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HE0040 - Ammine Magnesium Borohydride Complex as a New Material for Hydrogen Storage: Structure and Properties of Mg(BH4)2á2NH
The ammonia complex of magnesium borohydride Mg(BH4)2 á 2NH3 (I), which contains 16.0 wt % hydrogen, is a potentially promising material for hydrogen storage. This complex was synthesized by thermal decomposition of a hexaaammine complex Mg(BH4)2 á 6NH3 (II), which crystallizes in the cubic space group Fmø3m with unit cell parameter a ) 10.82(1) and is isostructural to Mg(NH3)6Cl2. We solved the structure of I that crystallizes in the orthorhombic space group Pcab with unit cell parameters a ) 17.4872(4) , b ) 9.4132(2) , c ) 8.7304(2) , and Z ) 8. This structure is built from individual pseudotetrahedral molecules Mg(BH4)2 á 2NH3 containing one bidentate BH4 group and one tridentate BH4 group that pack into a layered crystal structure mediated by N-Há á áH-B dihydrogen bonds. Complex I decomposes endothermically starting at 150 ¡C, with a maximum hydrogen release rate at 205 ¡C, which makes it competitive with ammonia borane BH3NH3 as a hydrogen storage material.
Grigorii Soloveichik, Jae-Hyuk Her, Peter W. Stephens, Yan Gao, Job Rijssenbeek, Matt Andrus, and J.-C. Zhao, Inorg. Chem., 2008, 47 (10), 4290-4298
HE0039 - Room temperature reversible hydrogen storage in polyaniline (PANI) nanofibers
We report for the first time the reversible hydrogen storage behavior at room temperature in polyaniline nanofibers. The rate of hydrogen sorption during the initial run was very rapid and an extended plateau pressure of about 30 bars was obtained from the pressure-composition isotherm profiles of these polyaniline nanofibers. The reversible cycling capacity of ~3-4 wt.% was demonstrated at room temperature and have been attributed due their unique microstructural and surface properties
Michael U. Jurczyk, Sesha S. Srinivasan, Ayala R. Phani, Ashok Kumar, D. Yogi Goswami, Elias K. Stefanakos
HE0038 - High-surface area biocarbons for reversible on-board storage of natural gas and hydrogen
An overview is given of the development of advanced nanoporous carbons as storage materials for natural gas (methane) and molecular hydrogen in on-board fuel tankss for next generation clean automobiles.
Peter Pfeiffer and al, Mater. Res. Soc. Symp. Proc. Vol. 1041 © 2008 Materials Research Society
HE0037 - Hydrogen Storage Properties of Ternary Nitrides Prepared by Mechanochemical Milling
Lithium nitride reacts with many elements or binary nitrides to form ternary nitrides. Synthesis procedures for ternary nitrides often involve solid-state reactions that require high temperatures. In the current work we prepare, for the first time, ternary nitrides based on both Li and Group 13 elements by mechanochemical milling of Li3N and the Group 13 nitrides Ð BN, AlN and GaN. The ternary nitrides obtained are not the known Li3XN2 systems and we have tentatively designated them as LiÐXÐN (where X = B, Al or Ga). We report here an investigation of the hydrogen absorptionÐdesorption behaviour of the LiÐXÐN ternary nitrides.
Henrietta W. Langmi, G. Sean McGrady, Poster
HE0036 - MixedÐMetal Li3NÐBased Systems for Hydrogen Storage: Li3AlN2 and Li3FeN2
The concept of destabilization has been employed by several groups working in the area of hydrogen storage by metal hydrides to identify and pursue systems with lower H2 desorption temperatures.
