taken along an orthogonal direction and gives an estimate reference SEM image position, which is then refined by an automated optimization procedure. This enables an unbiased comparison between the cell porosity morphologies provided by both methods. In the present experiment, nano-CT is shown to underestimate the number of pores smaller than 1 mu m and overestimate the size of the pores larger than 1.5 mu m. (C) 2013 Elsevier Inc. All rights reserved.

Published
2013
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23. Characterisation of Solid Oxide Fuel Cell Ni-8YSZ substrate by synchrotron X-ray nano-tomography: from 3D reconstruction to microstructure quantification

Author

Heikki Suhonen, Romain Quey, Pierre Bleuet, Peter Cloetens, Gérard Delette, Jérôme Laurencin, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Centre Science des Matériaux et des Structures (SMS-ENSMSE), École des Mines de Saint-Étienne (Mines Saint-Étienne MSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Département Microstructures et Propriétés Mécaniques (MPM-ENSMSE), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-SMS, UMR 5146 - Laboratoire Claude Goux (LCG-ENSMSE), European Synchrotron Radiation Facility (ESRF), 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), CEA-Liten, 17 rue des martyrs, 38054 Grenoble Cedex 9, CEA-Leti, MINATEC Campus, France, European Synchrotron Radiation Facility, BP 220, and 38043 Grenoble

Subjects
Materials science, Tortuosity factor, Energy Engineering and Power Technology, 02 engineering and technology, Substrate (electronics), 010402 general chemistry, 01 natural sciences, Tortuosity, law.invention, [SPI.MAT]Engineering Sciences [physics]/Materials, law, Electrical and Electronic Engineering, Physical and Theoretical Chemistry, Composite material, Porosity, X-ray nano-tomography, Renewable Energy, Sustainability and the Environment, Isotropy, Ni-8YSZ, 021001 nanoscience & nanotechnology, Microstructure, Microstructure modelling, Synchrotron, 0104 chemical sciences, Anode, Crystallography, Solid oxide fuel cell, 0210 nano-technology, Solid Oxide Fuel Cell
Abstract

A methodology, based on synchrotron X-ray nano-tomography measurements, is proposed to obtain 3D reconstructions of porous supports for Solid Oxide Fuel Cell (SOFC). The methodology has been applied to investigate the microstructure of a typical Ni–8YSZ cermet substrate of an Anode Supported Cell (ASC). Experimental conditions have been optimised so that a 3D reconstruction of 42 μm × 42 μm × 105 μm has been computed with a voxel size of 60 nm. The 3D reconstruction has been numerically analysed showing a quasi isotropy over the medium. A special attention has been paid to compute the morphological properties controlling the gas diffusion through the support. In this frame, it has been found that a volume as large as 35 μm × 35 μm × 35 μm is required to be statistically representative for the whole substrate. More particularly, the tortuosity factor τ has been calculated on the basis of finite element simulations. The effect of the boundary conditions taken for these simulations has been investigated. In the direction perpendicular to the anode/electrolyte interface, the tortuosity factor has been determined to τ z = 2.8 − 0.2 + 0.3 .

Published
2012
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24. Modelling of solid oxide steam electrolyser Impact of the operating conditions on hydrogen production

Author

D. Kane, Florence Lefebvre-Joud, Jérôme Laurencin, Jonathan Deseure, Gérard Delette, Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), European Project: 213009,EC:FP7:ENERGY,FP7-ENERGY-2007-1-RTD,RELHY(2008), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), and Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Exothermic reaction, Convective heat transfer, Electrolytic cell, 020209 energy, Analytical chemistry, Energy Engineering and Power Technology, Thermodynamics, 02 engineering and technology, Electrolyte, Overpotential, 7. Clean energy, Modelling, law.invention, [CHIM.GENI]Chemical Sciences/Chemical engineering, law, 0202 electrical engineering, electronic engineering, information engineering, Electrochemistry, Thermal analysis, Electrical and Electronic Engineering, Physical and Theoretical Chemistry, Hydrogen production, Renewable Energy, Sustainability and the Environment, Chemistry, Solid Oxide Electrolysis Cell (SOEC), 021001 nanoscience & nanotechnology, Cathode, Anode, 0210 nano-technology
Abstract

