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Light Metal Hydrides for Reversible Hydrogen Storage Applications

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Light Metal Hydrides for Reversible Hydrogen Storage Applications University of Wollongong Research Online University of Wollongong Thesis Collection 1954-2016 University of Wollongong Thesis Collections 2015 Light metal hydrides for reversible hydrogen storage applications Guanglin Xia University of Wollongong, [email protected] Follow this and additional works at: https://ro.uow.edu.au/theses University of Wollongong Copyright Warning You may print or download ONE copy of this document for the purpose of your own research or study. The University does not authorise you to copy, communicate or otherwise make available electronically to any other person any copyright material contained on this site. You are reminded of the following: This work is copyright. Apart from any use permitted under the Copyright Act 1968, no part of this work may be reproduced by any process, nor may any other exclusive right be exercised, without the permission of the author. Copyright owners are entitled to take legal action against persons who infringe their copyright. A reproduction of material that is protected by copyright may be a copyright infringement. A court may impose penalties and award damages in relation to offences and infringements relating to copyright material. Higher penalties may apply, and higher damages may be awarded, for offences and infringements involving the conversion of material into digital or electronic form. Unless otherwise indicated, the views expressed in this thesis are those of the author and do not necessarily represent the views of the University of Wollongong. Recommended Citation Xia, Guanglin, Light metal hydrides for reversible hydrogen storage applications, Doctor of Philosophy thesis, School of Mechanical, Materials, and Mechatronic Engineering, University of Wollongong, 2015. https://ro.uow.edu.au/theses/4586 Research Online is the open access institutional repository for the University of Wollongong. For further information contact the UOW Library: [email protected] LIGHT METAL HYDRIDES FOR REVERSIBLE HYDROGEN STORAGE APPLICATIONS A thesis submitted in fulfilment of the requirements for the award of the degree DOCTOR of PHILOSOPHY From the UNIVERSITY OF WOLLONGONG By GUANGLIN XIA, B. Sc., M. Eng. INSITITUTE FOR SUPERCONDUCTING & ELECTRONIC MATERIALS, FACULTY OF ENGINEERING 2015 2 CERTIFICATION I, Guanglin Xia, declare that this thesis, submitted in fulfilment of the requirements for the award of Doctor of Philosophy, in the Institute for Superconducting & Electronic Materials, Faculty of Engineering, University of Wollongong, is wholly my own work unless otherwise referenced or acknowledged. The document has not been submitted for qualifications at any other academic institution. Guanglin Xia 2015.7.10 3 ABSTRACT Although hydrogen as a fuel has been extensively regarded as one of the best alternatives, because the exhaust gases in hydrogen-powered vehicles mainly contain water, storage of hydrogen in an efficient, safe, and economical method remains an unsolved challenge for its widespread use. Nanoconfinement has been widely verified to be an effective and efficient tool to relieve the high kinetic barriers and thermodynamic stability of various complex hydrides which have high gravimetric and volumetric hydrogen capacities.The objective of this thesis is to improve the hydrogen storage performance of certain complex hydrides, such as sodium zinc borohydride, lithium borohydride, lithium nitride, and lithium amidoborane, by taking advantage of nanoconfinement. Based on the special physical and chemical properties of different materials, a series of synthetic methods were designed, and the synergistic effects of space-confinement, nanosize, and morphology towards enhancing hydrogen storage performance have been investigated in detail. NaZn(BH4)3 with high purity was first synthesized by a wet-chemical method, which led to the formation of pure NaZn(BH4)3 solution in tetrahydrofuran, and nanoconfinement of NaZn(BH4)3 in mesoporous SBA-15 was successfully realized by typical solvent infiltration via capillary action. It was demonstrated that the nanoconfined NaZn(BH4)3 could desorb hydrogen at temperatures between 50 and 150 oC without the emission of diborane. Induced by the nanosize effect, the dehydrogenation kinetics was significantly improved, and the apparent activation -1 energy of NaZn(BH4)3 was reduced by 5.3 kJ mol . A famous reactive metal hydride composite of LiAlH4 and LiBH4 was successfully nanoconfined in mesoporous carbon via a typical infusion through the capillary effect. 