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HE0028 - Mg-Ni-Cu 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 mixtures' 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 ''free Mg'' and the ''bonded Mg'' intermetallic compounds Mg2Ni and Mg2Cu. After full activation (3 charging/ discharging runs), ''free Mg'' hydrogenates 10 times quicker than the ''bonded Mg phases'', while the discharging of both ''free'' and ''bonded'' Mg hydrides takes place simultaneously with similar kinetics. The best kinetic performance is shown by the samples with Mg ¼ 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. Ó


C. Milanese, A. Girella, G. Bruni, P. Cofrancesco, V. Berbenni, P. Matteazzi, A. Marini, Intermetallics xxx (2009) 1-9

HE0027 - Synthesis of carbon nanotube-TiO2 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 ?2-3 ?m) are grown on a Ti substrate, and MWCNTs a few ?m in length and ?30-60 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 films--measured both by hydrogenography and by Sievert's method--we 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) xxx-xxx

HE0025 - Reactivity and hydrogen storage performances of magnesium-nickel-copper 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 ðPH2 ¼ 5 barÞ 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 (¼3 h, 8 h and 16 h) strongly affects the properties of the ''as milled powders'' (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 ''free Mg'' and the intermetallic compounds Mg2Ni and Mg2Cu (''bonded Mg''): 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 ''bonded Mg'' with respect to binary Mg-Ni and Mg-Cu mixtures. On the contrary, Ni- and Cu-containing phases did not exert any appreciable destabilizing effect towards ''free MgH2''.


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 446-447 (2007) 345-349

HE0023 - Activation of hydrogen storage materials in the Li-Mg-N-H 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 Li-Mg-N-H 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 pressure-composition-isotherm (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) 334-338

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 B-H (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 20-40 ?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) 294-302

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]2â42DMFâ11H2Oâ20CH3OH, 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

HE0020 - An overview of advanced materials for hydrogen storage

In a future sustainable energy system based on renewable energy, environmentally harmless energy carriers like hydrogen will be of crucial importance. One of the major impediments for the transition to a hydrogen-based energy system is the lack of satisfactory hydrogen storage alternatives. In the last years, the possible to store hydrogen in various materials was extensively studied. This paper is a preliminary study with the focus on advanced nanostructured materials such as solids of large surface area based on carbon structures, metals and different types of metal alloys, other intermetallic compounds, etc. as possibilities for hydrogen storage. The newest materials used for hydrogen storage are light metal alloys. We have so far focused in this review almost exclusively on experimental studies. Also there are presented the most important characteristics of these materials such as mechanical strength, porosity and affinity to hydrogen, and also the recent developments in the search for innovative materials with high hydrogen-storage capacity and our contribution in this field.


Michael A. Miller and Richard A. Page FY 2006 Annual Progress Report DOE Hydrogen Program 529-534

HE0019 - In situ synthesis and hydrogen storage properties of PdNi alloy nanoparticles in an ordered mesoporous carbon template

Organized mesoporous carbon has been used as a nanoreactor to prepare PdNi metallic particles using an incipient wetness method starting from Pd and Ni salts. The final composite material consists of nanosized metallic particles of an alloy with composition Pd0.60Ni0.40 highly dispersed within the carbon host structure. The thermodynamic hydrogenation properties of both the PdNi-free OMC and the Pd0.60Ni0.40- OMC composite have been determined by hydrogen isotherm sorption measurements. The introduction of the palladium-nickel alloy into the carbon matrix does not increase the hydrogen storage capacity at 77 K and 2 MPa, since the hydrogen uptake is mainly attributed to physisorption on the carbon surface. However, at room temperature and moderate pressure (0.5 MPa), the filling of the OMC with nanocrystalline Pd0.60Ni0.40 results in larger hydrogen uptake than that of the PdNi-free OMC.


