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E0187 - Effect of Ce-Zr mixed oxides on the thermal stability of transition aluminas at elevated temperature
Ce-Zr mixed oxides is a kind of promoted oxygen storage capability material widely used in three-way catalysts. Various contents (10, 20, 30 and 40%) of Ce-Zr were physically mixed into the pure gamma-alumina for surface modification. The thermal stability of a series of Ce-Zr/Al2O3 supports was examined. Differential thermal analysis shows Ce-Zr mixed oxides increase the theta-alumina transformation temperature up to 1222¡C. The powder X-ray diffraction studies show that minor theta-alumina phase still exists in the samples with > 20% Ce-Zr doping content after aging at 1050¡C for 50 h. The best stabilizing effect is observed in the case of 20% Ce-Zr/Al2O3. Even after the accelerated aging test, it maintains an acceptable specific surface area (24m2 g-1) in relation with the delayed transformation of theta into alpha-alumina.
X. Wu, B. Yang, D. Weng, Journal of Alloys and Compounds 376 (2004) 241-245
E0186 - Phase equilibria in the Bi2TeO5-Bi2SeO5 system and a high temperature neutron powder diffraction study of Bi2SeO5
Phase equilibria in the Bi2TeO5-Bi2SeO5 system were studied by X-ray, DTA and second harmonic generation (SHG). The samples were synthesized by solid state reactions of the Bi, Te and Se oxides. The phase diagram is interpreted as a quasibinary peritectic one with wide ranges of solid solutions on the basis of both compounds. The SHG study showed Bi2SeO5 to undergo a phase transition at about 250¡C. Neutron diffraction (25-650¡C) showed no major changes in the structure of Bi2SeO5 at high temperatures. However, the analysis of the oxygen atom thermal factors and site occupancies suggested that the mechanism of the phase transformation is an order-disorder transition involving reorientation of the SeO3 group.
O.A. Dityatyev, P. Smidt, S.Yu. Stefanovich, P. Lightfoot, V.A. Dolgikh, H. Opperman, Solid State Sciences 6 (2004) 915-922
E0185 - Characteristics of Pb[(Zn1/3Nb2/3)0.955Ti0.045]O3 single crystals versus growth method
Relaxor-based piezoelectric 0.955Pb(Zn1/3Nb2/3)O3-0.045PbTiO3 (PZN-4.5PT) single crystals were grown by two methods: the flux method and the modified Bridgman method from a flux of Pb3O4 in sealed platinum crucibles at about 1200¡C with a cooling rate of 0.8-1¡C/h for flux method and a translation rate of 0.4-0.6 mm/h for MB method. A dedicated oven suitable for two methods has been specially built. The ratio PZN-PT/Flux was 40/60 mol % for the two methods. In this paper, some characteristics of the crystals obtained by flux and modified Bridgmann method such as the lattice parameters and the melting point are compared. The dielectric properties of the grown PZN-4.5PT crystals have been measured as a function of temperature at various frequencies. The phase transition from the tetragonal P4mm to cubic phase takes place at 166¡C for the crystals grown by Bridgmann modified method and Flux method.
A. Benayad, D. Kobor, L. Lebrun, B. Guiffard, D. Guyomar, Journal of Crystal Growth 270 (2004) 137-144
E0184 - Preparation and crystallization of glasses in the system tetrasilicic mica-fluorapatite-diopside
The production of glasses whose composition ranged between tetrasilicic mica and fluorapatite-diopsite 50/50 (in wt.%) was investigated. Glass-ceramics were obtained by both bulk crystallization and sintering of glass powder compacts. The experimental results showed that increasing amount of apatite and diopsite components in the ternary system until 50% mica content generally caused decrease of melting temperature and increasing stability of glass against spontaneous crystallization during cooling after casting. Liquid immiscibility, whose features depend on the particular glass composition, characterized all the investigated glasses but it was more pronounced in the glasses with higher amount of apatite and diopsite components. The investigated glasses are preferably crystallized in bulk form between 700 and 900¡C, resulting in formation of different combinations between mica, fluorapatite and diopsite, depending on the particular composition. The obtained glass-ceramics exhibited attractive aesthetics, structural integrity and dense structure.