Henrietta W. Langmit, Scott D. Culligan and G. Sean McGrady, Poster
HE0035 - Sorption properties of NaBH4/MH2 (M[Mg, Ti) powder systems
The sorption properties of NaBH4/MH2 (M ? Mg, Ti) powder systems prepared by highenergy ball milling have been thoroughly investigated. Concerning the systems containing MgH2, the 2:1 and 1:2 molar compositions have been studied and both lead to a multistep desorption pathway, where the formation of MgB2 confirms the destabilization of NaBH4 induced by the presence of MgH2. A noticeable kinetic enhancement is achieved for the MgH2-rich system (composition 1:2) if compared with the NaBH4-rich system (composition 2:1). Even though full re-absorption is obtained for neither of the two compositions, fast kinetics is achieved. During absorption, the unsuspected formation of the perovskite-type hydride NaMgH3 is detected and it is showed that this ternary phase contributes to reduce the gravimetric capacity of the systems. Conversely, in the 2NaBH4/ TiH2 system, there is no formation of the intermetallic compound TiB2. Furthermore, a decrease in the sorption kinetics is found in comparison with the systems based on MgH2
S. Garroni, C. Milanese, A. Girella, A. Marini, G. Mulas, E. Menendez, C. Pistidda, M. Dornheim, S. Surinach, M.D. Baro, International journal of hydrogen energy 35 (2010) 5434-5441
HE0034 - Effect of C (graphite) doping on the H2 sorption performance of the MgÐNi storage system
Binary MgÐNi mixtures and ternary MgÐNiÐC (graphite) samples with fixed proportions of metals (Mg 85%ÐNi 15% by weight) and amount of C increasing in increments of 5 wt % from 5 wt % to 15 wt % were prepared by high energy ball milling (BM) in Ar for tBM ?2 h. The purpose of the study was to evaluate the effect of C addition on the reactivity, the sorption activation and the storage performance of the MgÐNi system. Increasing the amount of C had the effect of decreasing (from 10 to 3) the number of cycles needed for activation (performed at 623 K and 40 bar/0.9 bar charging/discharging H2 pressure). After full activation, the 5 wt % C-containing sample exhibited the best absorption kinetics performance: the average rate to charge up to 5 wt % H2 was about 3 times higher than that observed for the undoped sample. Unfortunately, increasing the amount of C had a negative impact on the desorption behaviour, causing an increase in the dehydrogenation activation energy and a decrease in the discharging rates. Within the present study, C reacted neither with H2 nor with the H2 active phases (the two discharged phases Mg and Mg2Ni and the related hydrides) and consequently did not lead to variation in the sorption enthalpies of the MgÐNi system. But, its presence did cause a small increase (4 K at 0.9 bar H2) in the minimum desorption temperatures of the hydrides and a consequent minor decrease (0.2 bar) in the equilibrium pressures. The best sorption properties were obtained for the 5 wt % C-sample, that on the whole worked better than the binary mixture.
C. Milanese, A. Girella, S. Garroni, G. Bruni, V. Berbenni, P. Matteazzi, A. Marini, International journal of hydrogen energy xx (2009) 1-11
HE0033 - Thermodynamics of hydrogen adsorption in MOF-177 at low temperatures:measurements and modelling
Hydrogen adsorption measurements and modelling for the Zn-based microporous metalÐorganic framework (MOF) Zn4O(1,3,5-benzenetribenzoate)2, MOF-177, were performed over the 50Ð77 K and 0Ð40 bar ranges. The maximum excess adsorption measured under these conditions varies over about 105Ð70 mg g?1. An analysis of the isotherms near saturation shows that hydrogen is ultimately adsorbed in an incompressible phase whose density is comparable to that of the bulk liquid. These liquid state properties observed under supercritical conditions reveal a remarkable effect of nanoscale confinement. The entire set of adsorption isotherms can be well described using a micropore filling model. The latter is used, in particular, to determine the absolute amounts adsorbed and the adsorption enthalpy. When expressed in terms of absolute adsorption, the isotherms show considerable hydrogen storage capacities, reaching up to 125 mg g?1 at 50 K and 25 bar. The adsorption enthalpies are calculated as a function of fractional filling and range from 3 to 5 kJ mol?1 in magnitude, in accordance with physisorption. These results are discussed with respect to a similar analysis performed on another Zn-based MOF, Zn4O(1,4-benzenedicarboxylate)3, IRMOF-1, presented recently. It is found that both materials adsorb hydrogen by similar mechanisms.
