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L0007 - BaTiO3 ceramics. Sintering and residual carbon content.
x
C. Le Calv-Proust, E. Husson, G. Blondiaux, J.P. Coutures, Third Euro-Ceramics 1 (1993) 799-804
L0006 - Grain growth and swelling of hot pressed BaTiO3 during annealing treatments
x
M. Demartin, C. Herard, J. Lemaitre and C. Carry, Third Euro-Ceramics 1 (1993) 775-780
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, supplment 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, supplment 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 Å 1; v Å 2; w Å 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)
HE0053 - Recommended Best Practices for the Characterization of Storage Properties of Hydrogen Storage Materials
This Recommended Practices for the Characterization of Hydrogen Storage Materials document provides an introduction to and overview of the recommended best practices in making measurements of the hydrogen storage properties of materials. Due to the breadth of the subjects covered, material will be presented in its most concise and accessible form. The authors will use examples from literature to add clarity to key topics and to provide the reader with avenues for further detailed inquiry into a specific subject. The Recommended Practices document is divided into an introductory section and will be followed by four or more chapters that cover the topic areas of:concentration and capacity, kinetics, thermodynamics and cycle life measurements of hydrogen storage materials as well as other important hydrogen storage materials properties.
Karl J. Gross, K. Russell Carrington, Steven Barcelo, Abhi Karkamkar, Justin Purewal,
HE0052 - Carbon monoliths for CO2 adsorption
In this article we present the characterization of some carbon monoliths, which have an open and permeable structure. Due to electrical and thermal conductivity of the carbon fibers these composites could be electrically desorbed. The monoliths were prepared from milled carbon fibers and a phenolic resin. The obtained monolithic composites were carbonized up to 650¡C and then the composites were steam activated at 800¡C. By activation, the adsorption capacity of carbon dioxide was improved. The carbon fibers composites were characterized using scanning electron microscopy, atomic force microscopy, X-ray diffraction, BET surface area analysis and volumetric measurements of gas adsorption.
C. Banciu, A. Bara, L. Leonat, D. Patroi, Optoelectronics and Advanced Materials Ð Rapid Communications Vol. 5, No. 12, December 2011, p. 1341 - 1345
HE0051 - Iodide substitution in lithium borohydride, LiBH4ÐLiI
The new concept, anion substitution, is explored for possible improvement of hydrogen storage properties in the system LiBH4ÐLiI. The structural chemistry and the substitution mechanism are analyzed using Rietveld refinement of in situ synchrotron radiation powder Xray diffraction (SRPXD) data, attenuated total reflectance infrared spectroscopy (ATRIR), differential scanning calorimetry (DSC) and Sieverts measurements. Anion substitution is observed as formation of two solid solutions of Li(BH4)1?xIx, which merge into one upon heating. The solid solutions have hexagonal structures (space group P63mc) similar to the structures of hLiBH4 and bLiI. The solid solutions have iodide contents in the range ?0Ð62 mol% and are stable from below room temperature to the melting point at 330 ?C. Thus the stability of the solid solutions is higher as compared to that of the orthorhombic and hexagonal polymorphs of LiBH4 and ? and ? LiI. Furthermore, the rehydrogenation properties of the iodide substituted solid solution Li(BH4)1?xIx, measured by the Sieverts method, are improved as compared to those of LiBH4. After four cycles of hydrogen release and uptake the Li(BH4)1?xIx solid solution maintains 68% of the calculated hydrogen storage capacity in contrast to LiBH4, which maintains only 25% of the storage capacity after two cycles under identical conditions.