D.U. Tulyaganov, S. Agathopoulos, H.R. Fernandes, J.M. Ventura, J.M.F. Ferreira, Journal of the European Ceramic Society 24 (2004) 3521-3528
E0183 - Thermal characterization of Cu60ZrxTi(40-x) metallic glasses (x = 15; 20, 22, 25, 30)
The crystallization behavior, the thermal stability and the microhardness of Cu60ZrxTi(40-x) amorphous alloys (x = 15; 20, 22, 25, 30) prepared by melt-spinning have been studied by means of differential scanning calorimetry (DSC), differential thermal analysis (DTA), X-ray diffraction (XRD) and microhardness tests. DSC analysis have confirmed the existence of glass transition, followed by a supercooled liquid region in all the compositions. However, depending on the Zr content, different crystallization behavior has been observed. The apparent activation energies of the crystallization processes have been determined and the obtained values indicate high thermal stability for all the alloys. XRD-patterns of the as-quenched samples showed a broad symmetric halo typical of a fully amorphous structure. Independently of the composition, after the first crystallization stage the XRD patterns present a structure similar to that of an amorphous one. But the final developed microstructure depends on the composition of the alloys. The addition of Zr has not shown significant differences in microhardness of the amorphous alloys, although they have exhibited good mechanical properties.
A. Concustell, M. Zielinska, A. RŽvŽsz, L.K. Varga, S. Surinach, M.D. Baro, Intermetallics 12 (2004) 1063-1067
E0182 - Pb(UO2)(V2O7), a novel lead uranyl divanadate
A new lead uranyl divanadate, PbUO2(V2O7), has been synthesized by high temperature solid-state reaction and its crystal structure was solved by direct methods using single-crystal X-ray diffraction data. It crystallizes in the monoclinic system with space group P21/n and following cell parameters: a=6.9212(9) , b=9.6523(13) , c=11.7881(16) , beta=91.74(1)¡, V=787.01(2) 3, Z=4, pmes=5.82(3), pcal=5.83(1) g/cm3. A full-matrix least-squares refinement on the basis of F2 yielded R1=0.029 and wR2=0.064 for 2136 independent reflections with I>2?(I) collected with a Bruker AXS diffractometer (MoKalpha radiation). The crystal structure of PbUO2(V2O7) consists of a tri-dimensional framework resulting from the association of V2O7 divanadate units formed by two VO4 tetrahedra sharing corner and UO7 uranyl pentagonal bipyramids and creating one-dimensional elliptic channels occupied by the Pb2+ ions. In PbUO2(V2O7), infinite ribbons of four pentagons wide are formed which can be deduced from the sheets with Uranophane type anion-topology that occurs, for example, in the uranyl divanadate (UO2)2(V2O7), by replacement of half-U atoms of the edge-shared UO7 pentagonal bipyramids by Pb atoms. Infrared spectroscopy was investigated at room temperature in the frequency range 400-4000 cm-1, showing some characteristic bands of uranyl ion and of VO4 tetrahedra.
S. Obbade , C. Dion, M. Saadi, S. Yagoubi, F. Abraham, Journal of Solid State Chemistry 177 (2004) 3909-3917
E0181 - Electrical impedance determination of phase transitions in glasses and melts
The electrical impedances of glasses in the system BaO*Al2O3*B2O3 were studied in the temperature range from 550 to 1150¡C using different heating and cooling rates. The specific conductivities were illustrated by fitting Arrhenius functions to the data and the derivative (-d ln ?/ d(1/kT)). In this system, the activation energy of the electrical conductivity depends on temperature. Crystallization of the melt affects the derivative. Depending on the specific conductivities and the respective activation energies of the liquid and the crystalline phase, maxima or minima (or both) are observed in the derivative. The melting of the crystalline phase during heating results in a maximum of the derivative. The shape of the derivative can be explained taking into account the specific conductivities and the attributed activation energies of the liquid and crystalline phase.
