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Thesis Reference Thesis Experimental and theoretical studies of boron and hydrogen containing compounds in relation to potential hydrogen storage and ionic conduction applications SHARMA, Manish Abstract This thesis deals with the fundamental studies of some materials containing boron-hydrogen bonds which can potentially be used either as the hydrogen storage materials (M(BH4)2, M=Alkaline earth metal), as the solid electrolytes for batteries (Na2B12H12) or as reducing agents for CO2 (Mg(BH4)2). First part of thesis deals with borohydrides (BH4-). Synthesis and characterization of halide-free Sr(BH4)2, Ba(BH4)2 and Eu(BH4)2 is reported. Crystallographic study of these compounds helped in identifying several new phases and a new species metal borohydride hydride (M2(BH4)H3). In depth study of B-H bond breaking is reported via isotope exchange reaction in Ca(BH4)2.A practical example of borohydride as reducing agent is reported by showing the reduction of CO2 with gamma-Mg(BH4)2. The second part of the thesis focuses on closoboranes derived from the B12H122- ion. Compounds of this family have recently attracted great interest as solid ionic conductors for Li and Na ions.Results of DFT calculations on isolated B12H122- anions and halogen (F, Cl or Br) substituted anions were analysed in detail. Synthesis of Na2B12(SCN)H11 is [...] Reference SHARMA, Manish. Experimental and theoretical studies of boron and hydrogen containing compounds in relation to potential hydrogen storage and ionic conduction applications. Thèse de doctorat : Univ. Genève, 2017, no. Sc. 5101 DOI : 10.13097/archive-ouverte/unige:96376 URN : urn:nbn:ch:unige-963769 Available at: http://archive-ouverte.unige.ch/unige:96376 Disclaimer: layout of this document may differ from the published version. 1 / 1 UNIVERSITÉ DE GENÈVE FACULTÉ DES SCIENCES Section de Chimie et Biochimie Professeur Hans Hagemann Département de Chimie Physique Experimental and Theoretical Studies of Boron and Hydrogen Containing Compounds In Relation to Potential Hydrogen Storage and Ionic Conduction Applications THÈSE présentée à la Faculté des sciences de l’Université de Genève pour obtenir le grade de Docteur ès Sciences, mention Chimie par Manish Sharma d’Inde Thèse N° 5101 GENÈVE Atelier d’impression ReproMail 2017 Acknowledgements I would like to express my sincere gratitude towards my supervisor, Prof. Hans Hagemann, for giving me the opportunity to study at the University of Geneva and for his explanations and scientific discussions. He created a very liberal work environment and encouraged me to think independently. He gave full freedom from the choice of projects and collaborations. For me Hans is a perfect example to learn the work-life balance. He emphasized on having a good social life outside office and encouraged to play sports, visit museums, music festivals and to travel. I would like to thank Prof. H. W. Li and Dr. A. Remhof for accepting and evaluating my thesis. I am grateful to Dr. L. M. L. Daku for helping me to conduct computational calculations discussed in the thesis and for being the part of the thesis review committee. Thanks to Prof. A. Hauser for his support and valuable suggestions throughout my PhD. I admire him for his art of explaining complex concepts in a lucid way. I would like to thank all the collaborators, in particular Prof. R. Černý, E. Didelot, Dr. D. Jeannerat, Dr. M. Pupier, Prof. T. Burgi, Dr. M. Chekini, Prof. Y. Filinchuk, F. Morelle, Prof. T. Jensen, Dr. B. Richter, Prof. H. W. Li, Dr. L. He, Dr. A. Remhof and Dr. E. Roedern for synergic work. I am thankful to Ma’am C. Ludy and I. Garin for helping me with bureaucratic formalities. N. Amstutz and P. Barman for providing technical support and to Dominique Lovy for IT support. I would like to acknowledge all the present and former members of Hauser-Hagemann group and my friends whom I met during my PhD: Teresa, Pablo, Romain, Angelina, Daniel, Andrea, Pradip, Jacob, Enza, Yolanda, Antoine, Quinchao, Jiji, Alexandra, Jan, Elia, Jakob, Igor, Ani, Rania, Mahshid, Martin and Roberto. They have been my closest friends in this period, sharing with me good and bad moments. Finally, I would like to thank my wife and my parents for having supported me during these years. i ii Résumé Ce travail de thèse porte sur les études fondamentales de certains matériaux contenant des liaisons bore-hydrogène qui peuvent potentiellement être utilisé comme des matériaux pour stockage de l'hydrogène, comme électrolyte solide dans les batteries, ou comme agents réducteurs pour le CO2. La première partie de cette thèse sera consacrée aux études expérimentales des borohydrures métalliques de type M(BH4)n. Le premier chapitre expérimental aborde la synthèse et la caractérisation des composés dépourvus d’halogénures Sr(BH4)2, Ba(BH4)2 et Eu(BH4)2. La synthèse de ces composés a été effectuée à partir de l'hydrure métallique et de Et3N-BH3. Lorsqu’ils sont chauffés à des