Line H. Rude, Elena Groppo, Lene M. Arnbjerg, Dorthe B. Ravnsb¾k, Regitze A. Malmkj¾r, Yaroslav Filinchuk, Marcello Baricco, Flemming Besenbacher, Torben R. Jensen, Journal of Alloys and Compounds 509 (2011) 8299Ð 8305
HE0050 - Metal Organic Frameworks as Adsorbents for Hydrogen Purification and Precombustion Carbon Dioxide Capture
Selected metal organic frameworks exhibiting representative propertiesÑhigh surface area, structural flexibility, or the presence of open metal cation sitesÑwere tested for utility in the separation of CO2 from H2 via pressure swing adsorption. Single-component CO2 and H2 adsorption isotherms were measured at 313 K and pressures up to 40 bar for Zn4O(BTB)2 (MOF-177, BTB3 = 1,3,5-benzenetribenzoate), Be12(OH)12(BTB)4 (Be-BTB), Co(BDP) (BDP2 = 1,4-benzenedipyrazolate), H3[(Cu4Cl)3(BTTri)8] (Cu-BTTri, BTTri3 = 1,3,5-enzenetristriazolate), and Mg2-(dobdc) (dobdc4 = 1,4-dioxido-2,5-benzenedicarboxylate). Ideal adsorbed solution theory was used to estimate realistic isotherms for the 80:20 and 60:40 H2/CO2 gas mixtures relevant to H2 purification and precombustion CO2 capture, respectively. In the former case, the results afford CO2/H2 selectivities between 2 and 860 and mixed-gas working capacities, assuming a 1 bar purge pressure, as high as 8.6 mol/kg and 7.4mol/L. In particular, metal organic frameworks with a high concentration of exposed metal cation sites, Mg2(dobdc) and Cu-BTTri, offer significant improvements over commonly used adsorbents, indicating the promise of such materials for applications in CO2/H2 separations.
Zoey R. Herm,Joseph A. Swisher,Berend Smit,Rajamani Krishna, Jeffrey R. Long, J. Am. Chem. Soc.2010
HE0049 - Mg-Ni-Cu mixtures for hydrogen storage: A kinetic study
Mg based ternary mixtures containing increasing amounts of Ni and Cu were prepared by ball milling under argon for 16 hours and then activated at high temperature (623K) by charging-discharging cycles at H2 pressures of 50 bar/0.7 bar. The work aims to analyze the influence of the mixture composition on the storage properties (H2 intake and sorption kinetics).
C. Milanese, A. Girella, P. Cofrancesco, G. Bruni, V. Berbenni, P. Matteazzi, A. Marini, Intermetallics 18 (2010) 203-211
HE0048 - Effect of C (graphite) doping on the H2 sorption performances of the Mg-Ni storage system
The purpose of the study was to evaluate the effect of C addition on the reactivity, the sorption activation and the sorption performances of the Mg-Ni system.
C. Milanese, A. Girella, S. Garroni, G. Bruni, V. Berbenni, P. Matteazzi, A. Marini, International journal of hydrogen energy 35 (2010) 1285-1295
HE0047 - Synergetic effect of C (graphite) and Nb2O5 on the H2 sorption properties of the Mg-MgH2 system
Ternary Mg-Nb2O5-graphitic C mixtures were prepared by high energy ball milling under Ar for different times and charcaterized especially by the calorimetric technique.The aims of the work are to assess the effect of the simultaneous presence of the two dopants on the reactivity and the sorption properties of the Mg-MgH2 system, to study the influence of the milling time on the performances of the mixtures.
C. Milanese, A. Girella, S. Garroni, G. Bruni, V. Berbenni, P. Matteazzi, A. Marini, International journal of hydrogen energy 35 (2010) 9027-9037
HE0046 - A Reversible Nanoconfined Chemical Reaction
Hydrogen is recognized as a potential, extremely interesting energy carrier system, which can facilitate efficient utilization of unevenly distributed renewable energy. A major challenge in a future Òhydrogen economyÓ is the development of a safe, compact, robust, and efficient means of hydrogen storage, in particular, for mobile applications. Here we report on a new concept for hydrogen storage using nanoconfined reversible chemical reactions. LiBH4 and MgH2 nanoparticles are embedded in a nanoporous carbon aerogel scaffold with pore size Dmax 21 nm and react during release of hydrogen and form MgB2. The hydrogen desorption kinetics is significantly improved compared to bulk conditions, and the nanoconfined system has a high degree of reversibility and stability and possibly also improved thermodynamic properties. This new scheme of nanoconfined chemistry may have a wide range of interesting applications in the future, for example, within the merging area of chemical storage of renewable energy.