4 By virtue of the synergistic effect between thermodynamic destabilization and nanoconfinement, the nanostructured 2LiBH4-LiAlH4 composite exhibited significantly improved hydrogen storage properties compared with its ball-milled counterpart, including the complete suppression of toxic diborane, a much lower hydrogen release temperature, and faster kinetics for dehydrogenation at a relatively lower temperature. More importantly, it was discovered that the thus-tailored thermodynamics and kinetics of the nanostructured composite laid the foundation for the extremely stable regeneration of Li3AlH6, which was realized for the first time without the addition of any catalysts. Overall, the capacity retention for the nd th nanoconfined 2LiBH4-LiAlH4 composite from the 2 to the 7 desorption remained over 98%, while lower than 15% was observed for the ball-milled composite, even after only 5 cycles. A simple one-pot method for the in-situ synthesis of three-dimensional (3D) porous carbon-coated Li3N nanofibers was developed and has been reported, based on a single-nozzle electrospinning technique with poly(vinyl alcohol) and LiN3 as the precursor. Due to the explosive release of N2 from the transformation of LiN3 into Li3N, which leads to the volume expansion of poly(vinyl alcohol) during heating, and the good distribution of LiN3 inside the as-electrospun nanofibers, 3D porous carbon- coated Li3N nanofibers were synthesized, which were full of mesopores and macropores. The mesoporous and macroporous structure provides favorable pathways for H2 delivery into and out of the of Li3N nanoparticles. The thus-fabricated Li3N nanofibers exhibit significantly improved thermodynamics and kinetics towards hydrogen storage performance compared with their bulk counterpart, which endows them with complete reversibility with a capacity close to the theoretical value at a temperature as low as 250 oC. This is the lowest temperature reported to date. More 5 importantly, it was found that the thus-tailored Li3N nanostructure features extremely stable regeneration without any apparent degradation after 10 de-/re-hydrogenation cycles at a temperature as low as 250 oC. Well-dispersed lithium amidoborane (LiAB) nanoparticles inside carbon nanofibers were fabricated by using carbon-coated Li3N nanofibers as the template. An abundance of micropores, mesopores, and macropores were generated during the formation of Li3N, which produced Li3N nanoparticles in-situ that were well-distributed and space- confined inside the separate pores, with sufficient space for the accommodation of ammonia borane to interact with Li3N, so that they serve as “smart” nanoreactors. Each Li3N nanoparticle is an active site separated by a porous carbon shell inside the porous carbon nanofibers and can initiate the formation of LiNH2BH3 via the reaction with AB with a molar ratio of 1:3 under the steric hindrance of the carbon coating, while simultaneously realizing the controllable synthesis of LiNH2BH3 with high loading, good dispersion, and robust stability. Taking advantage of the hierarchical porous architecture and the nanoscale size effects, the thus-formed LiNH2BH3 nanoparticles can release 10.6 wt.% hydrogen, approaching the theoretical value within only 15 min at a temperature as low as 100 oC. 6 ACKNOWLEDGEMENTS Firstly, I would like to express my gratitude to my supervisors Prof. Zaiping Guo and Prof. Huakun Liu for giving me the opportunity to work on this investigation. I wish to thank them for their expert guidance and support, discussions and encouragement, and giving me freedom during this research. I would also like to express my appreciation to Prof. Xuebin Yu from Fudan University for his great help and support. Other members from his group, such as Prof. Yanhui Guo, Dr. Yingbin Tan, Dr. Xiaowei Chen, Mr. Jiahao Su, Mrs. Jie Chen, Dr. Lijun Zhang, Mr. Ming Liang, Mrs. Yuqin Huang, Mrs. Meng Li, Mrs. Qili Gao, and Mr. Lei Wan are also gratefully acknowledged. Thanks also go to the staff, technicians, and my colleagues at ISEM, including Prof. Shixue Dou (Director), Mrs. Crystal Mahfouz (Administrative Officer), Mrs. Joanne George (Laboratory Officer), Dr. Tania Silver (paper and thesis editing), and others for their wonderful help. Also, I would like to thank all members of Prof. Guo’s group for their help, fruitful discussions and friendship, including Dr. Li Li, Dr. Dan Li, Mr. Tengfei Zhou, Mr. Hongqiang Wang, Dr. Chaofeng Zhang, and Mr Ruixiang Yu. I would like to express my deep appreciation and love to my entire family for their support, patience, and encouragement during all my studies. I would also like to thank my lovely wife Yanying Lv and my adorable daughter Xiaoyou Xia for the love and faith they have in me. It was my best gift to meet them during this study, and I love them forever with all my heart. 7 TABLE OF CONTENTS CERTIFICATION ..................................................................................................... 2 ABSTRACT ...............................................................................................................
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