R. Campesi, F. Cuevas, R. Gadiou, E. Leroy, M. Hirscher, C. Vix-Guterl, M. Latroche, Microporous and Mesoporous Materials 117 (2009) 511-514

HE0018 - 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 Pd-10 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. Campesi, F. Cuevas, R. Gadiou, E. Leroy, M. Hirscher, C. Vix-Guterl, M. Latroche, Carbon 46 (2008) 206-214

HE0017 - Novel Sieverts' type volumetric measurements of hydrogen storage properties for very small sample quantities

Novel volumetric analysis instrument for studying hydrogen storage property of very small quantities (?mg) of samples was developed and tested. Small pressure change arising from hydrogen uptake or release are precisely measured and equated to the change in the sample's hydrogen content using the gas lawequation.Very small volume pressure reservoir enables these precise measurements, and all internal volumes are calibrated with high-purity helium gas. Capacity, equilibrium isotherm, and kinetic measurements can be performed in the pressure range of vacuum to 4MPa and the temperature range from cryogenic-673 K. Test measurements were made on small carbon nanotube samples and measurement of less than ?3 g of hydrogen uptake was demonstrated, which corresponds to an accuracy of better than 0.15 wt% for a 2 mg sample.


Yong-Won Lee, Bruce M. Clemens, Karl J. Gross, Journal of Alloys and Compounds 452 (2008) 410-413

HE0016 - Heat of adsorption for hydrogen in microporous high-surface-area materials

The automated Sieverts PCTPro2000 was used with a so-called Microdoser (MD) from HyEnergy, USA. This Microdoser offers the possibility to measure the hydrogen uptake of very small amounts of material. Therefore the MD includes a 0.51 ml reservoir, a pressure sensor and minimizes the sample cell volume to 1.2ml. The sample mass was between 99 mg and 400 mg and the samples have been activated in high vacuum according to table 1. Adsorption isotherms (0-20 bar) were measured at liquid nitrogen, liquid argon and temperatures above 87 K. Latter is realized by heating the sample cell in a dewar cooled by liquid nitrogen. The temperature was controlled to +/- 1 K.


B. Schmitz, U. Müller, N. Trukhan, M. Schubert, G. Férey, M. Hirscher, ChemPhysChem 2008

HE0015 - Heat of Adsorption for Hydrogen in Microporous High-Surface-Area Materials

The heat of adsorption for hydrogen is determined over a wide range of surface coverages for activated carbon and several metal-organic frameworks. Heat determination is based on hydrogen adsorption measurements performed at temperatures between 77 and 296 K (see figure, BTC=benzene-1,3,5-tricarboxylate). The materials with smaller cavities show a higher heat of adsorption for hydrogen.


Barbara Schmitz, Ulrich Müller, Natalia Trukhan,Markus Schubert,Gérard Férey and Michael Hirscher, ChemPhysChem 2008

HE0014 - Improved hydrogen storage properties of a V decorated Mg nanoblade array

An ultra-thin layer of V has been coated onto the surface of individual Mg nanoblades by dynamic shadowing growth. This 2.25 at% V decorated Mg nanoblade array can absorb and desorb hydrogen rapidly at temperatures T 500 K after activation by one hydrogen cycle, with a low hydrogen absorption activation energy of 35.0 ± 1.2 kJ per mol H2 and a desorption activation energy of 65.0 ± 0.3 kJ per mol H2. The improved hydrogen sorption kinetics is attributed to both the catalytic effect of the V coating and the unique nanoblade morphology with a large surface area and small hydrogen diffusion length


Yuping He and Yiping Zhao, Phys. Chem. Chem. Phys., 2009

HE0013 - The formation of MgH2 nanowires during the hydrogenation of Ti-doped Mg film