R. Keding, D. Tauch, C. RŸssel, Journal of Non-Crystalline Solids 348 (2004) 123-130
E0180 - Floating zone growth and characterization of Pr5Si3 single crystals
Pr5Si3 single crystals have been grown by the floating zone technique with optical heating. The crystals are crack-free, 6mm in diameter and 40-60mm in length. Pr5Si3 crystallizes with the tetragonal Cr5B3 crystal structure type (space group: I4/mcm) and with lattice parameters a = b = 7.8172(7) and c = 13.816(3) . Single crystal XRD data have been refined based on the Cr5B3 structure. The electrical resistivity of Pr5Si3 single crystals exhibit metallic behavior with an anomaly at TC = 43.5(1.0)K corresponding to a ferromagnetic ordering transition, which was confirmed by magneticsusc eptibility measurements.
D. Souptel, A. Leithe-Jasper, W. Lšser, W. Schnelle, H. Borrmann, GŸnter Behr, Journal of Crystal Growth 273 (2004) 311-319
E0179 - Mixed crystals in the system Cu2MnGexSn(1-x)S4: Phase analytical investigations and inspection of tetrahedra volumes
Cu2MnGeS4 crystallizes orthorhombic in a wurtzite superstructure type while Cu2MnSnS4 crystallizes in a tetragonal sphalerite superstructure type. Lattice constants and thermal analyses of the solid solution series Cu2MnGexSn(1-x)S4 are presented. A two-phase region is found from Cu2MnGe0.3Sn0.7S4 to Cu2MnGe0.5Sn0.5S4. The cell volume of the mixed crystals increases with increasing Sn content. The melting points increase smoothly with increasing Ge content to x = 0:5 and then steeply for higher Ge contents. The single crystal X-ray structure analysis of Cu2MnGe0.55Sn0.45S4 is presented. The refinement converges to R = 0:0270 and wR2 = 0:0586, Z is 2. The volumes of the tetrahedra [MS4] (M = Cu, Mn, Ge, Sn) are calculated. From these volumes the differences in size of the tetrahedra are derived and compared with the corresponding differences in the end members of the solid solution series. It turns out that the resulting structure type in these materials depends on the volume differences of the constituting tetrahedra [MS4].
T. Bernert, M. Zabel, A. Pfitzner, Journal of Solid State Chemistry 179 (2006) 849-854
E0178 - Thermodynamic and structural analyses and mechanisms of the crystallisation of multi-alkane model mixtures similar to petroleum cuts
Thermodynamic and structural analyses were carried out by X-ray diffraction and differential thermal analyses as functions of the temperature on multi-alkane samples whose distribution of mole fractions shows a shape of the 'exponential decreasing' type, as observed in petroleum cuts. Nine samples, whose number of normal-alkanes, Cns, varied from 15 up to 23, were studied with continuous distributions of mole fractions going from the C22-C36 series to the C14-C36 series: C22 and C14 corresponding respectively to the first Cns of the two terminal series and C36 is always the last Cn of each series: each mixture differed from the previous sample by the addition of a lighter C'n-1). At the solid state and according to literature, the multi-alkane samples of C22-C36, C21-C36 and C20-C36 series are in a two-phase solid thermodynamic state, C19-C36 to C15-C36, three-phase, the broader distribution C14-C36, four-phase and the mixtures with numbers of Cns<11, single-phase. Thus, the Cns crystallise in the solid phase, where the thickness of molecule layers is compatible with their own chain length. The results allow for extracting the recurring structural and thermodynamic properties for these types of mixtures during crystallisation, and to clarify the molecular mechanisms involved in the number of observed solid phases, in the order of their appearance and in their thermodynamic and structural behaviour during the course of cooling from the liquid state.
A-J. Briard, M. Bouroukba, D. Petitjean, N. Hubert, J-C. Moise, M. Dirand, Fuel 85 (2006) 764-777
E0177 - Dielectric properties of sodium fluoride added kaolinite at different firing temperatures
The dielectric properties of NaF doped and undoped kaolinite were measured as a function of frequency in the range 40 kHz to 50 MHz. The epsilon', tan d and ?ac values are given as a function of firing temperature and NaF concentration. The addition of NaF increased the dielectric constant of pure kaolinite. However, the dielectric constant and ac conductivity of mullite obtained by the addition of NaF to kaolinite decreased from the value for pure kaolinite. Furthermore, the addition of NaF reduced the formation temperature of mullite from 1200 to 1000¡C.
