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Final Copy 2018 06 19 Pottic This electronic thesis or dissertation has been downloaded from Explore Bristol Research, http://research-information.bristol.ac.uk Author: Potticary, Jason L Title: Novel Approaches to Morphological and Polymorphological Control and Selectivity in Crystalline Systems General rights Access to the thesis is subject to the Creative Commons Attribution - NonCommercial-No Derivatives 4.0 International Public License. A copy of this may be found at https://creativecommons.org/licenses/by-nc-nd/4.0/legalcode This license sets out your rights and the restrictions that apply to your access to the thesis so it is important you read this before proceeding. Take down policy Some pages of this thesis may have been removed for copyright restrictions prior to having it been deposited in Explore Bristol Research. However, if you have discovered material within the thesis that you consider to be unlawful e.g. breaches of copyright (either yours or that of a third party) or any other law, including but not limited to those relating to patent, trademark, confidentiality, data protection, obscenity, defamation, libel, then please contact [email protected] and include the following information in your message: •Your contact details •Bibliographic details for the item, including a URL •An outline nature of the complaint Your claim will be investigated and, where appropriate, the item in question will be removed from public view as soon as possible. Novel Approaches to Morphological and Polymorphological Control and Selectivity in Crystalline Systems By JASON POTTICARY School of Chemistry UNIVERSITY OF BRISTOL A dissertation submitted to the University of Bristol in accordance with the requirements of the degree of DOCTOR OF PHILOSOPHY in the Faculty of Science. MARCH 2018 Word count: Forty seven thousand ABSTRACT he physical properties and the potential applications of a material are defined exclusively by the way in which the matter packs together and how discrete portions of this matter Tform on a macroscopic level. For example, the mineral quartz is a commonly used material for optical experiments. The way in which silicon and oxygen atoms pack allow a fairly uniform transmission of light from 1400 nm to 200 nm and our ability to grow large single-crystals, allow for applications such as cuvettes and optical windows. Issues arise when developing materials if they possess the required physical properties but cannot be grown in the right morphology or they have the required morphology but need their properties tuned. Quartz would not be as useful, if it only grew as highly anisotropic, crystalline needles. This thesis investigates the control of crystal packing (polymorphism) of molecular crystals, specifically the polyaromatic hydrocarbon coronene, using magnetic fields applied during the crystal growing process. A previously unknown polymorph of coronene was observed and fully characterised. The polymorph is accessible when grown from solution under a field between 0.9 T to 1.0 T. When investigating why this selectivity may be occurring, it was found that not only is the molecular conformation of the new polymorph the most energetically favourable via simulation, but the new polymorph is also accessible at cryogenic temperatures. Previous data reported on low-temperature coronene is readdressed with the knowledge of the new polymorph. Further to polymorphism, the morphology of a complex oxide material, specifically the high- temperature superconductor yttrium barium copper oxide (YBCO), is addressed in attempts to grow nanowires by mimicking the mechanism of micro-crucible growth without the use of a carbonaceous bio-template. Nanowires of various lengths and widths were grown using different amounts of a sodium-based flux. The nanowires were identified as a range of materials (Y2BaCuO5 (Y211), YBa2Cu3O7¡x (Y123), Ba2CuO) based on the temperature and sodium content. This method was easily translated to other, more complex, metal-oxide systems and promises to be a general route to the formation of inorganic nanowires. i DEDICATION AND ACKNOWLEDGEMENTS The real heroes of this thesis and work contained herein are the people that have helped me to embark on this obsessive journey and so in this small way I wish to convey my Timmense gratitude. Without some of whom, this work would have been impossible and without the others, these past few years would not have been even remotely as fun. First to my wife Stasja, my infinite source of encouragement and inspiration and also my ground. Your patience and understanding have made all of this possible. You have always made me want to be better and for you, I will always keep trying. It doesn’t even need stating that I wouldn’t be here and this thesis wouldn’t exist without you, but