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E0124 - Equilibrium phase diagram of the Ag-Au-Pb ternary system
The phase diagram of the ternary system Ag-Au-Pb has been established using differential thermal analysis and X-ray powder diffraction analysis. Four vertical sections were studied: XPb = 0.40, XAu/XPb = 1/3, XAg/XAu = 4/1 and XAg/XAu = 1/1. Two ternary transitory peritectics and one ternary eutectic were characterized. A schematic representation of the ternary equilibria is given.
S. Hassam, Z. Bahari, Journal of Alloys and Compounds 392 (2005) 120-126
E0123 - Thermodynamic exploitation of the liquidus curves in the MIPO3-Pb(PO3)2, MIPO3-Cu(PO3)2 AND MIPO3-Ce(PO3)3 SYSTEMS(MI=Li, Na, K, Rb, Cs, Ag, Tl)
The thermodynamic exploitation of the solid-liquid equilibria in the M I PO3-Pb(PO3)2, M I PO3-Cu(PO3)2 and M I PO3-Ce(PO3)3 systems (with M I =Li, Na, K, Rb, Cs, Ag, Tl) is carried out using a semi-empirical equation of the liquidus curves already used with success for similar binary systems. The enthalpy of fusion is calculated for each pure polyphosphate on the assumption that the liquid solution is ideal and only formed by M I PO3 and M(PO3)q entities (q=2 for Pb and Cu, q=3 for M=Ce). In the most binary systems, a wide difference between the calculated values of the melting enthalpies of these polyphosphates and the measured ones determined from the DTA curves, was observed. This difference is probably due to the existence of some molecular associations in the liquid phase. The enthalpy of fusion of each terminal phase was then recalculated on the assumption that the liquid contains a molecular association of the type of M pn I Mn(PO3)n(q+p) in the region of the diagram rich in M I PO3 or a molecular association of the type of M n IMnp(PO3)n(qp+1) in the region rich in M(PO3)q (q=2 for Pb and Cu, q=3 for M=Ce). In this case, the obtained values are in good agreement with experimental determinations.
C. Marhag, D. Ben Hassen-Chehimi and H. Said, Journal of Thermal Analysis and Calorimetry 86 (2006) 249-254
E0122 - Characterisation of antibacterial copper releasing degradable phosphate glass fibres
Phosphate-based glass fibres (PGF) of the general formula Na2O-CaO-P2O5 are degradable in an aqueous environment, and therefore can function as antibacterial delivery systems through the inclusion of ions such as copper. In this study, PGF with varying amounts of copper oxide (CuO) were developed for potential uses in wound healing applications. PGF with 0, 1, 5 and 10mol% CuO were produced with different diameters and characterised in terms of structural and antibacterial properties. The effect of CuO and fibre pulling speed on the glass properties were investigated using rapid differential scanning calorimetry, differential thermal analysis and X-ray diffraction. The effect of two fibre diameters on short-term (3 h) attachment and killing against Staphylococcus epidermidis were investigated and were related to their rate of degradation in deionised water, as well as copper ion release measured using ion chromatography. Thermal analysis showed that there was a significant increase in the PGF glass transition temperature as the CuO content increased. There was a significant decrease in the rate of degradation with increasing CuO content and an increase in fibre diameter. Over 6 h, both the amount and rate of copper ions released increased with CuO content, as well as a reduction in fibre diameter thus increasing the surface area to volume ratio. There was a decrease in the number of viable staphylococci both attached to the CuOcontaining fibres and in the surrounding environment.
