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Growth, Morphology and Solid State Miscibility of Alkali Nitrates

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Growth, Morphology and Solid State Miscibility of Alkali Nitrates Growth, Morphology and Solid State Miscibility of Alkali Nitrates Raúl Benages Vilau ADVERTIMENT. La consulta d’aquesta tesi queda condicionada a l’acceptació de les següents condicions d'ús: La difusió d’aquesta tesi per mitjà del servei TDX (www.tdx.cat) i a través del Dipòsit Digital de la UB (diposit.ub.edu) ha estat autoritzada pels titulars dels drets de propietat intel·lectual únicament per a usos privats emmarcats en activitats d’investigació i docència. No s’autoritza la seva reproducció amb finalitats de lucre ni la seva difusió i posada a disposició des d’un lloc aliè al servei TDX ni al Dipòsit Digital de la UB. No s’autoritza la presentació del seu contingut en una finestra o marc aliè a TDX o al Dipòsit Digital de la UB (framing). Aquesta reserva de drets afecta tant al resum de presentació de la tesi com als seus continguts. En la utilització o cita de parts de la tesi és obligat indicar el nom de la persona autora. ADVERTENCIA. La consulta de esta tesis queda condicionada a la aceptación de las siguientes condiciones de uso: La difusión de esta tesis por medio del servicio TDR (www.tdx.cat) y a través del Repositorio Digital de la UB (diposit.ub.edu) ha sido autorizada por los titulares de los derechos de propiedad intelectual únicamente para usos privados enmarcados en actividades de investigación y docencia. No se autoriza su reproducción con finalidades de lucro ni su difusión y puesta a disposición desde un sitio ajeno al servicio TDR o al Repositorio Digital de la UB. No se autoriza la presentación de su contenido en una ventana o marco ajeno a TDR o al Repositorio Digital de la UB (framing). Esta reserva de derechos afecta tanto al resumen de presentación de la tesis como a sus contenidos. En la utilización o cita de partes de la tesis es obligado indicar el nombre de la persona autora. WARNING. On having consulted this thesis you’re accepting the following use conditions: Spreading this thesis by the TDX (www.tdx.cat) service and by the UB Digital Repository (diposit.ub.edu) has been authorized by the titular of the intellectual property rights only for private uses placed in investigation and teaching activities. Reproduction with lucrative aims is not authorized nor its spreading and availability from a site foreign to the TDX service or to the UB Digital Repository. Introducing its content in a window or frame foreign to the TDX service or to the UB Digital Repository is not authorized (framing). Those rights affect to the presentation summary of the thesis as well as to its contents. In the using or citation of parts of the thesis it’s obliged to indicate the name of the author. UNIVERSITAT DE BARCELONA Departartament de Cristal·lografia, Mineralogia i Dipòsits Minerals. Grup de Aliatges Moleculars GROWTH, MORPHOLOGY AND SOLID STATE MISCIBILITY OF ALKALI NITRATES -2013- Programa de Doctorat: Ciències de la Terra El doctorand, Raúl Benages Vilau Dpt. Cristal·lografia, Mineralogia i Dipòsits Minerals. Universitat de Barcelona Els directors: La tutora: Dr. M A. Cuevas-Diarte. Dra. Mª T. Calvet i Pallàs Dpt. Cristal·lografia, Mineralogia Dpt. Cristal·lografia, Mineralogia i Dipòsits Minerals. i Dipòsits Minerals. Universitat de Barcelona Universitat de Barcelona Acknowledgements ACKNOWLEDGEMENTS This PhD thesis must be addressed to my mother’s memory. She was always proud of me and let me study what I want. She supported me until the end of her days. Although you can not read this THANK YOU GRACIAS!! To my family for their support. Thanks to Miquel Àngel and Teresa for trust me and support me in this thesis and in all other researches performed. They give me the opportunity to work with many techniques and many people in order to achieve satisfactory results in several fields. I should recollect here all the important people that conduct me to here. My first contact with crystallography was early, when I had 16-17 years old. My teacher explains us the seven crystal systems and the 320 point groups. I was amazed about symmetry. But, not only that, he also introduced us, in a certain way, the Kossel crystal and the kink sites for the preffered sites for a crystal growth. In that time, if I had thought about working on this subject I would not have believed it. Thus, my high- school teacher was the first who introduce me in the crystallography. Thank you, wherever you