températures élevées, ces composés sont plus stables que ceux rapportés dans la littérature obtenus par différentes voies de synthèse et impliquant des impuretés d'halogène. L'étude cristallographique de ces composés a permis d'identifier plusieurs nouvelles phases. Au cours des réactions de décomposition thermique, la formation d'un composé métal hydrure-borohydrure M2H3(BH4), avec M = Sr et Eu, a été observée pour la première fois. Le produit Eu(BH4)2 s'est révélé être un excellent luminophore émettant dans le bleu à 463 nm. De plus, plusieurs méthodes de synthèse infructueuses ou qui ont abouti à des produits impurs sont également discutées. Dans le chapitre subséquent, la réaction d'échange hydrogène-deutérium ainsi que la réaction inverse sont étudiées pour le composé Ca(BH4)2 en fonction de la température et de la pression de deutérium (resp. d'hydrogène). La progression de cette réaction est suivie par la spectroscopie IR. Cette réaction d'échange d'isotopes fournit l'énergie d'activation minimale nécessaire à la rupture de la liaison B-H sans induire d'autres changements structurels dans le composé. On constate que l'énergie d'activation pour Ca(BH4)2 est significativement plus grande que pour le composé analogue au Mg, ce qui implique que l'ion métallique joue un rôle important dans la rupture de la liaison B-H. Le dernier chapitre consacré aux borohydrures, étudie la réaction de Mg(BH4)2 avec le CO2. La consommation de CO2 et la formation de B2H6 sont contrôlées en utilisant la spectroscopie IR à phase gazeuse. Ces expériences montrent que le γ-Mg(BH4)2 poreux réagit facilement avec le CO2 même à température ambiante, tandis que la phase stable de α-Mg(BH4)2 réagit uniquement à température élevée. Cette réaction peut initier d'autres études concernant l’utilisation des borohydrures pour la réduction du CO2 ainsi que pour la régénération du carburant. 2- La deuxième partie de cette thèse porte sur les dérivés closoboranes de l'ion B12H12 . Les composés issus de cette famille ont récemment attiré un grand intérêt en tant que conducteurs ioniques solides pour les ions Li et Na. [1] iii 2- Les résultats des calculs DFT sur les anions B12H12 isolés et les anions substitués par les halogènes (F, Cl ou Br) ont été analysé en détail. Le but de cette étude est de prédire les données spectroscopiques pour les composés halogénés, puisque ces composés partiellement substitués sont difficile à préparer et à purifier. Des tendances systématiques dans diverses propriétés, comme par exemple pour l'étirement de la liaison B-H par rapport au nombre d'atomes d'hydrogène, sont observés. La stabilité thermodynamique de divers isomères est également discutée dans cette partie. Le dernier chapitre expérimental se concentre sur la synthèse de certains substitués des closoboranes. Un mélange de Na2B12(SCN)nH(12-n) avec (n =1 et 2) a été synthétisé. La mesure de la conductivité ionique de cet échantillon montre qu’à température ambiante, la conductivité est 1000 fois meilleure par rapport au composé Na2B12H12 pur. La bromation complète et partielle de Na2B12H12 est également rapportée. Cependant, la bromation partielle donne un mélange de différents produits. Et finalement, des résultats préliminaires sur d'autres systèmes sont également inclus dans cette partie. [1] Hansen, B. R. S.; Paskevicius, M.; Li, H.-W.; Akiba, E.; Jensen, T. R., Coord. Chem. Rev. Metal boranes: Progress and applications, 2016, 323, 60-70. iv Summary This thesis deals with the fundamental studies of some materials containing boron-hydrogen bonds which can potentially be used either as the hydrogen storage materials, as the solid electrolytes for batteries or as reducing agents for CO2. In the first part of thesis, experimental studies on metal borohydrides M(BH4)n are reported. The first experimental chapter presents the synthesis and characterization of halide-free Sr(BH4)2, Ba(BH4)2 and Eu(BH4)2 starting from the metal hydride and Et3N-BH3. These compounds are more stable upon heating compared to other preparations reported in the literature involving halogen impurities. The crystallographic study of these compounds allowed identifying several new phases. During the thermal decomposition reactions, the formation of a metal hydride-borohydride M2H3(BH4) for M = Sr and Eu was observed for the first time. Eu(BH4)2 has been shown to be an excellent phosphor emitting at 463 nm (blue colour). Several unsuccessful or partially successful reaction schemes which end up in impure products are also discussed. In the next chapter, the hydrogen-deuterium exchange reaction as well as the reverse reaction is studied for Ca(BH4)2 as a function of temperature and deuterium (resp. hydrogen) pressure. The progress of this reaction is monitored using IR spectroscopy. This isotope exchange reaction provides the minimum activation energy of breaking the boron hydrogen bond without inducing further structural changes in the compound.
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