Thomas K. Nielsen, Ulrike Bsenberg, Rapee Gosalawit, Martin Dornheim, Yngve Cerenius, Flemming Besenbacher, Torben R. Jensen, ACS Nano, Vol. 4, N¡ 7, 3903Ð3908 (2010)
HE0045 - Confinement of MgH2 Nanoclusters within Nanoporous Aerogel Scaffold Materials
Nanoparticles of magnesium hydride were embedded in nanoporous carbon aerogel scaffold materials in order to explore the kinetic properties of hydrogen uptake and release. A new modified procedure for the synthesis of magnesium hydride nanoparticles is presented. The procedure makes use of monoliths ( 0.4 cm3) of two distinct types of nanoporous resorcinol formaldehyde carbon aerogels loaded with dibutylmagnesium, MgBu2. Excess MgBu2 was removed mechanically, and the increase in mass was used as a measure of the amount of embedded MgH2. Energy-dispersive spectrometry revealed that MgH2 was uniformly distributed within the aerogel material. In situ synchrotron radiation powder X-ray diffraction showed that MgBu2 transformed directly to MgH2 at T 137 ¡C and p(H2) 50 bar. Two distinct aerogel samples, denoted X1 and X2, with pore volumes of 1.27 and 0.65 mL/g and average pore sizes of 22 and 7 nm, respectively, were selected. In these samples, the uptake of magnesium hydride was found to be proportional to the pore volume, and aerogels X1 and X2 incorporated 18.2 and 10.0 wt % of MgH2, respectively. For the two samples, the volumetric MgH2 uptake was similar, 12 vol %. The hydrogen storage properties of nanoconfined MgH2 were studied by SievertsÕ measurements and thermal desorption spectroscopy, which clearly demonstrated that the dehydrogenation kinetics of the confined hydride depends on the pore size distribution of the scaffold material; that is, smaller pores mediated faster desorption rates possibly due to a size reduction of the confined magnesium hydride.
Thomas K. Nielsen, Kandavel Manickam, Michael Hirscher, Flemming Besenbacher, Torben R. Jensen, ACS Nano, Vol. 3, N¡. 11, 3521Ð3528 (2009)
HE0044 - Improved Hydrogen Storage Kinetics of Nanoconfined NaAlH4 Catalyzed with TiCl3 Nanoparticles
Nanoparticles of NaAlH4 have been infiltrated in nanoporous carbon aerogel with TiCl3 nanoparticles in order to explore possible synergetic effects between nanoconfinement and a functionalized catalytic scaffold. Resorcinol formaldehyde carbon aerogels with an average pore size of 17 nm and total pore volume of 1.26 mL/g were infiltrated with TiCl3 to obtain an aerogel doped with 3.0 wt %TiCl3 nanoparticles. NaAlH4 was melt-infiltrated into the functionalized carbon aerogel at 189 C and p(H2) ? 186 199 bar. Energy-dispersive spectrometry (EDS) combined with focused ion beam (FIB) techniques revealed the presence of Na, Al, Ti, and Cl inside the aerogel scaffold material. The infiltrated NaAlH4 was X-ray amorphous, whereas 27Al magic-angle spinning (MAS) NMR spectroscopy confirmed the presence of nanoconfined NaAlH4. Temperature-programmed desorption mass spectroscopy (TPD-MS) and Sieverts' measurements demonstrated significantly improved hydrogen desorption kinetics for this new nanoconfined NaAlH4 TiCl3 material as compared to nanoconfined NaAlH4 without the catalysts TiCl3 and to bulk ball-milled samples of NaAlH4 TiCl3. We find that the onset temperature for hydrogen release was close to room temperature (Tonset = 33 C), and the hydrogen release rate reached a maximum value at 125 C, which demonstrates favorable synergetic effects between nanoconfinement and catalyst addition.
Thomas K. Nielsen, Marek Polanski, Dariusz Zasada, Payam Javadian, Flemming Besenbacher, Jerzy Bystrzycki, J¿rgen Skibsted, Torben R. Jensen, ACS Nano
HE0043 - Processing analysis of the ternary LiNH2ÐMgH2ÐLiBH4 system for hydrogen storage
In this article, we investigate the ternary LiNH2ÐMgH2ÐLiBH4 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 LiÐBÐNÐH 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 LiÐBÐNÐH 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 fullereneÐLiBH4 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 BÐH 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 ÒeutecticÓ 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
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