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9. In Situ Synthesis of MXene with Tunable Morphology by Electrochemical Etching of MAX Phase Prepared in Molten Salt.

Author

Liu, Liyuan, Zschiesche, Hannes, Antonietti, Markus, Gibilaro, Mathieu, Chamelot, Pierre, Massot, Laurent, Rozier, Patrick, Taberna, Pierre‐Louis, and Simon, Patrice

Subjects
FUSED salts, TRANSITION metal carbides, ETCHING, ENERGY storage, CARBON nanotubes, OXIDATION-reduction reaction, GRAPHENE oxide, ANODES
Abstract

MXenes, a rapidly growing family of 2D transition metal carbides, carbonitrides, and nitrides, are one of the most promising high‐rate electrode materials for energy storage. Despite the significant progress achieved, the MXene synthesis process is still burdensome, involving several procedures including preparation of MAX, etching of MAX to MXene, and delamination. Here, a one‐pot molten salt electrochemical etching (E) method is proposed to achieve Ti2C MXene directly from elemental substances (Ti, Al, and C), which greatly simplifies the preparation process. In this work, different carbon sources, such as carbon nanotubes (CNT) and reduced graphene oxide (rGO), are reacted with Ti and Al micro‐powders to prepare Ti2AlC MAX with 1D and 2D tuned morphology followed by in situ electrochemical etching from Ti2AlC MAX to Ti2CTx MXene in low‐cost LiCl‐KCl. The introduction of the O surface group via further ammonium persulfate (APS) treatment can act in concert with Cl termination to activate the pseudocapacitive redox reaction of Ti2CClyOz in the non‐aqueous electrolyte, resulting in a Li+ storage capacity of up to 857 C g−1 (240 mAh g−1) with a high rate (86 mAh g−1 at 120 C) capability, which makes it promising for use as an anode material for fast‐charging batteries or hybrid devices in a non‐aqueous energy storage application. [ABSTRACT FROM AUTHOR]

Published
2023
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10. Tuning the Surface Chemistry of MXene to Improve Energy Storage: Example of Nitrification by Salt Melt.

Author

Liu, Liyuan, Zschiesche, Hannes, Antonietti, Markus, Daffos, Barbara, Tarakina, Nadezda V., Gibilaro, Mathieu, Chamelot, Pierre, Massot, Laurent, Duployer, Benjamin, Taberna, Pierre‐Louis, and Simon, Patrice

Subjects
SURFACE chemistry, NITRIFICATION, SURFACE conductivity, ELECTRIC conductivity, FUSED salts, IRON chlorides, AQUEOUS electrolytes, ENERGY storage
Abstract

The unique properties of 2D MXenes, such as metal‐like electrical conductivity and versatile surface chemistry, make them appealing for various applications, including energy storage. While surface terminations of 2D MXene are expected to have a key influence on their electrochemical properties, the conventional HF‐etching method limits the surface functional groups to F, OH, and O. In this study, O‐free, Cl‐terminated MXenes (noted as Ti3C2Clx) are first synthesized by a molten salt (FeCl2) etching route. Then, a substitution of surface termination from Cl to N is performed via post‐thermal treatment of Ti3C2Clx in Li3N containing molten salt electrolytes. While the Cl‐terminated pristine material does not show electrochemical activity, the surface‐modified, N‐containing Ti3C2Tx exhibits a unique capacitive‐like electrochemical signature in sulfuric acid aqueous electrolyte with rate performance—more than 300 F g−1 (84 mAh g−1) at 2 V s−1. These results show that control of the MXene surface chemistry enables the preparation of high‐performance electrodes in a previously not accessed limit of energy storage. [ABSTRACT FROM AUTHOR]

Published
2023
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11. Isru taskforce in Toulouse toward in situ autonomous electrochemical and additive manufacturing processes of lunar