E.A. Abou Neel, I. Ahmed, J. Pratten, S.N. Nazhat, J.C. Knowles, Biomaterials 26 (2005) 2247-2254
E0121 - Nominal vs. actual stoichiometries in Al-doped NASICONs: A study of the Na1.4Al0.4M1.6(PO4)3 (M=Ge, Sn, Ti, Hf, Zr) family
Nominal Na1.4Al0.4M1.6(PO4)3 (M=Ge, Sn, Ti, Hf, Zr) NASICON compounds have been prepared as polycrystalline powders. Rietveld analysis of X-ray and neutron diffraction patterns showed that M=Ge and Sn samples crystallize in the R3ø space group (s.g.) and that M=Ti, Hf, Zr compositions crystallize in the R3øc s.g. Data analyses indicated that aluminum contents into the main NASICON phases are always smaller than the nominal ones. 27Al, 31P and 23Na magic angle spinning-nuclear magnetic resonance (MAS-NMR) spectroscopies have been used to deduce aluminum contents and local atomic environments. In samples with high aluminum contents, M=Ge, Sn and Ti, electrical conductivity has been deduced from impedance spectroscopy data. The titanium sample incorporates the maximum aluminum content and displays the lowest activation energy, 0.52(1) eV, and the highest conductivity, rT(400 K)=1.5(3) 10 5 S cm 1. The influence of structural parameters on conductivity values has been analyzed with the bond valence sum method. With this technique, the most probable conduction pathways in Na1+xAlxTi2 x(PO4)3 and Na1+xInxZr2 x(PO4)3 samples have also been deduced.
P. Maldonado-Manso, M.A.G. Aranda, S. Bruque, J. Sanz, E.R. Losilla, Solid State Ionics 176 (2005) 1613 - 1625
E0120 - Crystal structures of Rb2U2O7 and Rb8U9O31, a new layered rubidium uranate
Two alkali metal uranates Rb2U2O7 and Rb8U9O31 have been synthesized by solid state reaction at high temperature and their crystal structures determined from single crystal X-ray diffraction data, collected with a three circles Brucker SMART diffractometer equipped by Mo(Ka) radiation and a charge-coupled device (CCD) detector. Their structures were solved using direct methods and Fourier difference techniques and refined by a least-square method on the basis of F2 for all unique reflections, with R1 = 0,043 for 53 parameters and 746 independent reflections with I>2?(I) for Rb2U2O7, monoclinic symmetry, space group P21/c, a = 7,323(2) , b = 8,004(3) , c = 6,950(2) , beta = 108,81(1)¡, pmes = 6,56(3) g/cm3, pcal = 6,54(2) g/cm3, Z = 2 and R1 = 0,036 for 141 parameters and 2065 independent reflections with I>2?(I) for Rb8U9O31, orthorhombic, space group Pbna, a = 6,9925(9) , b = 14,288(2) , c = 34,062(5) , pmes = 6,47(3) g/cm3, pcal = 6,48(2) g/cm3, Z = 4. The Rb2U2O7 structure presents a strong analogy with that of K2U2O7 and can be described by layers of distorted UO2(O4) octahedra built from dimeric units of edge shared octahedra further linked together by opposite corners. In Rb8U9O31 puckered layers are formed by the association of two different uranium polyhedra, pentagonal bipyramids and distorted octahedra. The structure of Rb8U9O31 is built from a regular succession of 1[U4O14] 4- infinite ribbons similar to those observed in diuranates M2U2O7 (MQK, Rb) and infinite three polyhedra wide ribbons 1[U5O21] 12- , to create an original undulated sheets 2[U9O31] 8- . For both compounds Rb+ ions occupy the interlayer space and exhibit comparable mobility with conductivity measurements indicating an Arrhenius-type behavior.
S. Yagoubi, S. Obbade, C. Dion, F. Abraham, Journal of Solid State Chemistry 178 (2005) 3218-32
E0119 - Crystallization in the Na2O-CaO-Al2O3-SiO2-(LiF) glass compositions
Spodumene-nepheline glass-ceramics was prepared from Na2O-CaO-Al2O3-SiO2 glass compositions. Addition of LiF changes the course of the reaction toward the formation of beta-spodumene together with nepheline. The crystallization of beta-spodumene strongly reduce
E.M.A. Hamzawy, E.M. El-Meliegy, Ceramics International 33 (2007) 227-231
E0118 - A comparative study of the dehydroxylation process in untreated and hydrazine-deintercalated dickite
A dickite from Tarifa (Spain) was used to study the influence of the intercalation and the later deintercalation of hydrazine on the dehydroxylation process. The dehydroxylation of the untreated dickite occurs through three overlapping endothermic stages whose DTA peaks are centred at 586, 657 and 676¡C. These endothermic effects correspond, respectively, to the loss of the inner-surface, the inner hydroxyl groups, and the loss of the water molecules, product of dehydroxylation process, which has been trapped in the framework of the dehydroxylated dickite. The intercalation of hydrazine in the interlayer space of dickite and the later deintercalation affect the dehydroxylation process. It occurs through only two endothermic stages which DTA peaks are centred at 575 and 650¡C. The first corresponds to the simultaneous loss of both the inner and the inner-surface hydroxyl groups, whereas the second one is analogous to that at 676¡C observed in the DTA curve of untreated dickite. These effects appear shifted to lower temperatures compared to those observed in the untreated dickite.
