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L0005 - Sintering, grain growth and de-sintering processes in un-doped BaTiO3
X
M. Demartin, G. Pethybridge and C.Carry, Third Euro-Ceramics 1 (1993) 787-792
L0004 - Preparation of dense tetragonal zirconia ceramics from ZrO2 micropowders
x
A. Smith, B. Cales and J.F. Baumard, Journal de Physique, Colloque C1, supplément au n°2, Tome 47 (1986) 237-241
L0003 - The formation and characterization of a ceramic-ceramic interface between stabilized zirconia and lanthanum chromite
x
D. Smith, M. Sayer and P. Odier, Journal de physique, Colloque C1, supplément au n°2, Tome 47 (1986) 153-157
L0002 - Phase equilibrium and martensitic transformation in lanthana doped zirconia
The system ZrO2-La2O3 has been studied in the 0 to 15 mol% La2O3 range using X-ray diffraction and thermal analysis. Two kinds of diagrams were elaborated: First is a phase equilibrium diagram where the eutectoid decomposition of ZrO2,ss(T) => ZrO2,ss(M) + Pyss occurs at 1100°C and 0.75 mol% La2O3 (Py is the pyrochlore compound Zr2La2O7). The maximum solubility of La2O3 in ZrO2,ss(M) is 0.5 mol% at room temperature. Second, a nonequilibrium diagram is determined showing the correlations between grain size, La2O3 content, and the martensitic transformation temperature start (Ms).
B. Bastide, P. Odier and J.P. Coutures, Journal of the American Ceramic Society 71 (1988) 449-453
L0001 - Sintering behaviour of Y(u)Ba(v)Cu(w)O(7-d) (u ? 1; v ? 2; w ? 3)
x
B. Dubois, A. Douy, M. Gervais, F. Cabannes et P. Odier, International Conference on High Temperature Superconductors and Materials and Mechanisms of Superconductivity, Interlaken (Suisse) (1988)
HE0043 - Processing analysis of the ternary LiNH2-MgH2-LiBH4 system for hydrogen storage
In this article, we investigate the ternary LiNH2-MgH2-LiBH4 hydrogen storage system by adopting various processing reaction pathways. The stoichiometric ratio of LiNH2:MgH2:- LiBH4 is kept constant with a 2:1:1 molar ratio. All samples are prepared using solid-state mechano-chemical synthesis with a constant rotational speed, but with varying milling duration. Furthermore, the order of addition of parent compounds as well as the crystallite size of MgH2 are varied before milling. All samples are intimate mixtures of Li-B-N-H quaternary hydride phase with MgH2, as evidenced by XRD and FTIR measurements. It is found that the samples with MgH2 crystallite sizes of approximately 10 nm exhibit lower initial hydrogen release at a temperature of 150 C. Furthermore, it is observed that the crystallite size of Li-B-N-H has a significant effect on the amount of hydrogen release with an optimum size of 28 nm. The as-synthesized hydrides exhibit two main hydrogen release temperatures, one around 160 C and the other around 300 C. The main hydrogen release temperature is reduced from 310 C to 270 C, while hydrogen is first reversibly released at temperatures as low as 150 C with a total hydrogen capacity of w6 wt.%. Detailed thermal, capacity, structural and microstructural properties are discussed and correlated with the activation energies of these materials.