Author

Gibilaro, Mathieu, MASSOT, Laurent, Chiron, Christelle, Chamelot, Pierre, Favier, Jean-Jacques, Cutard, Thierry, Le Maoult, Yannick, Sentenac, Thierry, Pinet, P.C., Chevrel, S, Institut de recherche en astrophysique et planétologie (IRAP), Institut national des sciences de l'Univers (INSU - CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Observatoire Midi-Pyrénées (OMP), Météo France-Centre National d'Études Spatiales [Toulouse] (CNES)-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Météo France-Centre National d'Études Spatiales [Toulouse] (CNES)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), IMT École nationale supérieure des Mines d'Albi-Carmaux (IMT Mines Albi), Institut Mines-Télécom [Paris] (IMT), Institut Clément Ader (ICA), Institut Supérieur de l'Aéronautique et de l'Espace (ISAE-SUPAERO)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-IMT École nationale supérieure des Mines d'Albi-Carmaux (IMT Mines Albi), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut national des sciences de l'Univers (INSU - CNRS)-Observatoire Midi-Pyrénées (OMP), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université de Toulouse (UT)-Université de Toulouse (UT)-Institut national des sciences de l'Univers (INSU - CNRS)-Centre National d'Études Spatiales [Toulouse] (CNES)-Centre National de la Recherche Scientifique (CNRS)-Météo-France -Institut de Recherche pour le Développement (IRD)-Institut national des sciences de l'Univers (INSU - CNRS)-Centre National d'Études Spatiales [Toulouse] (CNES)-Centre National de la Recherche Scientifique (CNRS)-Météo-France -Centre National de la Recherche Scientifique (CNRS)

Subjects
[SPI]Engineering Sciences [physics], [SDU]Sciences of the Universe [physics], ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2021

12. Thermodynamic properties of CaCl$_2$-CaF$_2$-CaO System: Phase diagram investigation

Author

Claquesin, Julien, Gibilaro, Mathieu, Massot, Laurent, Lemoine, Olivier, Bourges, Gilles, Chamelot, Pierre, Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), VALDUC (DAM/VALDUC), Direction des Applications Militaires (DAM), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)

Subjects
Calcium Chloride, Calcium Fluoride, [SPI]Engineering Sciences [physics], Ternary System, Phase Diagram, [CHIM]Chemical Sciences, Differential Scanning Calorimetry (DSC), Calcium Oxide
Abstract

International audience; The CaCl$_2$-CaF$_2$-CaO phase diagram was investigated in the CaO low region (

Published
2021

13. Evaluation of Nitrogen Influence on the Uranium Metal Stability in LiCl-KCl

Author

Caretero, Théo, Massot, Laurent, Gibilaro, Mathieu, De Marco, Jérémie, Arab, Mehdi, Chiron, Christelle, and Chamelot, Pierre

Abstract

This study is focused on nitrogen influence on the uranium metal stability in molten eutectic LiCl-KCl (58.2–41.8 mol.%) in the 450 °C–550 °C temperature range. Preliminary study showed that nitrogen is soluble and electroactive in LiCl-KCl. Then, experiments were done by immersing an uranium plate in LiCl-KCl under two different atmospheres: a low nitrogen atmosphere and a saturated nitrogen one. It was found that uranium spontaneously reacts with nitrogen to form U(III) and N3-. The kinetics of this reaction was determined by monitoring the U(III) formation rate using chronopotentiometry. It appeared that increasing the temperature or the nitrogen partial pressure in the atmosphere leads to a faster uranium oxidation rate.

Published
2024
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14. Contributors

