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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 palladiumÐnickel 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) 511Ð514
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 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. Campesi, F. Cuevas, R. Gadiou, E. Leroy, M. Hirscher, C. Vix-Guterl, M. Latroche, Carbon 46 (2008) 206-214
HE0017 - Novel SievertsÕ 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 sampleÕs 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) 410Ð413
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. Mller, N. Trukhan, M. Schubert, G. Frey, 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 metalÐorganic 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 Mller, Natalia Trukhan,Markus Schubert,Grard Frey 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 MgÐSi 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: 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 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) 287Ð292
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. Frchet 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 metalÐorganic frameworks for which significantly lower enthalpies of adsorption, typically in the range of 4Ð7 kJ mol21, are measured.
Jonathan Germain, Jean M. J. Frchet and Frantisek Svec, J. Mater. Chem., 2007, 17, 4989Ð4997
HE008 - Hydrogen storage behavior of ZrNi 70/30 and ZrNi 30/70 composites
The ZrÐNi compositional alloys, namely (i) ZrNi 70/30 and (ii) ZrNi 30/70 (both by weight) have been investigated for the reversible hydrogenation behavior. These composites show ZrÐNi intermetallic multi-phase formation as explored by X-ray diffraction studies. The sorption kinetics of ZrNi 70/30 seems much faster (?3Ð4 times) than that of ZrNi 30/70 alloys. The initial desorption rate increasing with an increase in temperature. A well-defined plateau region was obtained for the ZrNi 70/30 with an equilibrium pressure range from <1 bar (300 ?C) to 10 bars (390 ?C). For ZrNi 30/70, the sloppy plateau region extends to higher equilibrium pressures. It is estimated that the total effective hydrogen concentration for ZrNi 70/30 (?1.0 wt.%) is at least 2 times that of ZrNi 30/70 (?0.5 wt.%) composites. From the PCT isotherms, the enthalpy of reaction ( H) has been calculated to be ?39 kJ/mol H2 for the ZrNi 70/30. The surface morphologies of the hydrogenated materials exhibit the presence of cracks and particle size pulverization in comparison to the pristine alloys
Diego Escobar, Sesha Srinivasan, Yogi Goswami, Elias Stefanakos, Journal of Alloys and Compounds 458 (2008) 223Ð230
HE007 - Polyaniline-based nanocomposite materials for hydrogen storage
Nanomaterials have diverse tunable physical properties as a function of their size and shape due to strong quantum confinement effect and large surface to volume ratio. On basis of these facts, nanocomposite materials can be considered as strong candidates for hydrogen storage. In the present work, we report a novel conducting polymeric nanocomposite material for hydrogen storage. Conducting polymer-based nanocomposites were modified using carbon nanotubes as filler material. This further increased the porous structure of the nanocomposite and the number of binding sites, which in turn enhances the hydrogen storage capacity. Additionally, fine aluminum powder was added to the polymeric nanocomposite, which further increased the hydrogen sorption of the material. The modified conducting polymeric nanocomposites were characterized with various analytical techniques including FTIR, DSC, TGA and SEM. Adsorption and desorption experiments are conducted using a Sieverts-type volumetric PCT instrument. Further experiments are in progress to understand the hydrogen storage mechanism in the proposed conducting polymer nanocomposites.
Michael Ulrich Jurczyk, Ashok Kumar, Sesha Srinivasan, Elias Stefanakos, International Journal of Hydrogen Energy 32 (2007) 1010 Ð 1015
HE006 - LaMg2PdH7, a new complex metal hydride containing tetrahedral [PdH4]4? anions
Hydrogenation of the intermetallic compound LaMg2Pd at 200 ?C and 10 bar leads to a complex metal hydride of composition LaMg2PdH7. Its structure has orthorhombic symmetry and displays tetrahedral [PdH4]4? anions. The PdÐH bond distances as measured on the deuteride range from 1.71 to 1.78 ¡A and the HÐPdÐH bond angles from 95? to 122?. Three additional hydride anions H? occupy La2Mg2-type interstices having tetrahedral metal configurations. Band structure calculations suggest the hydride to be non-metallic and to have a band gap of ?1.0 eV. The compound desorbs hydrogen at 125 ?C yielding a pressure of more than 1 bar absolute.
