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Design of New Sulfate-Based Positive Electrode Materials for Li- and Na-Ion Batteries Marine Reynaud

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Design of New Sulfate-Based Positive Electrode Materials for Li- and Na-Ion Batteries Marine Reynaud Design of new sulfate-based positive electrode materials for Li- and Na-ion batteries Marine Reynaud To cite this version: Marine Reynaud. Design of new sulfate-based positive electrode materials for Li- and Na-ion batteries. Material chemistry. Université de Picardie Jules Verne, 2013. English. tel-01018912 HAL Id: tel-01018912 https://tel.archives-ouvertes.fr/tel-01018912 Submitted on 7 Jul 2014 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Ph.D. Dissertation Speciality: Materials Science presented at the Université de Picardie Jules Verne by Marine REYNAUD for the degree of Doctor of Philosophy of the Université de Picardie Jules Verne Design of new sulfate-based positive electrode materials for Li- and Na-ion batteries defended on 9 December 2013, post referees’ approval, in front of the committee: Dr. Robert DOMINKO Research Director Referee Dr. M. Rosa PALACÍN Research Director CSIC Referee Dr. Valérie PRALONG Research Director CNRS Examiner Dr. Juan RODRÍGUEZ-CARVAJAL Research Scientist ILL Examiner Pr. Christian MASQUELIER Professor Examiner Dr. Gwenaëlle ROUSSE Assistant Professor ‒ HDR Examiner Dr. Jean-Noël CHOTARD Assistant Professor Director Pr. Jean-Marie TARASCON Professor Director Thèse de Doctorat Spécialité: Sciences des Matériaux présentée à l’ Université de Picardie Jules Verne par Marine REYNAUD pour obtenir le grade de Docteur l’Université de Picardie Jules Verne Elaboration de nouveaux matériaux à base de sulfates pour l’électrode positive des batteries à ions Li et Na soutenue le 9 décembre 2013, après avis des rapporteurs, devant le jury d’examen : Dr. Robert DOMINKO Directeur de Recherche Rapporteur Dr. M. Rosa PALACÍN Directeur de Recherche CSIC Rapporteur Dr. Valérie PRALONG Directeur de Recherche CNRS Examinateur Dr. Juan RODRÍGUEZ-CARVAJAL Scientifique ILL Examinateur Pr. Christian MASQUELIER Professeur Examinateur Dr. Gwenaëlle ROUSSE Maître de Conférences ‒ HDR Examinateur Dr. Jean-Noël CHOTARD Maître de Conférences Directeur Pr. Jean-Marie TARASCON Professeur Directeur A mes parents, mes frère et soeur, et mes grands-parents, A Mikel. Abstract The next generations of Li- and Na-ion batteries will rely on the development of new sustainable, low-cost and safe positive electrode materials. To this end, we explored the world of minerals with an emphasis on spotting structures having the prerequisites for insertion and deinsertion of alkaline ions. From this survey, we embarked on the investigation of bimetallic sulfates derived from the bloedite mineral and having the general formula AxM(SO4)2·nH2O (A = Li, Na, M = 3d transition metal and n = 0, 4). These systems present rich crystal chemistry, undergoing phase transitions upon heating and removal of water. The new structures were determined by combining X-ray, neutron and electron diffraction techniques. We have also shown that lithium-based compounds LixM(SO4)2 present interesting antiferromagnetic properties resulting from their peculiar structures, which solely enable super-super-exchange interactions. Finally, and more importantly, we identified among the isolated compounds three iron-based sulfates, namely Na2Fe(SO4)2·4H2O, Na2Fe(SO4)2 and Li2Fe(SO4)2, which present attractive electrochemical properties against both lithium and sodium. With a + 0 potential of 3.83 V vs. Li /Li , the new marinite phase Li2Fe(SO4)2 displays the highest potential ever observed for the FeIII+/FeII+ redox couple in a fluorine-free iron-based inorganic compound, only rivaled by the triplite form of LiFeSO4F. Résumé Les prochaines générations de batteries à ions lithium et sodium seront basées sur le développement de nouveaux matériaux d’électrode positive durables, peu chers et sûrs. Dans ce but, nous avons exploré le monde des minéraux à la recherche de structures présentant les pré-requis pour l’insertion et la désinsertion d’ions alcalins. Nous avons alors entrepris l’étude de sulfates bimétalliques dérivés du minéral bloedite, ayant pour formule générale AxM(SO4)2·nH2O (A = Li, Na, M = métal de transition 3d, et n = 0, 4). Ces systèmes présentent une cristallochimie riche, montrant des transitions structurales en fonction de la température ainsi qu’avec le départ des molécules d’eau. Les nouvelles structures ont été déterminées en combinant les techniques de diffraction des rayons X, neutrons et électrons. Nous avons également montré que les composés à base de lithium LixM(SO4)2 présentent des propriétés