H. Zipkin, L. Israel, S. GŸler, C. GŸler, Ceramics International 33 (2007) 663-667
E0176 - Influence of Ce3+ doping on the structure and luminescence of Er3+-doped transparent glass-ceramics
Transparent glass-ceramics possess high thermal and mechanical properties, easy shaping allowing fibers elaboration and easy synthesis. However, previously studied Yb:Er-doped glass-ceramics do not appear efficient enough for optical amplification at 1.5 µm in the telecommunication window. So, the addition of Ce3+ doping ions was performed. Oxyfluoride glasses (GeO2-PbO-PbF2) doped with ErF3, YbF3 and CeF3 were prepared and heated above glass transition temperature to obtain transparent glass-ceramics. Such treatment brings about the precipitation of fluorite-type nanocrystallites embedded into an amorphous oxide phase. Differential Thermal Analysis shows evidence that CeF3 acts as nucleating agent for the heterogeneous crystallization of the beta-PbF2 phase. Through Transmission Electron Microscopy the morphology of these glass-ceramics was studied. Energy dispersive X-ray microanalysis and unit cell parameter study show a segregation of the three rare-earth ions inside the fluorite crystallites, forming a solid solution Pb(1-x-y-z)Er(x)Yb(y)Ce(z)F(2+x+y+z). The luminescence characteristics of the glass-ceramics doped with ErF3, YbF3 and CeF3 were compared to those of Yb:Er-doped glass-ceramics. CeF3 enables to dramatically decrease the up-conversion fluorescence of Er3+. The study of temporal dynamic of the 4 I 13/2 level of Er3+ reveals a cross-relaxation process between Er3+ and Ce3+. Hence, the presence of Ce3+ enables to decrease the Er3+ up-conversion fluorescence at the benefit of the fluorescence of interest at 1.5 µm, which is strongly enhanced.
G. Dantelle, M. Mortier, D. Vivien, G. Patriarche, Optical Materials 28 (2006) 638-642
E0175 - Influence of the Ti/Zr ratio and the synthesis route on hydrogen absorbing properties of (Ti(1-x)Zrx)Mn1.5V0.5 alloys
The hydrogenation properties of two pseudo-binary Ti(1-x)ZrxMn1.5V0.5 alloys with x=0.15 and 0.5 obtained by arc melting and mechanical alloying have been studied. All alloys crystallize in the hexagonal C14 Laves phase. Arc-melted alloys are microcrystralline and exhibit local variations of Ti and Zr contents which are not overcome by annealing treatments. As for milled alloys, agglomerated nanocrystallites (~9 nm in diameter) are obtained after subsequent thermal annealing at 800¡C. For high Zr-contents, a better chemical homogeneity is obtained by the milling route. Whatever the synthesis route is, the hydrogen equilibrium pressure decreases with increasing Zr content due to cell-volume increase of the intermetallic compound. As concerns kinetics, very fast hydrogenation rates of few seconds are obtained at room temperature, particularly for milled alloys.
B. Villeroy, F. Cuevas, J. Bettembourg, P. Olier, M. Latroche, Journal of Physics and Chemistry of Solids 67 (2006) 1281-1285
E0174 - Homogeneity range and order-disorder transitions in R(1-x)Ni2 Laves phase compounds
The homogeneity range of R(1-x)Ni2 Laves phases (R=Ce, Gd, Tb) has been studied by X-ray diffraction, microprobe analysis and density measurements. In these compounds, the number of R vacancies varies as a function of the atomic number of the rare earth metal and the nominal composition. For R=Tb the number of vacancies varies by 0<x<0.5, with a change of the structure from a pure C15 structure to a 2a superstructure accompanied by a cell volume decrease. The order-disorder transition of the rare-earth vacancies has been studied under applied pressure for La7Ni16 and as a function of temperature for all the R(1-x)Ni2 compounds. The evolution of the transition pressure and temperature, which reflects the binding energy of the vacancies in the lattice, depends not only on the radius of the R atoms but also on their masses.