are. Next person was Laura Bayes. In the second year of chemistry degree we decided to assist to crystallography course. During the course she motivated me to study hard this subject. It was a fruitfull course because she and me begun to work in the crystallography department. I think that without her, probably I never started to make research here. For this reason I may say thank you to you. Obviously, our crystallography teacher was Miquel Àngel Cuevas-Diarte. So, a first thanks for him and for Teresa Calvet to let me start my career here while I was studying the chemistry and the material science degrees. About 6 years after that beginning I started this PhD. Thanks to all the ‘aliatges moleculars’ group people who has helped me at some time: Laura, Raquel, Mercedes, Evelyn, Xabier… and also for the rest of the department people: Thomas, Cristina, Montgarri… Big thanks for the people from Turin who make me understand the crystal morphology and the crystal growth. Thank you: Dino, Marco, Marco and Emmanuelle. Thank you for make me so easy and fruitfull my residencies there. Many thanks to Dino for his passion in this project and his hospitality. Than you to his wife Renata for ther lovely meals. Thank you to Carlos Pina for the fruitful experiments of epitaxy in the AFM. To Sander, for the nice pictures taken in the confocal microscopy on a growing surface of nitratine. During the PhD I learnt lots of things from the academic point of view. Apart from all the knowledge in this manuscript I performed some research work about solar thermal energy storage. Thanks to the people of Quality Chemicals to have done with us that Acknowledgements research. We have organized two crystal growth competitions to present high school students this beautiful subject. Next, I have to give a big thank YOU to Heura. We shared a flat during 1 year and a half. They were very pleasant and wonderful days. THANK YOU Heura to be with me in my hardest and sad days after my mother’s dead. Thank you to beer!!! It seems strange but I have lernt to brew in the past 4-5 years. I enjoy a lot to brew and to share the final product. Many people loved every beer I brew: a pleasure for me! Thank you to David and Dani to be friends and to create my outstanding logo! Thank you to Maria to take me out for a beer whenever I need it. To Pilar because she is always there Lastly, I want to give a large THANK YOU to Layita for all the wonderfull days you are with me: love forever! Thank you for the peace I feel at your side. Thank you to make me feel special… thank you to be with me! I hope you enjoy this reading with a good beer. Content GENERAL INTRODUCTION I CHAPTER 1: Alkali nitrates review 1 1.1. INTRODUCTION 3 1.2. LITHIUM NITRATE 5 1.2.1. Crystal structure, polymorphism and phase transitions. 5 1.2.2. Crystal growth. 6 1.2.3. Morphology. 6 1.3. SODIUM NITRATE 7 1.3.1. Crystal structure, polymorphism and phase transitions. 7 1.3.2. Crystal growth. 9 1.3.3. Morphology. 11 1.4. POTASSIUM NITRATE 13 1.4.1. Crystal structure, polymorphism and phase transitions. 13 1.4.2. Crystal growth. 16 1.4.3. Morphology. 18 1.5. RUBIDIUM NITRATE 20 1.5.1. Crystal structure, polymorphism and phase transitions. 20 1.5.2. Crystal growth. 23 1.5.3. Morphology. 23 1.6. CESIUM NITRATE 24 1.6.1. Crystal structure, polymorphism and phase transitions. 24 1.6.2. Crystal growth. 25 1.6.3. Morphology. 26 1.7. SOLID STATE MISCIBILITY AND BINARY PHASE DIAGRAMS 29 1.8. DISCUSSION 34 1.9. CONCLUSIONS 38 1.10. BIBLIOGRAPHY 40 CHAPTER 2: NITRATINE (NaNO3) THEORETICAL MORPHOLOGY 53 2.1. GENERAL INTRODUCTION 55 2.1.1. The Bravais-Friedel-Donnay-Harker (BFDH) approach. 58 2.1.2. The Hartman Perdok (HP) approach. 58 Content 2.1.3. Surface energy. 62 2.1.4. Equilibrium form: the Wulff’s plot. 64 2.2. INTRODUCTION TO THE NaNO3 SYSTEM 66 2.2.1. Previous works. 66 2.2.2. A crystallographic description of R3c space group. 67 Ŭ 2.2.3. The {104} and {012} problem. 71 2.3. DETERMINATION OF THE THEORETICAL MORPHOLOGY OF 72 NaNO3 2.3.1. The Bravais-Friedel-Donnay-Harker approach. 72 2.3.2. The Hartman-Perdok approach. 74 2.3.2.1. Building units of NaNO3. 74 2.3.2.2. PBC analysis of NaNO3 structure. 77 2.3.2.2.1. The [ ] direction. 77 Ŭ 2.3.2.2.2. The [441] direction. 80 Ŭ 2.3.2.2.3. The [010]421 direction. 86 2.3.2.2.4. The [001] direction. 91 2.3.2.3. The theoretical equilibrium morphology of NaNO calculated in 3 93 a vacuum. 2.4. DISCUSSION 96 2.5. CONCLUSIONS 99 2.6. BIBLIOGRAPHY 100 CHAPTER 3: Growth kinetics of the {104} faces of nitratine (NaNO3) 103 3.1.
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