Author

Allen, T.R., primary, Bauer, Thomas, additional, Bayer, Michael, additional, Beneš, O., additional, Bessada, Catherine, additional, Boghosian, Soghomon, additional, Briot, E., additional, Brousse, T., additional, Cassir, Michel, additional, Chamelot, Pierre, additional, Chavanne, Hervé, additional, Chien, Andrew C., additional, Claux, Benoit, additional, Daffos, B., additional, Delpech, Sylvie, additional, Dustmann, Cord-Henrich, additional, Eck, Markus, additional, Fehrmann, Rasmus, additional, Gibilaro, Mathieu, additional, Glatz, Jean-Paul, additional, Goto, Takuya, additional, Groult, Henri, additional, Hagiwara, Rika, additional, Hartenbach, Akane, additional, Irvine, John T.S., additional, Ito, Yasuhiko, additional, Iwadate, Yasuhiko, additional, Julien, C.M., additional, Kado, Yuya, additional, Kadoma, Y., additional, Kaesche, Stefanie, additional, Kawase, M., additional, Komaba, S., additional, Konings, R.J.M., additional, Kumagai, N., additional, Kuznetsov, S.A., additional, Laing, Doerte, additional, Lair, Virginie, additional, Lantelme, Frédéric, additional, Le Van, K., additional, Madden, P.A., additional, Magdinier, Pierre-Louis, additional, Malmbeck, Rikard, additional, Massot, Laurent, additional, Maurin-Perrier, Philippe, additional, Meier, Roland, additional, Monteux, Vincent, additional, Mosqueda, Hugo, additional, Murakami, Tsuyoshi, additional, Nishikiori, Tokujiro, additional, Nohira, Toshiyuki, additional, Ohtori, N., additional, Okada, Isao, additional, Ougier, Michel, additional, Pfleger, Nicole, additional, Ringuedé, Armelle, additional, Rollet, Anne-Laure, additional, Salanne, M., additional, Sato, Yuzuru, additional, Simon, C., additional, Simon, P., additional, Souček, Pavel, additional, Sridharan, K., additional, Steinmann, Wolf-Dieter, additional, Takeda, Osamu, additional, Tasaka, Akimasa, additional, Taxil, Pierre, additional, Tokushige, Manabu, additional, Turq, P., additional, Wang, Dihua, additional, Xiao, Wei, additional, and Yoshioka, Ritsuo, additional

Published
2013
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16. Zirconium(IV) electrochemical behavior and electrorefining in molten fluoride salts

Author

Quaranta, D., Mendes, E., Massot, Laurent, Gibilaro, Mathieu, Serp, J., CEA-Direction des Energies (ex-Direction de l'Energie Nucléaire) (CEA-DES (ex-DEN)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), CADARACHE, Bibliothèque, Laboratoire de génie chimique [ancien site de Basso-Cambo] (LGC), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS.NUCL] Physics [physics]/Nuclear Theory [nucl-th], [PHYS.NUCL]Physics [physics]/Nuclear Theory [nucl-th], [PHYS.NEXP] Physics [physics]/Nuclear Experiment [nucl-ex], Recycling, Zirconium, [PHYS.NEXP]Physics [physics]/Nuclear Experiment [nucl-ex], Pyroprocessing, molten fluorides
Abstract

International audience; Zirconium is a strategic metal used in various activity sectors and particularly for nuclear applications because of its physicochemical properties a low cross-section of neutron capture, corrosion resistance under extreme conditions (high temperature, aggressive media), excellent mechanical resistance and high pyrophoricity. Thus 90% of the production of zirconium metal is used in the nuclear field, as zirconium alloy claddings, UZr fuel, and dissolvers used for spent fuel reprocessing. Zirconium metal is commonly obtained in the form of zirconium sponges produced by Kroll process that consists in a chemical reduction of zirconium chlorides to zirconium metal. On the other hand, spent zircaloy claddings represent a consequent amount of zirconium considered nowadays as a waste. There could be an economic interest to recycle the irradiated zircaloy claddings in order to valorize Zr for further reuse within nuclear applications.One promising zircaloy recycling process consists of electrorefining in molten salt media. Although chloride salts seem not suitable to operate such process, mainly because of the several stable oxidation states of Zr coexisting in these media, the use of fluoride systems should stabilize Zr oxidation state as Zr$^{4+}$. A first step consists in investigating the feasibility of the electrochemical recovery of Zr metal in fluoride media. Thus, the present work focused on the electrochemical behavior study of zirconium in molten fluoride using transient electroanalytical techniques, e.g. Cyclic voltammetry, square wave voltammetry, and chronopotentiometry. These different technics allowed to understand the Zirconium reduction mechanism by determining the number of exchanged electrons and assessed the thermodynamic properties of Zr in the salt (diffusion coefficient, etc.). Zirconium electrocrystallisation process was also investigated by chronoamperometry and cyclic voltammetry. This set of data is of first importance in order to estimate the further potentialities of the process