International audience; A 2D multi-physic in-house-model has been developed to analyse the performances of Solid Oxide Electrolysis Cell (SOEC) stack This model encompasses a combined electrochemical and thermal description of the electrolyser An analytical solution for multi-species diffusion across the porous cathode has been implemented in the model This numerical tool is useful to provide all the important parameters of the stack operation distribution of temperature heat fluxes local current densities gas concentrations and overpotentials Simulations show that thermal equilibrium of the stack is strongly dependant on radiative heat losses whereas convective heat transfers are limited In the exothermic operation mode the cell warming depends on the radiation efficiency A parametric study has been carried out to analyse SOEC irreversible losses It is found that the anode activation overpotential is significant whereas the polarisation due to the cathode activation remains much more limited Anode concentration overpotentials are found to be insignificant whatever the operating condition Cathode concentration overpotentials are found to be moderate in the case of Electrolyte Supported Cell (ESC) while they can increase drastically with current density in the case of Cathode Supported Cell (CSC) Addition of diluent gases into the H(2) H(2)O mixture is found to increase the concentration overpotentials

Published
2011
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25. Strength of Highly Porous Ceramic Electrodes

Author

Gérard Delette, Xiaoxing Liu, Christrophe L. Martin, Jérôme Laurencin, Didier Bouvard, Stéphane Di Iorio, Science et Ingénierie des Matériaux et Procédés (SIMaP), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
010302 applied physics, Length scale, Materials science, Tension (physics), Oxide, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Compression (physics), Microstructure, 01 natural sciences, chemistry.chemical_compound, chemistry, visual_art, 0103 physical sciences, Materials Chemistry, Ceramics and Composites, visual_art.visual_art_medium, Fracture (geology), Ceramic, Particle size, Composite material, 0210 nano-technology
Abstract

International audience; Highly porous ceramics are critical components of Solid Oxide Fuel Cells. Nevertheless, their mechanical properties are poor and not fully understood. Herein, Discrete Element simulations are used to quantitatively assess the relation between the particulate microstructure of highly porous ceramics and their mechanical properties. Partially sintered ceramics are numerically generated with complex microstructures including pore formers and bilayers. These microstructures are then tested in tension and compression to obtain their elastic and fracture behavior. Compiling experimental data from the literature and simulations results, an Orowan-Petch type relation between strength and particle size is proposed for highly porous ceramics. It is based on the local fracture model at the length scale of solid bonds between sintered particles.

Published
2011
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26. Microstructure of porous composite electrodes generated by the discrete element method

Author

Thibaud Delahaye, Gérard Delette, Christophe L. Martin, Jérôme Laurencin, Didier Bouvard, Xiaoxing Liu, Science et Ingénierie des Matériaux et Procédés (SIMaP), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Renewable Energy, Sustainability and the Environment, Metallurgy, Non-blocking I/O, Composite number, Energy Engineering and Power Technology, Sintering, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, Microstructure, 01 natural sciences, Discrete element method, 0104 chemical sciences, Percolation, Particle, Electrical and Electronic Engineering, Physical and Theoretical Chemistry, Composite material, 0210 nano-technology, Triple phase boundary
Abstract

International audience; Typical microstructures of LSM/YSZ NiO/YSZ Ni/YSZ composite electrodes are simulated by the discrete element method The numerical microstructures are generated by taking into account in a realistic manner the sintering process This allows complex microstructures such as Mayers or microstructures containing pore formers to be obtained NiO particles in the NiO/YSZ composite electrodes are reduced to Ni Reduction is carried out with the discrete element formalism which allows particle rearrangement to be taken Into account We show that the mechanical percolation of the YSZ phase plays an important role during the reduction of NiO The various numerical microstructures generated by sintering and reduction are analyzed to evaluate important microstructural features such as macroscopic porosity pore surface area and Triple Phase Boundary length (c) 2010 Elsevier BV All rights reserved

Published
2011
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27. Solid Oxide Fuel Cells damage mechanisms due to Ni-YSZ re-oxidation: Case of the Anode Supported Cell