F. Franco and M.D. Ruiz Cruz, Journal of Thermal Analysis and Calorimetry 85 (2006) 369-375
E0117 - Contribution ˆ l'Žtude du systme quasi-binaire ZrAu-CeAu
x
A. Ait Chaou, M. Lomello-Tafin, P. Lejay, J. Allemand, Ph. Galez, 30ieme JEEP (2005) 87-88
E0116 - Phases and phase equilibria in the Fe-Al-Zr system
x
F. Stein, G. Sauthoff, M. Palm, Z. Metallkd. 95 (2004) 469-485
E0115 - Thermodynamic study of the solid-liquid equilibria in the MPO3-Cu(PO3)2 systems
Thermodynamic exploration of solid-liquid equilibria of the MIPO3-Cu(PO3)2 (with MI=Li, Na, K, Rb, Cs, Ag, Tl) systems is carried out with a semi-empirical equation of the liquidus curves. The enthalpies of fusion of pure polyphosphates and some intermediate compounds were determined from DTA curves. The temperature, enthalpy and entropy of fusion are calculated for each solid phase with the exception of silver polyphosphate and the intermediate compound Cs4Cu(PO3)6 which have very limited crystallization fields. The calculated values of the melting enthalpies are approximately equal to the measured ones. The melting enthalpy of Cu(PO3)2 calculated from different binary systems shows a wide variation in the obtained values, 35-54 kJ mol-1. The experimental value is 33.65 kJ mol-1. The calculated temperatures and compositions in most binary systems are in good agreement with experimental determinations.
C. Marhag, D.B. Hassen-Chehimi, H. Said, Journal of Thermal Analysis and Calorimetry 76 (2004) 417-428
E0114 - Thermodynamique des mŽlanges binaires LiPO3-Pb(PO3)2. Diagramme de phases et Žtude thermodynamique du liquide
Study of solid-liquid phase diagram of LiPO3-Pb(PO3)2 binary system, in certain calcination conditions, shows the existence of several metastable phasis. When heated at a temperature of 723 K the binary mixtures lead uncompletely to a defined compound Pb2Li(PO3). On heating these ternary solid mixtures, three eutectic reactions have been observed: (1) LiPO3+Pb(PO3)2Liquid at a temperature of 793 K (2) LiPO3+Pb2Li(PO3)5Liquid at a temperature of 843 K (3) Pb2Li(PO3)5+Pb(PO3)2Liquid at a temperature of 891 K The metastable liquid phase appears in the system at temperature of 793 K. DTA experiments performed on the binary LiPO3-Pb(PO3)2 mixtures, show a superposition of two diagrams. The first one is metastable and the second represents the stable equilibrium phase diagram. Measurements of liquid enthalpy of binary LiPO3-Pb(PO3)2 system at temperature of 979.65 K were reported. The corresponding values were very small and so the binary system can be considered as athermal. Assuming an ideal behaviour, the liquidus curves in the metastable diagram were calculated and the eutectic reaction (LiPO3-Pb(PO3)2Liquid) was confirmed at 793 K.
C. Marhag, H. Said, P. Satre, C. Favotto, J. Rogez, Journal of Thermal Analysis and Calorimetry 74 (2003) 275-285
E0113 - Equilibres solide-liquide dans le systme Al-Fe-Si
x
S. Pontevichi, M. Peronnet, F. Bosselet, J.C. Viala, J. Bouix, 28me JEEP (2002)
E0112 - Thermal and structural studies of sodium borosilicate glasses containing thorium oxide
x
K. Sreejith, V. Sudarsan, R. Mishra, C.G.S. Pillai, Thermans (2002) 280-282
E0111 - Etude du systeme LiPO3-Pr(PO3)3 donnŽes sur LiPr(PO3)4
The LiPO3-Pr(PO3)3 system was studied by micro-differential thermal analysis. The only new compound observed in the system was LiPr(PO3)4, melting incongruently at 1246 K. An eutectic appears at 926 K. Crystallographic data and powder diagram of the new compound are given. LiPr(PO3)4 crystallizes in the C2/c monoclinic system with unit cell: a=16.428(6), b=7.054(3), c=9.747(4) , =126¡31(3), V=910.2 3, Z=4. The IR and Raman spectra of this compound are given.