Published
2018

17. X-ray imaging of High Temperature furnace applied to glass melting

Author

Boloré, Damien, Gibilaro, Mathieu, Massot, Laurent, Chamelot, Pierre, Cid, Emmanuel, Masbernat, Olivier, Pigeonneau, Franck, Centre de Mise en Forme des Matériaux (CEMEF), MINES ParisTech - École nationale supérieure des mines de Paris, Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Centre National de la Recherche Scientifique (CNRS), Surface du Verre et Interfaces (SVI), Université Pierre et Marie Curie - Paris 6 (UPMC)-SAINT-GOBAIN-Centre National de la Recherche Scientifique (CNRS), Laboratoire de génie chimique [ancien site de Basso-Cambo] (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, and Institut de mécanique des fluides de Toulouse (IMFT)

Subjects
[PHYS.PHYS.PHYS-FLU-DYN]Physics [physics]/Physics [physics]/Fluid Dynamics [physics.flu-dyn], [SPI.FLUID]Engineering Sciences [physics]/Reactive fluid environment, [PHYS.MPHY]Physics [physics]/Mathematical Physics [math-ph], [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018

18. Etudes de voies potentielles pour le recyclage du zirconium des gaines en Zircaloy des combustibles uses

Author

Quaranta, D., Mendes, E., Massot, Laurent, Gibilaro, Mathieu, Chamelot, Pierre, Serp, J., CADARACHE, Bibliothèque, CEA-Direction des Energies (ex-Direction de l'Energie Nucléaire) (CEA-DES (ex-DEN)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS.NUCL] Physics [physics]/Nuclear Theory [nucl-th], [PHYS.NUCL]Physics [physics]/Nuclear Theory [nucl-th], [PHYS.NEXP] Physics [physics]/Nuclear Experiment [nucl-ex], [PHYS.NEXP]Physics [physics]/Nuclear Experiment [nucl-ex], ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2018

22. French R&D Activities Progress Summary, GIF MSR

Author

MERLE, Elsa, Allibert, Michel, Gerardin, Delphine, Heuer, Daniel, Laureau, Axel, Martinet, Johann, Delpech, Sylvie, Duran, Gabriela, Rodrigues, David, Giot, Lydie, Chamelot, Pierre, Gibilaro, Mathieu, Massot, Laurent, Laboratoire de Physique Subatomique et de Cosmologie (LPSC), Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Centre National de la Recherche Scientifique (CNRS), Institut de Physique Nucléaire d'Orsay (IPNO), Centre National de la Recherche Scientifique (CNRS)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université Paris-Sud - Paris 11 (UP11), Laboratoire de physique subatomique et des technologies associées (SUBATECH), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-IMT Atlantique Bretagne-Pays de la Loire (IMT Atlantique), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Laboratoire de génie chimique [ancien site de Basso-Cambo] (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées

Subjects
[PHYS]Physics [physics], ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2017

23. X‐ray imaging of a high‐temperature furnace applied to glass melting.

Author

Boloré, Damien, Gibilaro, Mathieu, Massot, Laurent, Chamelot, Pierre, Cid, Emmanuel, Masbernat, Olivier, and Pigeonneau, Franck

Subjects
X-ray imaging, GLASS furnaces, MOLTEN glass, OPTICAL flow, STANNIC oxide, GRANULAR materials
Abstract

The dynamics of soda‐lime‐silica glass grain melting is investigated experimentally using a nonintrusive technique. A cylindrical alumina crucible is filled with glass cullet and placed into a furnace illuminated by an X‐ray source. This glass granular bed is gradually heated up to 1100°C, leading to its melting and the generation of a size‐distributed population of bubbles rising in the molten glass. An image processing algorithm of X‐ray images of the cullet bed during melting allows the characterization of bubbles size distribution in the crucible as well as their velocity. The introduction of tin dioxide μ‐particles in the glass matrix before melting enhances the texture of the images and makes possible the determination of the bubble‐induced molten glass velocity field by an optical flow technique. The bubble size distribution can be fitted by a log‐normal law, suggesting that it is closely related to the initial size distribution in the cullet bed. The liquid motion induced by the bubbles in Stokes' regime is strongly affected by the flow confinement and the determination of bubble rising velocity along its trajectory unveils the existence of local tiny temperature fluctuations in the crucible. Overall, the measuring techniques developed in this work seem to be very promising for the improvement of models and optimization of industrial glass furnaces. [ABSTRACT FROM AUTHOR]