V. Paul-Boncour, A. Lindbaum, M. Latroche, S. Heathman, Intermetallics 14 (2006) 483-490
E0172 - Characteristics of chabazite modified by hexadecyltrimethylammonium bromide and of its affinity toward chromates
The FTIR, XRD, SEM and equilibrium data concerning the chabazite modified by hexadecyltrimethylammonium bromide (HDTMA) are presented. The zeolite plays the role of surfactant carrier. Its sodium form is converted to surfactant form through its equilibration with aqueous solutions of HDTMA. It is established that HDTMA cations are incorporated into the chabazite structure via ion-exchange and Van der Waals forces. Gauche and trans conformers are recognised in alkyl chains arrangement of surfactant cations. HDTMA-chabazite is evaluated as efficient adsorbent for chromates with quick kinetics (equilibrium completed in 120 min) and high adsorption maximum a=0.00005 mol/g.
M. Majdan, S. Pikus, Z. Rzaczynska, M. Iwan, O. Maryuk, R. Kwiatkowski, H. Skrzypek, Journal of Molecular Structure 791 (2006) 53-60
E0171 - Pt29Zn49, a complex defective AlB2-type derivative structure
The crystal structure of the title compound has been determined by X-ray diffraction means. Pt29Zn49 forms a complex superstructure of a defective AlB2-type derivative of the order 58: a = 279.0(1) pm, b = 11895.2(4) pm, c = 698.0(1) pm, space group Amm2, Z = 2. Ordering of vacancies is accompanied by a particular distortion of defective graphite-like 63 nets consisting exclusively of Zn atoms. The ordering induces a modulation of the structure along ah of an AlB2-type structure with a periodicity of nearly 12 nm. A mechanistic model is proposed elucidating how Pt29Zn49 evolves from the eutectoid decomposition of the inter-mediate high temperature precursor Pt7Zn12.
S. Thimmaiah, B. Harbrecht, Journal of Alloys and Compounds 417 (2006) 45-49
E0170 - Er3+-doped PbF2: Comparison between nanocrystals in glass-ceramics and bulk single crystals
An appropriate annealing of a GeO2-PbO-PbF2:ErF3 glass leads to the formation of a glass-ceramic, composed of Pb(1-x)ErxF(2+x) nanosized crystallites dispersed throughout an amorphous oxide matrix. These nanocrystallites are compared to Er3+-doped PbF2 bulk single crystals. The influence of the annealing temperature on the glass-ceramics characteristics is thoroughly investigated. For several glass-ceramics resulting from different heat treatments, the quantity of crystallized PbF2, as well as the segregation of Er3+ ions into the crystallites, has been studied through two methods: first, the study of the crystallographic characteristics and second, the evolution of the optical properties. It was evidenced that, for a heat treatment over 365¡C, the whole PbF2:Er has completely crystallized and that the segregation of Er3+ ions into the crystallites was total. Strong interactions between Er3+ ions occur in the Pb(1-x)ErxF(2+x) single and nanocrystals, promoting cross-relaxation processes, under 488-nm excitation, and favouring the 660- (red) and 810-nm emissions at the expense of the 550-nm (green) one.
G. Dantelle, M. Mortier, G. Patriarche, D. Vivien, Journal of Solid State Chemistry 179 (2006) 1995-2003
E0169 - Growth and characterization of a new nonlinear optical crystal Ca5(BO3)3F
A new nonlinear optical crystal calcium fluoroborate (Ca5(BO3)3F) has been grown successfully using LiF as a flux for the first time. Phase diagram of the pseudobinary Ca5(BO3)3F-LiF system within the composition range from 10 to 60wt% LiF was investigated by Xray powder diffraction and differential thermal analysis. Our experiments demonstrated that the composition of LiF from 15 to 35wt% was beneficial to the growth of Ca5(BO3)3F crystals in Ca5(BO3)3F-LiF system. Transmission spectrum was recorded from 185 to 3000 nm, which showed that the UV cutoff for Ca5(BO3)3F crystal was about 190 nm. Second-harmonic generation efficiency was measured from Kurtz's powder technique, which indicated that Ca5(BO3)3F could be phase matchable, and second-harmonic generation efficiency of Ca5(BO3)3F was about two times as large as that of KDP. Ca5(BO3)3F has potential application as a nonlinear optical material in UV region.
