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Carbon-Based Nanoporous Materials for Hydrogen Storage Montanuniversität Leoben Carbon-based nanoporous materials for hydrogen storage MSc. Nikolaos Kostoglou Doctorate thesis submitted to the Department of Physical Metallurgy and Materials Testing (Chair of Functional Materials and Materials Systems) of the Montanuniversität Leoben in partial fullfilment of the requirements of the degree of a Doktor der montanistischen Wissenschaften (Dr. mont.) Leoben, November 2017 The current thesis was not funded by any kind of project within its course of three years, instead, was significantly supported by a worldwide network of collaborators, including scientific institutions and companies, in terms of materials availability and experimental measurements. Statutory declaration I declare in lieu of oath that the present thesis was created by myself independently and only using the literature cited. Leoben, November 2017 Signature Acknowledgments This study would have not been feasible without the contribution of certain people from various institutions and companies worldwide. My deep and sincere gratitude goes to my mentor/supervisor Prof. Claus Rebholz (Department of Mechanical and Manufacturing Engineering, University of Cyprus, Nicosia, Cyprus), and my supervisor Prof. Christian Mitterer (Chair of Functional Materials and Materials Systems, Montanuniversität (MU) Leoben, Austria), for their proper guidance and endless support during the three years of my doctoral studies. Both had faith and confidence in me, offered drastic solutions on important issues, and I have benefited greatly from their advice. I sincerely acknowledge the significant contribution of researchers, collaborators and friends from different universities and institutes in terms of materials availability and experimental studies. At first, I am truly grateful to Prof. Biljana Babic and Prof. Branko Matovic from the University of Belgrade in Serbia (Institute of Physics and Vinča Institute of Nuclear Sciences, respectively) for their constant support in this work by providing promising carbon-based materials and invaluable feedback. In addition, I am very obliged to Prof. Georgios Constantinides from the Cyprus University of Technology (Lemesos, Cyprus), Prof. Kyriaki Polychronopoulou from the Khalifa University of Science and Technology (KUST, Abu Dhabi, UAE) as well as Dr. Mark Baker and Dr. Steve Hinder from the University of Surrey (Guildford, UK) for providing important experimental data and knowledge related to advanced characterization methods. Furthermore, my doctoral work has been significantly supported by the Institute of Nanoscience and Nanotechnology of the National Center of Scientific Research (NCSR) ‘’Demokritos’’ (Athens, Greece). More specifically, I am truly thankful to the research director of the HYSORB laboratory, Dr. Theodore Steriotis, for providing a constant and constructive feedback during the course of my doctoral studies and his Ph.D. student, Mr. Christos Tampaxis, for performing a great number of gas adsorption measurements. Referring to the same institute, I also express my gratitude to Dr. Athanassios Kontos, Dr. Konstantinos Giannakopoulos and Dr. Vasileios Tzitzios for all the structural characterization studies performed in their laboratories as well as the useful experimental data provided by their side. Sincere acknowledgments are given to Dr. Vladislav Ryzhkov from Fibrtec Inc. (Atlanta, USA) for the endless discussions on the interpretation of data derived from diffraction and spectroscopy methods and his very interesting ideas, as well as Mr. Ian Walters and Dr. Afshin Tarat from Perpetuus Carbon Technologies (Ammanford, UK) for providing a series of graphene-based materials I for our studies. Finally, I express my appreciation to the rest of the co-authors included in my papers that contributed to the completion of my work, including Mrs. Velislava Terziyska, Mr. Christian Koczwara, Dr. Christian Prehal and Prof. Oskar Paris from MU Leoben, Dr. Georgia Charalambopoulou, Dr. Aggeliki Papavasiliou, Dr. Maria Giannouri and Dr. Georgia Basina from NCSR Demokritos, as well as Prof. Charalabos Doumanidis, Dr. Yuanqing Li and Prof. Kin Liao from KUST. On a personal level, I would like to thank my parents, Konstantinos and Evgenia, my sisters, Kyriaki and Sofia, and my girlfriend Stela, for their constant support and encouragement in every aspect of my life. I am aware that my parents make tremendous sacrifices to ensure that we achieve our goals and this is the reason why I dedicate the current work to them. Nikolaos K. Kostoglou II Table of Contents List of Abbreviations and Symbols ....................................................................................................... V 1 Introduction ................................................................................................................................ 1 1.1 The alternative of hydrogen energy ............................................................................................. 1 1.2 The unique properties of hydrogen ............................................................................................. 4 2 The challenge of hydrogen storage ..................................................................................... 8 2.1 Terminology and definitions ........................................................................................................... 8 2.2 Technical targets and milestones .................................................................................................. 9 2.3 Technologies and methods ............................................................................................................ 11 2.3.1 Compressed hydrogen .......................................................................................................... 12 2.3.2 Liquefied hydrogen ................................................................................................................ 13 2.3.3 Cryo-compressed hydrogen ............................................................................................... 14 2.3.4 Solid-state hydrogen storage ............................................................................................. 15 2.3.4.1 Metal hydrides ....................................................................................................... 16 2.3.4.2 Porous adsorbents ............................................................................................... 17 3 Hydrogen adsorption in porous materials ..................................................................... 19 3.1 Terminology and definitions ........................................................................................................ 19 3.2 Basic principles of adsorption ...................................................................................................... 20 3.3 Classification of porous materials .............................................................................................. 22 3.4 Physical adsorption mechanisms ............................................................................................... 23 4 Materials and experimental methods .............................................................................. 26 4.1 Studied materials ............................................................................................................................... 26 4.1.1 Graphene-based nanostructures ..................................................................................... 26 4.1.2 Carbon nanotubes .................................................................................................................. 27 4.1.3 Activated carbons ................................................................................................................... 28 4.1.4 Beyond carbon – metal-organic frameworks ............................................................. 29 4.2 Nitrogen adsorption and desorption at 77 K ......................................................................... 30 4.2.1 Adsorption/desorption isotherms .................................................................................. 32 4.2.2 Total specific area – multi-point BET method ........................................................... 35 4.2.3 Total pore volume – single-point Gurvich rule .......................................................... 36 4.2.4 Micropore specific area and volume .............................................................................. 36 4.2.5 Pore size distribution ............................................................................................................ 37 4.2.6 Average pore size .................................................................................................................... 38 III 4.3 Hydrogen storage measurements .............................................................................................. 39 4.3.1 Low-pressure hydrogen adsorption ............................................................................... 39 4.3.2 High-pressure hydrogen adsorption .............................................................................. 40 5 Summary, conclusions and future work ......................................................................... 43 6 References ................................................................................................................................. 49 7 Publications .............................................................................................................................. 56
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