Published
2020
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26. Method for recovering elemental silicon from cutting remains

Author

Ulset, Torgeir, Julrud, Stein, Cassayre, Laurent, Chamelot, Pierre, Massot, Laurent, Taxil, Pierre, Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Renewable Energy Corporation - REC-Group (NORWAY), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Centre National de la Recherche Scientifique - CNRS (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Silicon, Génie chimique
Abstract

This invention relates to a method for recovering elemental silicon cutting remains containing silicon particles, wherein the method comprises manufacturing solid anodes from the cutting remains, arranging one or more manufactured anode (s) in an electrolytic cell with a molten salt electrolyte and one or more cathode (s), and applying a potential difference between the one or more anode (s) and cathode (s) to obtain an oxidation of metallic silicon in the one or more anode (s), transportation of dissolved silicon in the electrolyte, and reduction of the dissolved silicon to a metallic phase at the one or more cathode (s).

Published
2008

27. Comparison between Derived Sol-Gel and conventional methods for the preparation of Dimensionally Stable Ta/IrO2 Anodes for oxygen evolution

Author

Massot, Laurent, Palau, Patrice, Savall, André, Taxil, Pierre, Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), and Centre National de la Recherche Scientifique - CNRS (FRANCE)

Subjects
Sol-Gel, DSA®, Génie chimique, Tantalum, Oxygen evolution, Iridium dioxide
Abstract

The elaboration of inert anodes suitable for oxygen evolution in acidic media was investigated. These electrodes are formed of a tantalum substrate covered by a catalyst layer of iridium oxide IrO2. In this work, the catalyst coating was obtained by thermal decomposition of coating solutions prepared by two methods: (1) the derived Sol-Gel method using iridium acetylacetonate ([CH3COCH=C(O)CH3]3Ir) dissolved in an isopropanol – acetic acid mixture and (2) the classic method which uses a solution of iridium tetrachloride dissolved in a ethanol – isopropanol mixture. These electrodes were characterised by electrochemical and physical techniques. The use of the derived Sol-Gel method for the preparation of Ta/IrO2 electrodes yields very active electrocatalytic layer, such an electrocatalytic coating may be expected to be used for short time electrolysis runs with high rates of production.

Published
2007

29. Thermodynamic Properties Determination in LiF-CaF2 Using Electrochemistry in High Temperature Fused Salts: Application to CeF3

Author

Gibilaro, Mathieu, Massot, Laurent, and Chamelot, Pierre

Abstract

Combining thermodynamic database and electrochemical measurements, CeF3 thermodynamics properties were determined between 1113K and 1233K in LiF-CaF2 solution. First, standard potentials of CeF3/Ce were calculated in different reference states: liquid and solid, and infinite dilution. Then activity coefficients of CeF3 were estimated in the different reference states and for different composition scales: molarity, molality and molar fraction. Finally, constants which interconnected the infinite dilution reference state and the solid and liquid reference states were evaluated.

Published
2017

33. Cyclic Voltammetric Experiment - Simulation Comparisons of the Complex Mechanism Associated with Electrochemical Reduction of Zr4+ in LiCI-KCI Eutectic Molten Salt.

Author

Fabian, Cesimiro P., Luca, Vittorio, Le, Thanh H., Bond, Alan M., Chamelot, Pierre, Massot, Laurent, Caravaca, Conception, Hanley, Tracey L., and Lumpkin, Gregory R.

Subjects
NUCLEAR energy, ZIRCONIUM, ELECTROCHEMICAL analysis, EUTECTICS, SOLID solutions
Abstract

Nuclear energy increasingly represents an important option for generating largely clean CO2-free electricity and zirconium is a fission product that is expected to be present in irradiated fuels. The present investigation addresses the electrochemical reduction of Zr4+ to Zr0 in LiCl - KCl eutectic molten salt in the temperature range 425-550 °C using cyclic voltammetry (CV), square-wave voltammetry (SWV) and bulk electrolysis. Simulations of the CV data indicate that the initial reduction proceeds through surface confined steps: Zr4+*+ 2e- ↔ Zr2+* and Zr2+* + 2e-↔ Zr* processes (* adsorbed species) followed by a peak-shaped complex diffusion controlled step that consists of a combination of closely spaced processes associated with the reactions Zr4+ + 4e- ↔ Zr0 and Zr4+ + 3e- ↔ Zr2+, probably in the form of ZrCI* is then further ↔ reduced to Zr0* at even more negative potentials. The simulations provide the first quantitative analysis of the thermodynamics and kinetics of the Zr4+ reduction in the LiCI-KCI eutectic. [ABSTRACT FROM AUTHOR]