I’m sure you agree, it is nice to have in writing. Also to the third member of our family, whom I cannot wait to meet! My supervisor Dr. Simon Hall, your boundless enthusiasm, encouragement and support have kept me not only steady but constantly interested in the work at hand. Thank you for granting me the opportunity to work in this field and within your group. May your innovative perspectives ever flow - Omnis caro et caseus omnis!. To my partner in death-defying experiments Dr. Lui Terry, as far as I’m concerned you haven’t lived if you have never manned a fumehood with an HF spill kit. You have only added positive things to my life and I know there is more to come. Dr. Ben and Mr. Sparticus Mills, never a dull moment, you guys were the best company one could hope for in a lab, a vast source of knowledge both scientific and otherwise. To all those in the Complex Functional Materials Group, past and present who have kept things interesting and been a constant stream of enthusiasm; Tash, Tom, Becky, Omar, Julia, Charlie, Torsten, Nicole, Ge, Pedr, George, Alex and all those I’ve missed. There is clearly not enough room to correctly articulate how valuable you have all been. Throughout the University of Bristol and School of Chemistry, to the people who have always been ready to offer assistance when needed. Dr. Chris Bell, thank you for always providing me with a new perspective. Mr. Jonathan Jones for help with the microscopes and keeping them ticking. Dr. Hazel Sparkes and Dr. Natalie Pridmore for endless amounts of support with anything related to X-ray diffraction. Professor Charl Faul for keeping the lab ship-shape and Bristol fashion. Ms. Ilerha Hassimova for keeping me optimistic and Jonesy Worrall for pleasant distractions from the past. To all collaborators with whom I have had the pleasure of working with specifically, Drs. Enrico Da Como and Simon Crampin from the University of Bath, Dr Hans Engelkamp from Radboud University, Dr. Yoichi Kamihara from Keio University and Dr. Liana Vella-Zarb from iii the University of Malta. Also to Professors Yoshihiro Yamazaki and Sossina Haile for giving me a leg-up back into science. My family of whom there are clearly too many to name but I will do so anyway; Mum and Nick, Nana and Granddad, Matthew, Adam, Robin, Faye, Alicia, Lauren, Hannah, Ryan, Julia, Heidi, Lucy, Amelia, Cassie, Olivia, Paul, Vicky, Liam, Debbie, Nigel, Kat, Matt, Matt and Effie for never giving me a hard time for constantly being too busy and going months without contact, you were all one less stress to have to deal with and nothing I could ever do would make me deserving of being genetically stuck to such a fantastic group of people. My friend Mr. Gareth Rees, for great times at the Carrington institute and being one of the best people I know. Not sure where I’d be if I’d never met you. Finally, to the Bristol Centre for Functional Nanomaterials for giving me this opportunity and the seemingly bottomless funding, specifically for the support from Annela, Terry, Joanna, Becky and yes, even Andy. Thank you all. iv AUTHOR’S DECLARATION declare that the work in this dissertation was carried out in accordance with the requirements of the University’s Regulations and Code of Practice for Research IDegree Programmes and that it has not been submitted for any other academic award. Except where indicated by specific reference in the text, the work is the candidate’s own work. Work done in collaboration with, or with the assistance of, others, is indicated as such. Any views expressed in the dissertation are those of the author. SIGNED: ................................................... DATE: ...................................... v TABLE OF CONTENTS Page List of Figures xi List of Tables xv Acronyms xvii 1 Introduction 1 1.1 Rationale............................................ 1 1.2 Crystals and crystalline matter............................... 2 1.2.1 Crystallisation .................................... 2 1.2.2 Types of crystal.................................... 3 1.2.3 The unit cell...................................... 3 1.2.4 Naming conventions used in this thesis ..................... 5 1.3 Crystal nucleation....................................... 7 1.3.1 Secondary nucleation ................................ 7 1.3.2 Primary nucleation.................................. 7 1.4 Polymorphism ......................................... 10 1.4.1 Naming polymorphs................................. 12 1.4.2 Metastable polymorphs............................... 12 1.5 Morphology........................................... 13 1.5.1 Polymorph directed morphology.......................... 14 1.6 Characterisation of crystalline matter........................... 14 1.6.1 X-ray diffraction ..................................
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