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Physical and Chemical Destabilization of Ammonia Borane for an Improved Hydrogen Storage System

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Physical and Chemical Destabilization of Ammonia Borane for an Improved Hydrogen Storage System UNIVERSIDAD AUTÓNOMA DE MADRID FACULTAD DE CIENCIAS Dpto. de QUÍMICA FÍSICA APLICADA Physical and chemical destabilization of ammonia borane for an improved hydrogen storage system Desestabilización de borano de amoníaco por métodos físicos y químicos: hacia un mejor sistema de almacenamiento de hidrógeno MEMORIA Para aspirar al grado de DOCTOR EN CIENCIAS QUÍMICAS con Mención Doctor Internacional MARIA JOSÉ VALERO PEDRAZA Instituto de Catálisis y Petroleoquímica (CSIC) Madrid, 2015 MARIA JOSÉ VALERO PEDRAZA Physical and chemical destabilization of ammonia borane for an improved hydrogen storage system Desestabilización de borano de amoníaco por métodos físicos y químicos: hacia un mejor sistema de almacenamiento de hidrógeno MEMORIA Para aspirar al grado de DOCTOR EN CIENCIAS QUÍMICAS con Mención Doctor Internacional Dirigida por Prof. Dr. Miguel Ángel Bañares González Profesor de Investigación Instituto de Catálisis y Petroleoquímica (CSIC) Dr. Ángel Martín Martínez Profesor Universidad de Valladolid UNIVERSIDAD AUTÓNOMA DE MADRID FACULTAD DE CIENCIAS Dpto. de QUÍMICA FÍSICA APLICADA Madrid, 2015 Summary The worlwide energy demand, estimated to be 10,000 million tonnes oil equivalent is currently covered in more than 87 % by fossil fuels such as coal, petroleum or natural gas. This strong dependency brings economic and environmental impacts and is not sustainable in the long term. Therefore, public institutions point to a necessary and controlled transition towards a clean, reliable and safe energy structure. One of the possible alternative is electrical combustion of hydrogen used as an energy vector in fuel cells. But for such transition to the so called “hydrogen economy” to be achieved, the challenge of finding efficient ways to store and deliver hydrogen to mobile devices has to be solved as; due to its low energy density, huge volumes of hydrogen would be necessary to feed high energy consuming processes. One of the most promising approaches in this sense is the solid storage of hydrogen using complex hydrides of light elements among which aminoboranes (R(NH2BH3)n). Up to now, ammonia borane stands as the most intensively studied compound from this group due to its high stability, easy handling and considerable hydrogen density. But ammonia borane decomposition also exhibits some drawbacks as its excessive exothermicity that hampers regeneration of the residue thus impeding reversibility of the process; low kinetics at the working temperature for fuel cells (85 ºC) and the concomitant release of volatile impurities simultaneous to hydrogen as are ammonia, diborane or borazine which are highly undesirable because they can poison the catalyst from fuel cell electrodes. But despite these hurdles, ammonia borane still remains a promising alternative for hydrogen reversible storage on account of its impressive safety features and high hydrogen content of 19.6 wt.%. Furthermore, ammonia borane offers the combination of hydridic B-H and protonic N-H bounds enclosed in the same molecule thus appearing considerably destabilized compared to the amide parent compound. Thus, many recent studies focused on reducing the decomposition temperature, improving kinetics of hydrogen release while minimizing borazine desorption during ammonia borane thermal decomposition. Some interesting works showed that hydrides with nanosized particles exhibit significantly improved kinetics properties for reversible hydrogen storage when compared to the neat material. In this context, one of the most promising approaches consists in confining ammonia borane in porous materials to reduce its particles size and fine tune thermodynamics and kinetics of thermal decomposition. i The research group in which this thesis work was carried out is strongly experienced in temperature programmed in-situ Raman studies with online analysis of released gases by mass spectrometry (MS) conforming the so-called operando Raman-MS system. Such studies allow following details of the structural evolution of the material under working conditions (in-situ Raman spectroscopy) simultaneously to the detection of hydrogen and volatiles release (online mass spectrometry), thus performing a real-time study of structure/activity relationship. This Thesis focuses on the study of compounds based on ammonia borane for solid hydrogen storage by means of the operando Raman-MS technique, among others. This is a novel approach for investigating aminoboranes decomposition processes. In a first part of the study, the effect of confining ammonia borane onto the pores of several porous materials such as mesoporous silica and metal oxides was investigated. Samples