M. Ferid, B. Piriou and M. Trabelsi-Ayedi, Journal of Thermal Analysis and Calorimetry 53 (1998) 227-234
E0110 - Thermodynamic study of the solid-liquid equilibria in the systems MPO3-Pr(PO3)3 (M=Na, Rb, Cs or Ag)
A previously established equation of a stoichiometric phase liquidus curve was applied to determination of the phase diagrams of the systems MIPO3-Pr(PO3)3 (with MI=Na, Rb, Cs or Ag). The temperature, enthalpy and entropy of fusion were calculated for each solid phase with the exception of silver polyphosphate, the crystallization field of which was very limited. The enthalpy of fusion of the polyphosphate Pr(PO3)3 was determined from the DTA curve. The melting enthalpy of Pr(PO3)3 calculated from the different binary systems was approximately equal to the measured value. The calculated temperatures and compositions were in good agreement with those determined experimentally.
D. Ben Hassen-Chehimi, N. Kbir-Ariguib and M. Trabelsi-Ayedi, Journal of Thermal Analysis and Calorimetry 53 (1998) 871-882
E0109 - DSC Study of Y(a)Ba(b)Cu(c)O(7-d) homogeneity in the region 1050-1300K
Phase transitions of the compositions Y1±xBa2±yCu3±zO72212; (x,y=0-0.2;z=0-0.5; step 0.1) were studied by DSC in argon atmosphere in the temperature range 1050-1300 K. The formation of three polymorphous modifications of the 123 phase was observed. The solubilities of yttrium, barium and copper oxides in every modification were determined. TheT-x-y phase microdiagram for the 123 phase was mapped out.
K.S. Gavrichev, A.V. Khoroshilov, G.D. Nipan and P. Manca, Journal of Thermal Analysis and Calorimetry 48 (1997) 1039-1050
E0108 - Determination of phase diagrams by heat evaluation from DTA.
Basing on a quantitative analysis of DTA heat flow measurements the compositions of eutectic and peritectic reactions in complicated systems can be sensitively determined. In addition to the conventionally used DTA onset temperatures, the quantitative analysis of the corresponding heat flows provides important further information which significantly improve the determination of phase relations in complicated systems. The general concept is demonstrated for simple model systems. The sensitivity of detection and the separability of the DTA events will be discussed in detail. The applicability of the method is proved for two complicated examples from the Y---Ba---Cu---O system: (1) the quasibinary section YBa2Cu3O7 - delta---BaCuO2 and (2) the ternary eutectics YBa2Cu3O7 - delta---bBaCuO2---bCuO.
U. Wiesner, W. Bieger and G. Krabbes, Thermochimica Acta 290 (1996) 115-121
E0107 - The ruthenium-tin system.
The Ru---Sn liquid-solid and some solid-solid equilibria have been completely revised by means of differential thermal analysis, X-ray powder diffraction and microprobe investigations. The existence of two intermetallic phases has been clearly established: Ru0.4Sn0.6 decomposed by a peritectic reaction at 1266(± 4)¡C and Ru0.1Sn0 - congruently melting at 1257(± 2)¡C.
L. Perring, P. Feschotte, F. Bussy and J.C. Gachon, Journal of Alloys and Compounds 245 (1996) 157-163
E0106 - The germanium-ruthenium system.
x
L. Perring, P. Feschotte and J.C. Gachon, Journal of Phase Equilibria 17 (1996) 101-106
E0105 - Brasage d'aciers rŽfractaires par des poudres de brasage ˆ base de nickel.
x
J.D. Bartout, Y. Bienvenu, A. Germidis and J. Favennec
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