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Redox Shuttle and Positive Electrode Protection for Li-O2 Systems Remi Blanchard

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Redox Shuttle and Positive Electrode Protection for Li-O2 Systems Remi Blanchard Redox shuttle and positive electrode protection for Li-O2 systems Remi Blanchard To cite this version: Remi Blanchard. Redox shuttle and positive electrode protection for Li-O2 systems. Other. Université Grenoble Alpes, 2017. English. NNT : 2017GREAI098. tel-01781457 HAL Id: tel-01781457 https://tel.archives-ouvertes.fr/tel-01781457 Submitted on 30 Apr 2018 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. THÈSE Pour obtenir le grade de DOCTEUR DE LA COMMUNAUTE UNIVERSITE GRENOBLE ALPES Spécialité : Matériaux, Mécanique, Génie Civil, Electrochimie Arrêté ministériel : 25 mai 2016 Présentée par Rémi BLANCHARD Thèse dirigée par Marian CHATENET, Professeur, Grenoble- INP , et codirigée par Arnaud MANTOUX, Maitre de Conférence, Université Grenoble-Alpes préparée au sein du Laboratoire d'Electrochimie et de Physicochimie des Matériaux et des Interfaces-LEPMI dans l'École Doctorale Ingénierie-Matériaux, Mécanique, Energétique Environnement procédés Production Redox shuttles and Positive Electrode Protection for Li-O2 systems Thèse soutenue publiquement le 15 décembre 2017, devant le jury composé de : Monsieur Daniel BELLET Professeur des Universités, Grenoble INP, Président Monsieur Sanjeev MUKERJEE Professeur, Northeastern University, Rapporteur Monsieur Mikhael BECHELANY Chargé de Recherche, CNRS, Rapporteur Monsieur Marian CHATENET Professeur des Universités, Grenoble-INP, Directeur de thèse Monsieur Arnaud MANTOUX Maitre de Conférences, Université Grenoble-Alpes, Co-Directeur de thèse Monsieur Marc ZIMMERMAN Ingénieur, HUTCHINSON SA, Examinateur Seul l'impossible mérite réflexion Dezso Kosztolanyi / Les aventures de Kornel Esti Acknowledgments Three years. It is a lot, and in many ways, it is not enough. Thanks to this wonderful experience, my personality and vision of the world and of science changed drastically. Some aspects still appear painful, with a lot of sweat, nerve crisis because of experiment failure, and sometime, this immeasurable joy when finally, the attended result is observed, for the first time. I would never trade this experience for anything, blood and tears, laugh and excitements, late nights at the lab, and late nights at the pub...And finally, I could not have met more wonderful persons that I had the chance to work with and made this thesis possible. For this reason, it feels necessary to acknowledge them, in proper ways. Firstly, my two advisors, Marian CHATENET and Arnaud MANTOUX. Both Wonderful scientists and persons. They had this incredible patience, and were always willing to help me, which enabled me to seize my subject, and sense the important conclusions and directions for my work. They were also highly comprehensive, always helping me and comforting me during the harsh emotional time. For this reason I really want to thanks them for their support and their humanity. Secondly, without the staff members of LEPMI, SIMAP and CMTC, nothing could have been done. For this reason, I really would like to thanks Claire and Yasmine of the LEPMI administrative service, for their reactivity and help, organizing conferences booking, but also filling all those purchase orders (I was a compulsive buyer). Also without their willing to form me on the Atomic Layer Deposition, a whole part of my thesis will have not been possible. For this reason, I am really grateful for Alex Crisci and Roman Reboud, thanks for your help and patience. I must also stress how I was annoying to Alex, as I wanted to do Raman, Ellipsometry, but also Vanadium deposition, on the "nano" reactor, and he was willing to help me doing those manipulations, even though he was grudgingly doing it (Joke).I would also like to thank very much Rachel Martin, which enabled me to do a lot of SEM and X-EDS analysis, late in my thesis and was always willing to help me, with the smile. For your kindness and help, thank you. Also the XPS analysis would have not been possible without Gregory Berthomé of SIMAP, thank you for your help and your patience, for explaining this powerful technique to me. Thirdly, I would like to thanks all my PhD students colleagues, along with the other researchers of the EIP team that I had the chance to work with, with always a lot of laughs and good moments at the Lunch time at the lab, but also during all those parties organized with the entire team, which really demonstrated how we were united. Vincent, for his Jokes and weird stories that were allowing me to fully disconnect during the lunch time, Céline and Raphael, also for their kindness and friendship and all the three of you, for supporting me during the harsh time. I would also like to thank Marc, for being my mentor at the beginning of my PhD, giving me the chance to not waste any time for the seizing of the experimental apparatus. Tristan, Matthieu (Deplagne), Fanny, Clémence, Marion, Fabien, Guillaume for their friendship, and for their patience (for my jokes that can be a little bit clumsy sometimes). To the end, I would like to thank my girlfriend, Orane, which supported me the whole time, enabled me to regain confidence when needed (but also kept my feet firmly to the ground, when I was dreaming of solving the energy crisis by myself), but also my beloved family, which supported me and make this experience possible. Merci à tous! Table of Contents Chapter I:Non aqueous Li-O2 batteries .............................................................................. 1 I. Green pathways toward energy Storing .................................................................. 3 a. Actual Energy Sources .............................................................................................................. 3 b. Replacement solutions for the electrical power grid ............................................................... 6 c. Toward high energy systems for gasoline replacement in Mobile application ...................... 11 II. The Li-O2 systems................................................................................................... 15 a. Discovery of Li-oxygen batteries ............................................................................................ 15 b. ORR and OER mechanisms in aprotic medium ....................................................................... 20 c. Effect of water ........................................................................................................................ 29 d. Issues of Li-O2 cathodes and improvement paths .................................................................. 31 Conclusion ................................................................................................................... 36 References.....................................................................................................................37 Chapter II :Experimental section .................................................................................................. 43 I. Electrochemistry ........................................................................................................................ 44 a. Washing of the glassware ...................................................................................................... 44 b. Chemicals ............................................................................................................................... 44 c. Three-electrodes setup ........................................................................................................... 45 d. Differential Electrochemical Mass Spectrometry ................................................................... 45 e. Full cell experiment ................................................................................................................ 46 f. Electrochemical testing .......................................................................................................... 47 II. Characterization techniques ..................................................................................................... 47 a. Differential Electrochemical Mass Spectrometry ................................................................... 47 b. Raman Spectroscopy .............................................................................................................. 52 c. Field-Emission Gun-Scanning Electron Microscopy (FEG-SEM) .............................................. 53 d. X-Ray Energy Dispersive Spectrometer (X-EDS) ..................................................................... 54 e. UV-Visible Spectrophotometry ............................................................................................... 54 f. X-ray Photoelectron Spectroscopy (XPS) ................................................................................ 55 g. Ellipsometry ............................................................................................................................ 57 h. X-ray Diffraction ..................................................................................................................... 58 References .............................................................................................................................
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