K. Yvon, J.-Ph. Rapin , N. Penin, Zhu Mab, M.Y. Choub, Journal of Alloys and Compounds 446Ð447 (2007) 34Ð38
HE005 - National Testing Laboratory for Solid-State Hydrogen Storage Technologies
Develop and operate a national-level testing and core reference laboratory aimed at assessing and validating the performance of emerging solid-state hydrogen storage materials and full-scale systems. Establish and validate measurement techniques for hydrogen sorption and related performance metrics.
Michael A. Miller and Richard A. Page FY 2006 Annual Progress Report DOE Hydrogen Program 529-534
HE004 - Dependence of dissociation pressure upon doping level of Ti-doped sodium alanateÑa possibility for ÔÔthermodynamic tailoringÕÕ of the system
PressureÐconcentration isotherms have been recorded for NaAlH4 with different doping levels of titanium. It is well known that titanium accelerates the hydrogenation and dehydrogenation reactions in this system. Our studies have shown that the titanium doping also significantly alters the thermodynamics of the system, which is demonstrated by the change of the dissociation pressure with doping level. This can be explained by changes in the systems energy by dilution of the TiAl-alloy present after doping: Such an alloy forms as a result of the doping reaction. Aluminum generated during the dehydrogenation reaction dilutes this alloy, which gives an additional contribution to the free energy of the system.
Guido Streukens, Borislav Bogdanovic, Michael Felderhoff and Ferdi Schth, Phys. Chem. Chem. Phys., 2006, 8, 2889Ð2892
HE003 - Independent verification of the saturation hydrogen uptake in MOF-177 and establishment of a benchmark for hydrogen adsorption in metalÐorganic frameworks
Hydrogen isotherms for MOF-177, Zn4O(1,3,5-benzenetribenzoate)2, crystals were independently measured by volumetric and gravimetric methods at 77 K to confirm its hydrogen uptake capacity and to establish the importance of calibrating gas adsorption instrumentation prior to evaluating H2 storage capacities. Reproducibility of hydrogen adsorption experiments is important because non-systematic errors in measurements can easily occur leading to erroneous reports of capacities. The surface excess weight percentage of hydrogen uptake in MOF-177 samples is 7.5 wt% at 70 bar, which corresponds to an absolute adsorbed amount of 11 wt%. These values are in agreement with our previous report and with those found independently by Southwest Research Institute. Considering its well-known structure and its significant H2 uptake properties, we believe MOF-177 is an excellent material to serve as a benchmark adsorber.
Hiroyasu Furukawa, Michael A. Miller and Omar M. Yaghi J. Mater. Chem., 2007, 17, 3197Ð3204
HE002 - Thermodynamische und katalytische Eigenschaften von Titan- und Cer-dotierten komplexen Aluminiumhydriden
x
Thesis of Guido Streukens Fakultt fr Chemie der Ruhr Universitt Bochum Germany 2007
HE001 - Crystal structure determination and reaction pathway of amideÐhydride mixtures
Combined synchrotron in situ X-ray diffraction and neutron diffraction studies were performed on 2:1 mixtures of lithium amide and magnesium hydride, which have shown promise as solid-state hydrogen storage materials. The dehydrogenated product is a mixed lithium and magnesium imide, Li2Mg(NH)2, whose crystal structure has not heretofore been determined. Furthermore, at elevated temperatures, Li2Mg(NH)2 undergoes two structural transitions from an orthorhombic structure to a primitive cubic structure at intermediate temperature (350 ?C) followed by a facecentered cubic crystal structure at high temperature (500 ?C). Disordering of the Li, Mg and cation vacancies as a function of temperature drives the structural transitions.We report the reaction pathway from in situ X-ray diffraction studies and the crystal structures of the three structural variants of Li2Mg(NH)2 as determined by high-resolution X-ray and neutron powder diffraction. We also report the hydrogen storage reaction pathways for mixtures with other cation ratios.
Job Rijssenbeek, Yan Gao, Jonathan Hanson, Qingzhen Huang, Camille Jones, Brian Toby Journal of Alloys and Compounds xxx (2007) xxxÐxxx
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