antiferromagnétiques intéressantes, du fait notamment de leurs structures particulières qui permettent seulement des interactions de super-super-échange. Enfin et surtout, nous avons, parmi les composés isolés, identifié trois sulfates à base de fer, à savoir Na2Fe(SO4)2·4H2O, Na2Fe(SO4)2 et Li2Fe(SO4)2, qui présentent des propriétés électrochimiques intéressantes face au lithium et au sodium. Avec un potentiel de 3,83 V vs. Li+/Li0, la nouvelle phase III+ II+ marinite Li2Fe(SO4)2 affiche le plus haut potentiel jamais observé pour le couple redox Fe /Fe dans un composé inorganique à base de fer et dépourvu de fluor, et est en fait seulement dépassé par celui de la forme triplite de LiFeSO4F. This thesis work has been carried out with the financial support of the French “Ministère de l’Enseignement Supérieur et de la Recherche”. It was prepared at the laboratory: Laboratoire de Réactivité et Chimie des Solides (LRCS) Université de Picardie Jules Verne (UPJV) Unité Mixte de Recherche CNRS (UMR 7314) 33, rue Saint Leu 80039 AMIENS cedex FRANCE under the supervision of: Pr. Jean-Marie Tarascon Dr. Jean-Noël Chotard and in close collaboration with: Dr. Gwenaëlle Rousse Ce travail de thèse a été réalisé avec le concours financier du Ministère de l’Enseignement Supérieur et de la Recherche. Il a été préparé au laboratoire : Laboratoire de Réactivité et Chimie des Solides (LRCS) Université de Picardie Jules Verne (UPJV) Unité Mixte de Recherche CNRS (UMR 7314) 33, rue Saint Leu 80039 AMIENS cedex FRANCE sous la direction de : Pr. Jean-Marie Tarascon Dr. Jean-Noël Chotard et en étroite collaboration avec: Dr. Gwenaëlle Rousse Acknowledgements First and foremost, I would like to express my sincere gratitude to my supervisors Jean-Marie Tarascon and Jean-Noël Chotard, as well as to Gwenaëlle Rouse for their support and their guidance, and above all for having instilled in me their love of research. I would also like to thank the other members of my PhD committee Robert Dominko, Rosa Palacín, Valérie Pralong, Juan Rodríguez-Carvajal and Christian Masquelier, for their interest in my work and their insightful comments. Besides, I am very grateful to all the people who have actively taken part in this research work : Moulay Sougrati for the Mössbauer spectroscopy, Robert Messinger for the solid-state NMR, Artem Abakumov and Gustaaf Van Tendeloo for the TEM studies, Matthieu Courty for the TGA-DSC measurements, Alexandre Ponrouch for the coating of some electrode materials, Sylvain Boulineau for the SPS syntheses, Thomas Hansen, Erik Elkaïm and Matthew Suchamel for their assistance in NPD and Synchrotron XRD experiments. Many thanks also to all past and present members of the LRCS for their help, advice and support during the last four years. Last but not least, I would like to thank my friends, my family and Mikel for their constant support and encouragement. Merci à tous. Table of contents General introduction .................................................................................... 1 Chapter I. State of the art .................................................................... 5 I.1 Brief overview of the main technologies of batteries ...................................................... 5 I.1.1 Lead-acid batteries ........................................................................................................ 6 I.1.2 Nickel-based technologies ............................................................................................. 6 I.1.3 High-temperature batteries .......................................................................................... 7 I.1.4 The first room-temperature lithium batteries .............................................................. 8 I.1.5 Lithium-ion batteries ..................................................................................................... 9 I.1.6 Lithium polymer batteries ............................................................................................. 9 I.1.7 Sodium-ion batteries ................................................................................................... 10 I.2 Positive electrode materials for Li- and Na-ion batteries ............................................... 12 I.2.1 The first electrode material for lithium batteries: titanium sulfide TiS2 ..................... 14 I.2.2 Lithium transition-metal oxides................................................................................... 15 I.2.2.1 Layered oxides ..................................................................................................... 15 I.2.2.2 Spinel manganese oxide .....................................................................................
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