Eric Poirier and Anne Dailly, Nanotechnology 20 (2009) 204006
HE0032 - Structure and Charge Control in MetalÐOrganic Frameworks Based on the Tetrahedral Ligand Tetrakis(4-tetrazolylphenyl)methane
Use of the tetrahedral ligand tetrakis(4-tetrazolylphenyl)methane enabled isolation of two three-dimensional metalÐorganic frameworks featuring 4,6- and 4,8-connected nets related to the structures of garnet and fluorite with the formulae Mn6-(ttpm)3á5DMFá3H2O (1) and Cu-(Cu4Cl)(ttpm)2]2áCuCl2á5DMFá11H2O (2) (H4ttpm=tetrakis(4-tetrazolylphenyl) methane). The fluorite-type solid 2 displays an unprecedented post-synthetic transformation in which the negative charge of the framework is reduced by extraction of copper(II) chloride. Desolvation of this compound generates Cu4(ttpm)2á0.7CuCl2 (2d), a microporous material exhibiting a high surface area and significant hydrogen uptake
Mircea Dinca, Anne Dailly and Jeffrey R. Long, Chem. Eur. J. 2008, 14, 10280 Ð 10285
HE0031 - Ternary nitrides for hydrogen storage: LiÐBÐN, LiÐAlÐN and LiÐGaÐN systems
This paper reports an investigation of hydrogen storage performance of ternary nitrides based on lithium and the Group 13 elements boron, aluminum and gallium. These were prepared by ball milling Li3N together with the appropriate Group 13 nitrideÑBN, AlN or GaN. Powder X-ray diffraction of the products revealed that the ternary nitrides obtained are not the known Li3BN2, Li3AlN2 and Li3GaN2 phases. At 260 ?C and 30 bar hydrogen pressure, the LiÐAlÐN ternary system initially absorbed 3.7wt.% hydrogen, although this is not fully reversible. We observed, for the first time, hydrogen uptake by a pristine ternary nitride of Li and Al synthesized from the binary nitrides of the metals. While the LiÐGaÐN ternary system also stored a significant amount of hydrogen, the storage capacity for the LiÐBÐN system was near zero. The hydrogenation reaction is believed to be similar to that of Li3N, and the enthalpies of hydrogen absorption for LiÐAlÐN and LiÐGaÐN provide evidence that AlN and GaN, as well as the ball milling process, play a significant role in altering the thermodynamics of Li3N.
Henrietta W. Langmi, G. Sean McGrady, Journal of Alloys and Compounds 466 (2008) 287Ð292
HE0030 - Hydrogen storage properties of Pd nanoparticle/carbon template composites
Theoretical studies predict improved hydrogenation properties for hybrid carbon/metal composites. The hydrogen storage capacity of ordered porous carbon containing Pd clusters was measured. The C/Pd composite was obtained by chemical impregnation of an ordered porous carbon template (CT) with a H2PdCl4 solution followed by a reduction treatment. 10 wt.% of palladium clusters were introduced in the carbon porosity; the Pd clusters (2 nm in size) being homogeneously distributed. Thermodynamic hydrogenation properties of both Pd-free CT and the PdÐ10 wt.% CT composite have been determined by hydrogen isotherm sorption measurements and thermal desorption spectroscopy (TDS) analysis. The introduction of the palladium into the carbon matrix does not increase the hydrogen storage capacity at 77 K and 1.6 MPa, since here the hydrogen uptake is being attributed to physisorption on the carbon. However, at room temperature and moderate pressure (0.5 MPa), the filling of the CT with 10 wt.% nanocrystalline Pd results in an hydrogen uptake eight times larger than that of the Pd-free CT. After the second cycle, a good reversibility is observed. TDS measurements confirm that the sharp increase of the hydrogen uptake is due to the presence of the Pd clusters in the carbon porosity
R. Campesia, F. Cuevas, R. Gadiou, E. Leroy, M. Hirscher, C. Vix-Guterl, M. Latroche, Carbon 46 (2008 ) 206 Ð214
HE0029 - H2 sorption performance of NaBH4ÐMgH2 composites prepared by mechanical activation