G. Chen, Y. Wu, P. Fu, Journal of Crystal Growth 292 (2006) 449-453
E0168 - Cytotoxicity of Zr-based bulk metallic glasses
Recently we developed a family of Ni-free Zr-based bulk metallic glasses in the Zr-Cu-Fe-Al system. X-ray diffraction and differential thermal analysis measurements demonstrate its good glass-forming ability, and amorphous rods of up to 13 mm in diameter can be produced for the alloy Zr58Cu22Fe8Al12. This new glassy system is potentially very interesting for biomedical applications. Thus we have investigated the effect of surface modification (treatment with nitric acid and oxygen plasma) on the alloy's cytotoxicity and compared it with the results for a Ni-bearing Zr-based bulk metallic glass. The surfaces were analyzed by X-ray photoelectron spectroscopy, and cytotoxicity was tested by measuring the viability and metabolic activity of mouse fibroblasts. Our results show that the surfaces of the as-cast glasses consist almost exclusively of zirconium oxide, which yields good biocompatibility. With nitric acid treatment this oxide layer can be stabilized further, to the extent that the cytotoxicity becomes as good as that of the non-toxic negative control (polystyrene).
S. Buzzi, K. Jin, P.J. Uggowitzer, S. Tosatti, I. Gerber, J.F. Lšffler, Intermetallics 14 (2006) 729-734
E0167 - Production and identification of rare-earth doped lithium triborate
Research in the field of non-linear optical (NLO) devices lead to an increasing interest in new borate compounds, capable of expanding the frequency range provided by common laser sources. Lithium triborate (LBO) is a newly developed ideal non-linear optical crystal used in laser weapon, welder, radar, tracker, surgery, communication, etc. In this study, synthesis and identification of rare-earth doped lithium triborate was carried out. Borates containing rare-earth elements are of great interest since they are found to be superior in non-linear optical applications. Lithium triborate was produced from the solid-state reaction. Lithium triborate was then doped with some rare-earth elements (Gd, La, Y, etc.) in several different concentrations. In this study, LBO samples doped with Gd are presented. Characterization of the new products was done by X-ray diffraction (XRD) and infrared (IR) analysis. Differential thermal analysis (DTA) was used for examination of the thermal properties of the compounds, morphology of new compounds was observed by scanning electron microscopy (SEM). The compounds are then subjected to thermoluminescence (TL) studies. From the XRD studies, no change related to addition of the rare-earth elements was observed. IR analysis showed that there is no change related to B-O link with the addition of rare-earth elements. DTA studies showed that the melting point of LBO decreases with the addition of rare-earth elements. In the SEM images, particles of rare-earth elements and lithium triborate were observed clearly.
B. Ardioglu, G. ...zbayoglu, Z. ...zdemir, A. Yilmaz, Journal of Alloys and Compounds 418 (2006) 77-79
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- May 16, 2012 - May 18, 2012
INNOSTOCK 2012
Lleida, SpainINNOSTOCK 2012The 12th International Conference on Energy Storage16-18 May 2012Innostock 2012 is part of the Stock conference series sponsored by the ECES IA of the International Energy Agency.Innostock 2012 will gather the world’s leading specialists and academic researchers within the field of energy efficiency through energy storage. Energy storage will present in all its topics:• Underground thermal energy storage• Sensible, latent and thermochemical energy storage• Electrical storage
- May 14, 2012 - May 18, 2012
11th International Hydrocolloids Conference
Purdue University, USA11th International Hydrocolloids ConferenceBiofunctionality and Technofunctionality of Hydrocolloids14-18 May 2012, Whistler Center for Carbohydrate Research, Purdue University, USAThe 11th International Hydrocolloids Conference is organized by the world-renowned Whistler Center for Carbohydrate Research and will be held at The Stewart Center at Purdue University, Indiana, USA.
- 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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