Michael U. Niemann, Sesha S. Srinivasan, Ashok Kumar, Elias K. Stefanakos, D. Yogi Goswami, Kimberly McGrath, International Journal of hydrogen energy, xxx (2009) 1-8
HE0042 - Novel catalytic effects of fullerene for LiBH4 hydrogen uptake and release
The addition of catalysts to complex hydrides is aimed at enhancing the hydrogen absorption desorption properties. Here we show that the addition of carbon nanostructure C60 to LiBH4 has a remarkable catalytic effect, enhancing the uptake and release of hydrogen. A fullerene-LiBH4 composite demonstrates catalytic properties with not only lowered hydrogen desorption temperatures but also regenerative rehydrogenation at a relatively low temperature of 350 ?C. This catalytic effect probably originates from C60 interfering with the charge transfer from Li to the BH4 moiety, resulting in a minimized ionic bond between Li+ and BH4 , and a weakened covalent bond between B and H. Interaction of LiBH4 with an electronegative substrate such as carbon fullerene affects the ability of Li to donate its charge to BH4, consequently weakening the B-H bond and causing hydrogen to desorb at lower temperatures as well as facilitating the absorption of H2. Degradation of cycling capacity is observed and is probably due to the formation of diboranes or other irreversible intermediates
Matthew S. Wellons, Polly A Berseth, Ragaiy Zidan, Nanotechnology 20 (2009) 204022
HE0041 - The Investigation of MgH2and LiBH4Mixtures Potential for Hydrogen Storage
MgH2has been examined as a potential hydrogen storage due to its high gravimetric capacity of 7.6 wt.%; however, its kinetics is slow. LiBH4has even higher capacity, 13.9 wt.% when it decomposes to LiH; unfortunately, this reaction requires high temperature exceeding 400oC. ?Destabilization of LiBH4with MgH2[1] and also of MgH2with LiBH4[2], have been reported. Vajo et al. [1] reported thermodynamic improvement of the hydrogen storage performance of MgH2destabilized with LiBH4; however, no kinetic improvement was observed. The reaction pathway through Mg and then MgB2corresponding to a two-step desorption was suggested. The MgB2formation was believed to improve the reversibility [3]. Johnson et al. [2] reported kinetic improvement of the hydrogen storage performance of LiBH4destabilized withMgH2. The presence of Li+in the crystal structure was suggested to be the reason for this enhancement. However, evidence of thermodynamic enhancement from LiBH4addition was not observed. ?We have examined if there is a "eutectic" molar ratio existing between MgH2and LiBH4that may improve both kinetic and thermodynamic hydrogen storage performances. We have found that a 3:1 mole ratio of MgH2and LiBH4mixture has the fastest desorption rate and highest hydrogen desorption capacity. The 3:1 mixture was doped with TiCl3and the result shows good reversibility and cycle stability.
Uncharat Setthanan, G. Sean McGrady, Poster
HE0040 - Ammine Magnesium Borohydride Complex as a New Material for Hydrogen Storage: Structure and Properties of Mg(BH4)2·2NH
The ammonia complex of magnesium borohydride Mg(BH4)2 · 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 · 6NH3 (II), which crystallizes in the cubic space group Fm¯3m with unit cell parameter a ) 10.82(1) Å 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) Å, b ) 9.4132(2) Å, c ) 8.7304(2) Å, and Z ) 8. This structure is built from individual pseudotetrahedral molecules Mg(BH4)2 · 2NH3 containing one bidentate BH4 group and one tridentate BH4 group that pack into a layered crystal structure mediated by N-H· · ·H-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 - BN, AlN and GaN. The ternary nitrides obtained are not the known Li3XN2 systems and we have tentatively designated them as Li-X-N (where X = B, Al or Ga). We report here an investigation of the hydrogen absorption-desorption behaviour of the Li-X-N ternary nitrides.
Henrietta W. Langmi, G. Sean McGrady, Poster
HE0036 - Mixed-Metal Li3N-Based 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 ¼ 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 Mg-Ni storage system
Binary Mg-Ni mixtures and ternary Mg-Ni-C (graphite) samples with fixed proportions of metals (Mg 85%-Ni 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 ¼2 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 Mg-Ni 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 Mg-Ni 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 metal-organic framework (MOF) Zn4O(1,3,5-benzenetribenzoate)2, MOF-177, were performed over the 50-77 K and 0-40 bar ranges. The maximum excess adsorption measured under these conditions varies over about 105-70 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 Metal-Organic 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 metal-organic frameworks featuring 4,6- and 4,8-connected nets related to the structures of garnet and fluorite with the formulae Mn6-(ttpm)3·5DMF·3H2O (1) and Cu-(Cu4Cl)(ttpm)2]2·CuCl2·5DMF·11H2O (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)2·0.7CuCl2 (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 - 10285
HE0031 - 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
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 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. Campesia, F. Cuevas, R. Gadiou, E. Leroy, M. Hirscher, C. Vix-Guterl, M. Latroche, Carbon 46 (2008 ) 206 -214
HE0029 - H2 sorption performance of NaBH4-MgH2 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 - 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. Barò, S. Suriñach & A. Marini, Ecosystems and Sustainable Development VII 389
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