The current research on solid state hydrogen storage materials for on-board applications is focused on reactive hydrides composites (RHC), i.e. systems based on the improvement of the dehydrogenation thermodynamic of a complex hydride when one (generally the light hydride MgH2) or more hydrides take part to the reaction. The extent of the destabilization, as well as the sorption characteristics of the composites, strongly depends on the structural and nanostructural properties of the constituent hydrides, which are in turn affected by the preparation route. The aim of this work is to evaluate the influence of different mechanical activation conditions on the storage properties of NaBH4 Ð MgH2 composites, up to now scarcely explored in literature. The first results regard composites with 2:1 and 1:2 stoichiometry milled under different atmosphere (Ar or H2). X-ray powders diffraction analysis shows that milling does not lead to the formation of any new phase, but it reduces the average crystallite size of the powders down to nanometric scale. All the mixtures release an H2 amount close to the theoretical value expected for the full dissociation of both the hydrides and much higher than the target fixed by the US Department of Energy for on-board application. The thermal programmed desorption profiles of the mixtures clearly show two steps, with MgH2 dissociating first and with higher rate and NaBH4 gradually dehydrogenating at temperatures close to 400¡C. Concerning the 2:1 stoichiometry, when the samples are processed under Ar the two dehydrogenation processes are characterized by a lower starting temperature but also by a lower average rate with respect to the sample milled in H2. The 1:2 sample milled under Ar shows the best kinetic performance. Unfortunately, also for this mixture more than 10 h are required to obtain full desorption at a temperature as high as 450¡C.
C. Milanese, A. Girella, G. Mulas, S. Enzo, S. Medici, S. Garroni, M. D. Bar, S. Suri-ach & A. Marini, Ecosystems and Sustainable Development VII 389
HE0028 - MgÐNiÐCu mixtures for hydrogen storage: A kinetic study
Mg-based ternary mixtures (40 Mg wt% 80) containing increasing amount (up to 30 wt %) of Ni and Cu were prepared by ball milling (BM) under Ar for 16 h and subsequently activated at high temperature (623 K) by charging/discharging cycles at H2 pressure of 50 bar/0.7 bar. The work aims to analyze the influence of the mixturesÕ composition on the storage properties (H2 intake and sorption kinetics) and to describe the role played by an ad-hoc activation in reaching these same properties. The storage capacity of the mixtures decreases by decreasing the Mg starting content, the H2 active phases being ÔÔfree MgÕÕ and the ÔÔbonded MgÕÕ intermetallic compounds Mg2Ni and Mg2Cu. After full activation (3 charging/ discharging runs), ÔÔfree MgÕÕ hydrogenates 10 times quicker than the ÔÔbonded Mg phasesÕÕ, while the discharging of both ÔÔfreeÕÕ and ÔÔbondedÕÕ Mg hydrides takes place simultaneously with similar kinetics. The best kinetic performance is shown by the samples with Mg ? 60 wt% and 70 wt% and the highest Ni content (30% and 20% respectively), with sorption rates up to 7 times higher than those of the pure Mg/ MgH2 system. î
C. Milanese, A. Girella, G. Bruni, P. Cofrancesco, V. Berbenni, P. Matteazzi, A. Marini, Intermetallics xxx (2009) 1Ð9
HE0027 - Synthesis of carbon nanotubeÐTiO2 nanotubular material for reversible hydrogen storage
A material consisting of multi-walled carbon nanotubes (MWCNTs) and larger titania (TiO2) nanotube arrays has been produced and found to be efficient for reversible hydrogen (H2) storage. The TiO2 nanotube arrays (diameter ?60 nm and length ?2Ð3 ?m) are grown on a Ti substrate, and MWCNTs a few ?m in length and ?30Ð60 nm in diameter are grown inside these TiO2 nanotubes using chemical vapor deposition with cobalt as a catalyst. The resulting material has been used in H2 storage experiments based on a volumetric method using the pressure, composition, and temperature relationship of the storage media. This material can store up to 2.5 wt% of H2 at 77 K under 25 bar with more than 90% reversibility.
