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PROPERTIES and STRUCTURES of Li-N BASED HYDROGEN STORAGE MATERIALS

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PROPERTIES and STRUCTURES of Li-N BASED HYDROGEN STORAGE MATERIALS Michigan Technological University Digital Commons @ Michigan Tech Dissertations, Master's Theses and Master's Dissertations, Master's Theses and Master's Reports - Open Reports 2013 PROPERTIES AND STRUCTURES OF Li-N BASED HYDROGEN STORAGE MATERIALS Junqing Zhang Michigan Technological University Follow this and additional works at: https://digitalcommons.mtu.edu/etds Part of the Materials Chemistry Commons, and the Physical Chemistry Commons Copyright 2013 Junqing Zhang Recommended Citation Zhang, Junqing, "PROPERTIES AND STRUCTURES OF Li-N BASED HYDROGEN STORAGE MATERIALS", Dissertation, Michigan Technological University, 2013. https://doi.org/10.37099/mtu.dc.etds/579 Follow this and additional works at: https://digitalcommons.mtu.edu/etds Part of the Materials Chemistry Commons, and the Physical Chemistry Commons PROPERTIES AND STRUCTURES OF Li-N BASED HYDROGEN STORAGE MATERIALS By Junqing Zhang A DISSERTATION Submitted in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY In Materials Science and Engineering MICHIGAN TECHNOLOGICAL UNIVERSITY 2013 © 2013 Junqing Zhang This dissertation has been approved in partial fulfillment of the requirements for the Degree of DOCTOR OF PHILOSOPHY in Materials Science and Engineering. Department of Materials Science and Engineering Dissertation Advisor: Yun Hang Hu Committee Member: Jaroslaw W. Drelich Committee Member: Stephen A. Hackney Committee Member: Feng Zhao Department Chair: Stephen L. Kampe Table of Contents List of Figures ........................................................................................................... viii List of Tables .............................................................................................................. xi Preface ....................................................................................................................... xii Acknowledgements .................................................................................................. xiv List of Abbreviations ................................................................................................ xvi Abstract .................................................................................................................... xvii Chapter 1 Background .................................................................................................. 1 1.1 Why choosing hydrogen as fuel for transportation? ........................................... 1 1.2 Hydrogen storage targets .................................................................................... 3 1.3 Technologies for hydrogen storage ..................................................................... 4 1.3.1 Compressing hydrogen ................................................................................. 5 1.3.2 Liquefying hydrogen .................................................................................... 6 1.3.3 Physical adsorption ...................................................................................... 8 1.3.4 Metal hydrides .............................................................................................. 9 1.3.5 Complex hydrides ...................................................................................... 10 1.3.6 Clathrate ..................................................................................................... 11 1.4 Lithium nitride for hydrogen storage ................................................................ 11 1.5 Lithium nitride crystal structure and optical property ...................................... 15 1.5.1 Crystal structure ......................................................................................... 15 1.5.2 Optical property ......................................................................................... 17 1.6 Lithium nitride halides structure and properties ............................................... 18 1.7 Scope of this study ............................................................................................ 19 Chapter 2 Decomposition of lithium amide * ............................................................ 21 2.1 Introduction ....................................................................................................... 21 2.2 Experiments ...................................................................................................... 22 2.2.1 Sample preparations ................................................................................... 22 2.2.2 Temperature-programmed decomposition ................................................. 23 2.2.3 X-ray diffraction (XRD) ............................................................................ 24 v 2.3 Results and discussion ...................................................................................... 25 2.4 Conclusion ........................................................................................................ 32 Chapter 3 Decomposition of lithium imide * ............................................................. 33 3.1 Introduction ...................................................................................................... 33 3.2 Experiments and kinetic calculation method .................................................... 34 3.2.1 Sample preparations ................................................................................... 34 3.2.2 Temperature-programmed decomposition ................................................. 34 3.2.3 X-ray diffraction (XRD) ............................................................................ 35 3.2.4 Kinetic calculation method for TPD-TCD peaks ...................................... 35 3.3 Results and discussion ...................................................................................... 39 3.4 Conclusion ........................................................................................................ 52 Chapter 4 Effect of anion promoter Cl- on the decomposition of lithium amide * .... 53 4.1 Introduction ...................................................................................................... 53 4.2 Experiments ...................................................................................................... 57 4.2.1 Sample preparations ................................................................................... 57 4.2.2 Temperature-programmed decomposition ................................................. 57 4.2.3 X-ray diffraction (XRD) ............................................................................ 58 4.3 Results and discussion ...................................................................................... 58 4.4 Conclusion ........................................................................................................ 63 Chapter 5 Chemical stability of lithium nitride in air* .............................................. 64 5.1 Introduction ...................................................................................................... 64 5.2 Experiments ...................................................................................................... 66 5.2.1 Treatment of Li3N in O2............................................................................. 66 5.2.2 Degradation of Li3N in air ......................................................................... 66 5.2.3 Characterization ......................................................................................... 67 5.3 Results and discussion ...................................................................................... 69 5.3.1 Oxidation of Li3N in O2 ............................................................................. 69 5.3.2 Effect of H2O in air on Li3N ...................................................................... 70 5.4 Conclusion ........................................................................................................ 76 Chapter 6 Chemical stability of lithium nitride bromide Li13N4Br in air * ............... 78 vi 6.1 Introduction ....................................................................................................... 78 6.2 Experiments ...................................................................................................... 80 6.2.1 Lithium nitride bromide Li13N4Br preparation .......................................... 80 6.2.2 X-ray diffraction (XRD) ............................................................................ 80 6.2.3 Temperature-programmed decomposition mass spectroscopy (TPD-MS) 81 6.2.4 Ultraviolet−visible (UV-vis) absorption .................................................... 82 6.3 Results and discussion ...................................................................................... 82 6.3.1 XRD and TPD-MS analysis ....................................................................... 82 6.3.2 UV-vis absorption analysis ........................................................................ 87 6.4 Conclusion ........................................................................................................ 95 Chapter 7 Summary .................................................................................................... 97 References .................................................................................................................. 99 Appendix .................................................................................................................. 118 vii List of Figures Figure
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