A unique diffusion barrier structure, consisting of layers of a Ti nanorod array and Ti film, has been fabricated on Si substrate for a subsequent 2 at.% Ti-doped Mg film deposition using a combinational technique of multilayer growth, co-deposition and dynamic shadowing growth. The hydrogenation of the Ti-doped Mg film on such a barrier structure shows that the barrier can prevent direct Mg-Si contact and suppress the formation of Mg2Si alloy in a high-temperature process. When this film has been hydrogenated at temperatures T 300 ?C for approximately 150 h, tetragonal single-crystal MgH2 nanowires are formed on the surface of the Ti-doped Mg film. The hydrogenation time and temperature are the two main factors for the nanowire formation. The doping of Ti also plays a significant role. This result reveals that complicated dynamic processes could occur during the hydrogenation of Ti-doped Mg film when Mg2Si formation can be eliminated by an effective diffusion barrier layer


Yuping He, Yongjun Liu and Yiping Zhao, Nanotechnology 19 (2008) 465602

HE0012 - Hydrogenation of Mg film and Mg nanoblade array on Ti coated Si substrates

The hydrogenation of Mg film and Mg nanoblade array fabricated on Ti coated Si substrates has been studied and compared. The nanoblades start to absorb hydrogen at a temperature between 250 and 300 °C, which is much lower than 350 °C for Mg film. However, the saturated total hydrogen uptake in nanoblades is less than half of that in the film, resulting from MgO formation by air exposure. The nanoblade morphology with large surface area and small hydrogen diffusion length, and the catalytic effect of Ti layer, are two main reasons for the nanoblade hydrogenation behavior.


Yuping He, Yiping Zhao, Liwei Huang, Howard Wang, and Russell J. Composto, APPLIED PHYSICS LETTERS 93, 163114 2008

HE0011 - Ternary nitrides for hydrogen storage: Li-B-N, Li-Al-N and Li-Ga-N 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 nitride.BN, 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 Li.Al.N 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 Li.Ga.N ternary system also stored a significant amount of hydrogen, the storage capacity for the Li.B.N system was near zero. The hydrogenation reaction is believed to be similar to that of Li3N, and the enthalpies of hydrogen absorption for Li.Al.N and Li.Ga.N 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) 287-292

HE0010 - Nanoporous Polymers for Hydrogen Storage

The study clearly demonstrates that hypercrosslinked nanoporous polymers with high hydrogen adsorption capacity are good candidates for use in future hydrogen storage systems. The major advantages of nanoporous polymers are light weight, and rapid complete adsorption and desorption with no appreciable hysteresis. Using a variety of well known reaction, these synthetic polymers can be easily modified and their adsorption ability further tuned.


Jonathan Germain, Jean M. J. Fréchet and Frantisek Svec, Polymeric Materials: Science & Engineering 2007, 97, 272

HE009 - Hypercrosslinked polyanilines with nanoporous structure and high surface area: potential adsorbents for hydrogen storage

A method for the preparation of an entirely new type of nanoporous material, hypercrosslinked polyaniline, with permanent porous structure and specific surface areas exceeding 630 m2 g21 has been developed. The hypercrosslinking reaction was carried out with commercial polyaniline and diiodoalkanes or paraformaldehyde using both conventional and microwave assisted processes. Polyaniline swollen in an organic solvent was hypercrosslinked to form a rigid, mesh-like structure with permanent porosity and a high surface area. The resulting materials were characterized using infrared spectroscopy and elemental analysis. Porous properties were determined by means of scanning electron microscopy as well as nitrogen and hydrogen adsorption. Short crosslinks such as those formed using paraformaldehyde and diiodomethane led to materials with the highest surface areas. Surface area also increased with the concentration of polyaniline in solution used during preparation. The hydrogen storage capacities of these materials were also tested and a capacity of 2.2 wt% at 77 K and 3.0 MPa was found for the best adsorbent. Hypercrosslinked polyanilines exhibit a remarkably high affinity for hydrogen, which results in enthalpies of adsorption as high as 9.3 kJ mol21 (exothermic), in sharp contrast with hypercrosslinked polystyrenes and metal-organic frameworks for which significantly lower enthalpies of adsorption, typically in the range of 4-7 kJ mol21, are measured.


Jonathan Germain, Jean M. J. Fréchet and Frantisek Svec, J. Mater. Chem., 2007, 17, 4989-4997


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