Amrita Mishra, Subarna Banerjee, Susanta K Mohapatra, Olivia A Graeve and Mano Misra, Nanotechnology 19 (2008) 445607
HE0026 - Effect of the substrate on the thermodynamic properties of PdHx films studied by hydrogenography
We investigated the influence of the substrate on the thermodynamic properties of metal hydride thin films by hydrogenography, using PdHx as a model system. After appropriate hydrogen cycling, reproducible hydrogenation properties are found at the same equilibrium pressure for all substrates studied. Comparing these thin films with free-standing filmsÑmeasured both by hydrogenography and by SievertÕs methodÑwe find a very similar behavior. Hence, thin films can be used to study the hydrogenation behavior of the corresponding bulk materials.
Y. Pivak, R. Gremaud, K. Gross, M. Gonzalez-Silveira, A. Walton, D. Book,H. Schreuders, B. Dama and R. Griessen, Scripta Materialia xxx (2008) xxxÐxxx
HE0025 - Reactivity and hydrogen storage performances of magnesiumÐnickelÐcopper ternary mixtures prepared by reactive mechanical grinding
Ternary Mg-based mixtures (50 Mg weight% 80) containing increasing amount of Ni (up to 30 wt%) and Cu (up to 20 wt%) have been prepared by ball milling in hydrogen reactive atmosphere ?PH2 ? 5 bar? to determine the effects of both the processing conditions and the concurrent presence of the two transition metals on the sorption mechanisms and the storage properties of the Mg/MgH2 system. Combined SEM, TG and XRPD analyses showed that the processing time tBM (?3 h, 8 h and 16 h) strongly affects the properties of the ÔÔas milled powdersÕÕ (average particle sizes and microstructure, nature of the phases, amount of hydrogen absorbed upon milling, and desorption characteristics). However, after a combined high temperature/high pressure activation cycle, all the charged samples were composed of MgH2, Mg2NiH4 and MgCu2 while the discharged samples contained ÔÔfree MgÕÕ and the intermetallic compounds Mg2Ni and Mg2Cu (ÔÔbonded MgÕÕ): in all cases the definitive storage performances are related only on the relative amounts of these three phases that, in turn, depend on the starting composition of the mixtures. Both Ni- and Cu-containing phases hydrogenated/dehydrogenated according to their own sorption reaction schemes; however, Mg2NiH4 and MgCu2 destabilized each other, with the beneficial effect of rising the desorption plateau pressures of the ÔÔbonded MgÕÕ with respect to binary MgÐNi and MgÐCu mixtures. On the contrary, Ni- and Cu-containing phases did not exert any appreciable destabilizing effect towards ÔÔfree MgH2ÕÕ.
C. Milanese, A. Girella, G. Bruni, P. Cofrancesco, V. Berbenni, M. Villa, P. Matteazzi, A. Marini , International Journal of Hydrogen Energy 33 (2008) 4593-4606
HE0024 - Hydrogen storage properties of 2LiNH2 + LiBH4 +MgH2
We have investigated the ternary mixture of complex hydrides with stoichiometry 2LiNH2 + LiBH4 +MgH2, and have identified a set of novel hydrogen storage reactions. One of these reactions involves the known reversible reaction Mg(NH2)2 + 2LiH?Li2Mg(NH)2 +2H2. Previous studies have shown that initiating this reaction from the binary mixture 2LiNH2 +MgH2 results in poor hydrogen desorption kinetics and a small amount of NH3 release. In contrast to this behavior, here we demonstrate that by starting from the ternary mixture 2LiNH2 + LiBH4 +MgH2, the above reaction can proceed at lower temperatures and with improved kinetics, while maintaining reversibility. The advantage of starting with the ternary mixture can be traced to the subsequent formation, melting, and reaction of Li4BH4(NH2)3 with MgH2 to form the mixed imide phase Li2Mg(NH)2, which acts as a seed for the reversible reaction, and is at least partly responsible for the improved kinetic response
Jun Yang, Andrea Sudik, Donald J. Siegel, Devin Halliday, Andy Drews, Roscoe O. Carter III, Christopher Wolverton, Gregory J. Lewis, J.W.A. Sachtler, John J. Low, Syed A. Faheem, David A. Lesch, Vidvuds Ozolins, Journal of Alloys and Compounds 446Ð447 (2007) 345Ð349
HE0023 - Activation of hydrogen storage materials in the LiÐMgÐNÐH system:Effect on storage properties
We investigate the thermodynamics, kinetics, and capacity of the hydrogen storage reaction: Li2Mg(NH)2 +2H2?Mg(NH2)2 + 2LiH. Starting with LiNH2 and MgH2, two distinct procedures have been previously proposed for activating samples to induce the reversible storage reaction. We clarify here the impact of these two activation procedures on the resulting capacity for the LiÐMgÐNÐH reaction. Additionally, we measure the temperature-dependent kinetic absorption data for this hydrogen storage system. Finally, our experiments confirm the previously reported formation enthalpy ( H), hydrogen capacity, and pressureÐcompositionÐisotherm (PCI) data, and suggest that this system represents a kinetically (but not thermodynamically) limited system for vehicular on-board storage applications.