Author

Bertrand Morel, M. Dupeux, Jérôme Laurencin, Gérard Delette, Florence Lefebvre-Joud, Laboratoire Essais et Validations (LEV), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Science et Ingénierie des Matériaux et Procédés (SIMaP), and Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Hydrogen, cracking, Oxide, Energy Engineering and Power Technology, chemistry.chemical_element, Impedance spectroscopy, reduction, 02 engineering and technology, Electrolyte, coatings, 010402 general chemistry, 01 natural sciences, Redox, [SPI.MAT]Engineering Sciences [physics]/Materials, chemistry.chemical_compound, microstructural characterization, SOFC, Cermet Ni-YSZ, Electrical and Electronic Engineering, Physical and Theoretical Chemistry, sofc anodes, redox behavior, cermet, degradation, Renewable Energy, Sustainability and the Environment, Cermet, [CHIM.MATE]Chemical Sciences/Material chemistry, electrode, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Dielectric spectroscopy, Anode, chemistry, Chemical engineering, Re-oxidation, Solid oxide fuel cell, 0210 nano-technology, zirconia
Abstract

International audience; The effects of Ni-YSZ cermet re-oxidation in anode supported Solid Oxide Fuel Cells (SOFCs) have been investigated. Damage mechanisms have been studied in both cases of direct oxidation in air (i.e., fuel shutdown) or by an ionic current (i.e., fuel starvation). Direct oxidation tests show that the electrolyte cracks for a conversion degree of Ni into NiO ranging between similar to 58 and similar to 71%. This failure mode has been modelled considering both the bulk expansion of the cermet induced by the transformation of the Ni phase and the change of mechanical stresses in the multilayered cell. In the case of fuel starvation, a thin layer of the cermet was electrochemically re-oxidised at 800 degrees C and then reduced under a hydrogen stream. This 'redox' cycle was repeated until the degradation of the cell. The evolution of the impedance diagrams recorded after each cycle suggests that the cermet damages in an area close to anode/electrolyte interface. The mechanical modelling states that a delamination can occur along the interface between the Anode Functional Layer(AFL) and the Anode Current Collector (ACC) substrate. This theoretical result confirms the experimental trends observed by impedance spectroscopy. (C) 2009 Elsevier B.V. All rights reserved.

Published
2009
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28. Electrode kinetics of porous Ni-3YSZ cermet operated in fuel cell and electrolysis modes for solid oxide cell application

Author

Bertrand Morel, Dario Montinaro, Elisabeth Djurado, Jérôme Laurencin, Maxime Hubert, E. Effori, E. Siebert, Gregory Geneste, F. Monaco, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), ESRF-The European Synchrotron, Matériaux Interfaces ELectrochimie (MIEL), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI), Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA), SOLIDPower SpA, and European Synchroton Radiation Facility [Grenoble] (ESRF)

Subjects
Electrolysis, Materials science, General Chemical Engineering, Limiting current, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, Electrochemistry, 7. Clean energy, 01 natural sciences, 0104 chemical sciences, Anode, law.invention, Chemical engineering, law, Electrode, Hydrogen spillover, 0210 nano-technology, Triple phase boundary, Polarization (electrochemistry)
Abstract

International audience; The electrochemical reactions of hydrogen oxidation and steam reduction have been investigated for a porous cermet electrode made of Ni and 3YSZ. The electrochemical characterizations have been performed over a large range of gas compositions at 700°C. It has been shown that the fuel electrode response is activated by the potential under anodic current while a limiting current density appears under cathodic polarization. Moreover, the impedance diagrams exhibit a shape representative of a kind of finite-length Gerischer element with a low-frequency contribution sensitive to the steam content. To interpret these experimental results, a continuous dynamic model has been developed by describing the mass and charge transfers within the electrode. The reaction has been divided into a sequence of elementary steps considering two scenarios of charge transfer based on the oxygen and hydrogen spillover mechanisms. Three-dimensional reconstructions obtained by synchrotron X-ray nano-holotomography have been used to provide the cermet structural properties for the simulations. The numerical computations have shown that the hydrogen spillover scenario is the most appropriate mechanism to reproduce correctly the experiments. Besides, the electrode response is controlled by the charge transfer at triple phase boundary lengths, the oxygen vacancies migration in the 3YSZ network and a pure chemical surface process depending on the polarization. In fuel cell mode, desorption of water molecules from 3YSZ would co-limit the electrode response, while in electrolysis mode, the steam adsorption on Ni would become one of the rate determining steps. Finally, a sensitivity analysis has shown that surface diffusion would also play a key role in the electrode response.

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