Published
2013
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34. Cyclic Voltammetric Experiment - Simulation Comparisons of the Complex Mechanism Associated with Electrochemical Reduction of Zr4+ in LiCl-KCl Eutectic Molten Salt

Author

Fabian, Cesimiro P., Luca, Vittorio, Le, Thanh H., Bond, Alan M., Chamelot, Pierre, Massot, Laurent, Caravaca, Concepcion, Hanley, Tracey L., and Lumpkin, Gregory R.

Abstract

Nuclear energy increasingly represents an important option for generating largely clean CO2-free electricity and zirconium is a fission product that is expected to be present in irradiated fuels. The present investigation addresses the electrochemical reduction of Zr4+ to Zro in LiCl - KCl eutectic molten salt in the temperature range 425-550degC using cyclic voltammetry (CV), square-wave voltammetry (SWV) and bulk electrolysis. Simulations of the CV data indicate that the initial reduction proceeds through surface confined steps: Zr4+* + 2e[?] - Zr2+* and Zr2+* + 2e[?] - Zr* processes (* adsorbed species) followed by a peak-shaped complex diffusion controlled step that consists of a combination of closely spaced processes associated with the reactions Zr4+ + 4e[?] - Zro and Zr4+ + 3e[?] - Zr+*. Zr+*, probably in the form of ZrCl* is then further reduced to Zro* at even more negative potentials. The simulations provide the first quantitative analysis of the thermodynamics and kinetics of the Zr4+ reduction in the LiCl-KCl eutectic.

Published
2013

35. Thermodynamic Properties Determination in LiF-CaF2Using Electrochemistry in High Temperature Fused Salts: Application to CeF3

Author

Gibilaro, Mathieu, Massot, Laurent, and Chamelot, Pierre

Abstract

Combining thermodynamic database and electrochemical measurements, CeF3thermodynamics properties were determined between 1113K and 1233K in LiF-CaF2solution. First, standard potentials of CeF3/Ce were calculated in different reference states: liquid and solid, and infinite dilution. Then activity coefficients of CeF3were estimated in the different reference states and for different composition scales: molarity, molality and molar fraction. Finally, constants which interconnected the infinite dilution reference state and the solid and liquid reference states were evaluated.

Published
2017
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36. Cyclic Voltammetric Experiment - Simulation Comparisons of the Complex Mechanism Associated with Electrochemical Reduction of Zr4+in LiCl-KCl Eutectic Molten Salt

Author

Fabian, Cesimiro P., Luca, Vittorio, Le, Thanh H., Bond, Alan M., Chamelot, Pierre, Massot, Laurent, Caravaca, Concepción, Hanley, Tracey L., and Lumpkin, Gregory R.

Abstract

Nuclear energy increasingly represents an important option for generating largely clean CO2-free electricity and zirconium is a fission product that is expected to be present in irradiated fuels. The present investigation addresses the electrochemical reduction of Zr4+to Zroin LiCl - KCl eutectic molten salt in the temperature range 425–550°C using cyclic voltammetry (CV), square-wave voltammetry (SWV) and bulk electrolysis. Simulations of the CV data indicate that the initial reduction proceeds through surface confined steps: Zr4+*+ 2e−↔ Zr2+*and Zr2+*+ 2e−↔ Zr*processes (* adsorbed species) followed by a peak-shaped complex diffusion controlled step that consists of a combination of closely spaced processes associated with the reactions Zr4++ 4e−→ Zroand Zr4++ 3e−→ Zr+*. Zr+*, probably in the form of ZrCl*is then further reduced to Zro*at even more negative potentials. The simulations provide the first quantitative analysis of the thermodynamics and kinetics of the Zr4+reduction in the LiCl-KCl eutectic.

Published
2013
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