Jun Yang, Andrea Sudik, C. Wolverton, Journal of Alloys and Compounds 430 (2007) 334Ð338
HE0022 - Nanocatalyst doping of Zn(BH4)2 for on-board hydrogen storage
In this work, we report the synthesis and characterization of Zn(BH4)2, a new class of complex borohydrides for on-board hydrogen storage. The thermal decomposition of Zn(BH4)2 comprises of not only the evolution of H2, but also an appreciable amount of BÐH (borane) compounds. Lowering the decomposition temperature by catalytic doping may lead to negligible release of boranes. An amount of 1.5 mol% nanoNi was estimated and found to be the optimum concentration for nanocatalyst doping of Zn(BH4)2. Significance of the nanoNi doping, lowers the melting and thermal decomposition temperatures (at least 20Ð40 ?C) of Zn(BH4)2 as evidenced from the calorimetric analysis. At these low temperatures, the nanocatalyzed Zn(BH4)2 exhibits reduction in the amount of borane gases released by a factor of 20 as compared to the undoped sample
Sesha Srinivasan, Diego Escobar, Michael Jurczyk, Yogi Goswami, Elias Stefanakos, Journal of Alloys and Compounds 462 (2008) 294Ð302
HE0021 - Hydrogen Storage in a Microporous Metal-Organic Framework with Exposed Mn2+ Coordination Sites
Use of the tritopic bridging ligand 1,3,5-benzenetristetrazolate (BTT3-) enables formation of [Mn- (DMF)6]3[(Mn4Cl)3(BTT)8(H2O)12]242DMF11H2O20CH3OH, featuring a porous metal-organic framework with a previously unknown cubic topology. Crystals of the compound remain intact upon desolvation and show a total H2 uptake of 6.9 wt % at 77 K and 90 bar, which at 60 g H2/L provides a storage density 85% of that of liquid hydrogen. The material exhibits a maximum isosteric heat of adsorption of 10.1 kJ/mol, the highest yet observed for a metal-organic framework. Neutron powder diffraction data demonstrate that this is directly related to H2 binding at coordinatively unsaturated Mn2+ centers within the framework.
Mircea Dinca ,Anne Dailly, Yun Liu, Craig M. Brown, Dan. A. Neumann and Jeffrey R. Long, J. AM. CHEM. SOC. 2006, 128, 16876-16883
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- April 30, 2012 - May 03, 2012
Carbon Capture Utilization & Sequestration
Pittsburgh, Pennsylvania - United States 11th Annual Conference on Carbon Capture Utilization & Sequestration April 30 - May 3, 2012Pittsburgh, Pennsylvania The 2012 Conference program follows in the footsteps of the past 10 events, with an added emphasis this year on potential utilization of anthropogenic carbon emissions that is reflected in the new name of the conference. The focus is on systems and technologies that are being or could be deployed in the U.S. and North America.
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