of ammonia borane impregnated into materials offering different porosities and compositions applying different loading levels on one the support were prepared and characterized thus evaluating both the effects of porosity and ammonia borane loading level. Previously, the effect of the solvent used during the incipient wetness impregnation to support ammonia borane on the porous materials is evaluated. It was demonstrated that recrystallization of ammonia borane from different solvents produces small morphological variations, but without changes in structural properties. The operando Raman-MS results corroborated a nucleation and growth mechanism for ammonia borane decomposition samples. Several characterization techniques were used to evaluate the confinement of ammonia borane in the pores of the supports and to detect possible changes in thermodynamics of ammonia borane decomposition when impregnated to thus check which porous material can decrease dehydrogenation temperature to values below 100 ºC. Impregnation of ammonia borane onto porous materials has been shown to improve the kinetic performance, but limited by the amount of ammonia borane that can be impregnated in mesoporous Ga2O3 as considerable improvement in H2 desorption properties in terms of lowered temperature and kinetics were observed for the 0.5:1 AB/Ga2O3 samples in which decomposition proceeds to a one-step mechanism. The same effects were observed for mesoporous SBA-15 materials for an ammonia borane 1:1 loading level as the porosity of these supports is much more accessible with a higher pores volume to host ammonia borane. All the AB/Ga2O3 materials were shown to induce simultaneous NH3 desorption probably due to interactions between the support surface and ammonia borane particles. ii In the second part of this Thesis, another aminoborane compound, ethane 1,2-diaminebisborane (CH2NH2BH3)2, was synthetized and characterized. Hydrogen release features for this compound were quite different from those for ammonia borane as ethane 1,2-diaminebisborane offers a decomposition temperature higher than that of ammonia borane with faster hydrogen release and no concomitant borazine desorption. Several characterization techniques were applied to compare thermodynamics properties of ethane 1,2-diaminebisborane dehydrogenation and ammonia borane. The results show that EDAB presents a thermal stability higher than that of ammonia borane under both, vacuum and inert gas flow. Contrary to this compound, EDAB releases pure hydrogen when heated under inert flow while moderate fractions of diborane, residual tetrahydrofuran, and volatile B−N−C−H species were released under dynamic vacuum. The bonding properties of the reaction products were investigated based on the operando Raman-MS and NMR studies of the thermolytic decomposition of EDAB and a reaction scheme was proposed for this process which slightly differs from the one described in the literature. In the last part of this Thesis, ammonia borane thermal decomposition in various ionic liquids was studied. Ionic liquids are solid salts with low melting temperatures that are even liquid at room temperature in some cases. Besides dissolving ammonia borane, ionic liquids offer low volatility, they are stable at high temperatures, they can be easily recovered with low activity loss and they exhibit an impressive chemical inertia that make of them a suitable environment for controlled thermal decomposition of ammonia borane. It was shown in previous studies on the thermal decomposition of ammonia borane in ionic liquids that they high polarity stabilized diammonate of diborane, the intermediate decomposition compound thus considerably reducing the induction period necessary for this species to be formed during neat ammonia borane decomposition. Besides, hydrogen yield was also enhanced in some of the tested ammonia borane/ionic liquids dissolutions under isothermal conditions close to the working temperature of fuel cells. In this Thesis work, ionic liquids that weren´t previously tested were used to dissolve ammonia borane. While most of these dissolutions exhibited similar properties to those previously described in literature, it was seen that by using ionic liquids with bis(trifluoromethylsulfanyl) imide Tf2N anion, the foaming problem was reduced and in some cases, the residue remained dissolved in the ionic liquid. This is a unique feature, never reported up to now, which may facilitate recycling of the material by rehydrogenation of ammonia borane. It was also observed that some ionic liquids, that contained choline cation (2-hydroxy-N,N,N-trimethylethanaminium ), showed very high hydrogen yields. This may be caused by ammonia borane thermolysis proceeding through an alternative route which is supported by IR characterization of the residue. iii The complete study on dehydrogenation processes for these materials based
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