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E0166 - A novel simple method to stably synthesize Ti3AlC2 powder with high purity
In this work, a novel simple method is presented to synthesize highly pure Ti3AlC2 powder by heating 2TiC/Ti/Al (molar ratio) powder system between 1300¡C and 1400¡C for 15-30 min in flowing argon atmosphere. 2TiC/Ti/Al is selected as the raw material because of its much lower exothermal quantity than elemental 3Ti/Al/2C powder system in reacting process. The purity of Ti3AlC2 is not sensitive to the final temperature, soaking time or raw material scale. Its content is maintained around 97 wt.%, even though the scale of mixed raw materials vary from 5 g to 1000 g. The synthesized samples can be easily ground into powders with a mean particle size of 4.9 µm. Synthesis mechanism shows that both Ti2AlC and Ti3AlC2 will generate from the reaction among TiC, Ti and Al below 1200¡C. Above 1300¡C, Ti2AlC will continue to react with TiC and generate Ti3AlC2. The formation of Al liquid phase above 660¡C is considered as a promoting factor in the reacting process.
C. Peng, C-A. Wang, Y. Song, Y. Huang, Materials Science and Engineering A 428 (2006) 54-58
E0165 - High temperature phase transition in Sm0.95MnO2.925
Samarium deficient SmMnO3 crystallizes in orthorhombic phase and it transforms to another orthorhombic phase at ~743 K. The above phase transformation was experimentally investigated by a variety of techniques like differential thermal analysis, dilatometry, high temperature X-ray diffraction and electrical conductivity measurements.
R.V. Wandekar, B.N. Wani, S.R. Bharadwaj, Journal of Alloys and Compounds 437 (2007) 53-57
E0164 - Crystal structure and thermal evolution of inedite alpha-Zr2O(PO4)2 and alpha-Hf2O(PO4)2
The structures of isotypic alpha-Zr2O(PO4)2 (S.G. I 2/m, a = 10.2726(6), b = 6.5957(3), c = 10.0665(5) , beta = 95.433(3)¡, V = 679.00(6) 3, Z = 4) and alpha-Hf2O(PO4)2 (S.G. I 2/m, a = 10.2301(3), b = 6.5819(2), c = 10.0075(5) , beta = 95.371(1)¡, V = 670.87(3) 3, Z = 4) have been resolved ab initio by Rietveld analysis. At variance with the beta-form, they show both MO6 and MO7 polyhedra (M = Zr, Hf), forming ribbons with the PO4 tetrahedra. A lattice energy calculation explains why the alpha-form is less stable than the beta-form, thus making the alpha-beta transition irreversible. However, the substitution of smaller HfIV for ZrIV allows to keep the alpha-framework up to 1500¡C by stabilizing the MO6 octahedra.
G. Wallez, J-P. Souron, M. Quarton, Solid State Sciences 8 (2006) 1061-1066
E0163 - Effect of acrylic polymer and nanocomposite with nano-SiO2 on thermal degradation and fire resistance of APP-DPER-MEL coating
Acrylic nanocomposite and flame retardant coatings with different acrylic polymers were prepared. The effect of molecular structure and molecular weight of acrylic resins and nanocomposite with nano-SiO2 on the interaction and char formation of ammonium polyphosphate- dipentaerythritol-melamine (APP-DPER-MEL) coating was investigated using differential thermal analysis (DTA), thermogravimetry (TG), Limiting Oxygen Index (LOI), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and fire protection test. The interaction of APP, DPER, MEL and 3F-1 acrylic resin led to the formation of intumescent coherent char at 300-450¡C. Owing to low molecular weight and lack of benzene rings, F-963 acrylic resin decomposed at lower temperature than APP, and hence their endothermic interaction was destroyed. The well-distributed nano-SiO2 particles in acrylic nanocomposite could modify char formation and anti-oxidation of char structure at high temperature. It is noted that the fire protection properties of nanocoating with acrylic nanocomposite were better than those of flame retardant coatings with conventional acrylic resins.
Z. Wang, E. Han, W. Ke, Polymer Degradation and Stability 91 (2006) 1937-1947
E0162 - Synthesis and characterization of alpha-GaPO4 single crystals grown by the flux method
Hexagonal gallium orthophosphate crystals with sizes of 6 x 4 x 1mm3 have been obtained by spontaneous nucleation using the slow cooling method from X2O-3MoO3 fluxes with X = Li, K. Infrared transmission measurements revealed samples without significant hydroxyl groups and thermal analyses have pointed out the total reversibility state of the phase transition alpha-quartz GaPO42 <-> beta-cristobalite GaPO4.
M. Beaurain, P. Armand , P. Papet, Journal of Crystal Growth 294 (2006) 396-400
E0161 - Study of the magnesia additive on the characterization of zirconia-magnesia composite sphere
Zirconia composite with varying amounts of magnesia was prepared by sol-gel technique. A series of carefully designed experiments were conducted to obtain data needed to assist the comparison of the resultant composites in terms of surface area, pore diameter, pore volume, crystalline phase and their stability to temperature. The results show that the presence of magnesia can be helpful for stabilization of zirconia composite, and different amounts of magnesia doping result in ultimate composite materials with different properties. We can tailor the structural and surface characteristics through changing the reactant ratio of magnesium chloride to zirconyl chloride to cater for its various applications, such as catalysts, chromatographic packings and so on.
Z-G. Shi, L. Xu, S-L. Da, Y-Q. Feng, Microporous and Mesoporous Materials 94 (2006) 34-39
E0160 - The A(1-x)UNbO(6-x/2) compounds (x = 0, A = Li, Na, K, Cs and x = 0.5, A = Rb, Cs): from layered to tunneled structure
Attempts to prepare alkaline metal uranyl niobates of composition A(1-x)UNbO(6-x/2) by high-temperature solid-state reactions of A2CO3, U3O8 and Nb2O5 led to pure compounds for x = 0 and A = Li (1), Na (2), K (3), Cs (4) and for x = 0.5 and A = Rb (5), Cs (6). Single crystals were grown for 1, 3, 4, 5, 6 and for the mixed Na0.92Cs0.08UNbO6 (7) compound. Crystallographic data: 1, monoclinic, P2 1/c, a = 10.3091(11), b = 6.4414(10), c = 7.5602(5) , beta = 100.65(1), Z = 4, R1 = 0.054 (wR2 = 0.107); 3, 5 and 7 orthorhombic, Pnma, Z = 8, with a = 10.307(2), 10.272(4) and 10.432(3) , b = 7.588(1), 7.628(3) and 7.681(2) , c = 13.403(2), 13.451(5) and 13.853(4) , R1 = 0.023, 0.046 and 0.036 (wR2 = 0.058, 0.0106 and 0.088) for 3, 5 and 7, respectively; 6, orthorhombic, Cmcm, Z = 8, and a = 13.952(3), b = 10.607(2) , c = 7.748(2) , R1 = 0.044 (wR2 = 0.117). The crystal structure of 1 is characterized by [UNbO6]- layers of uranophane sheet anion topology parallel to the (100) plane. These layers are formed by the association by edge-sharing of [UO5]4- chains of edge-shared UO7 pentagonal bipyramids and [NbO4]3- chains of corner-shared NbO5 square pyramids alternating along the [010] direction. The Li+ ions are located between two consecutive layers and hold them together; the Li+ ions and two layers constitute a neutral "sandwich" {(UNbO6)- - (Li)2 2+ - (UNbO6)-}. In this unusual structure, the neutral sandwiches are stacked one above another with no formal chemical bonds between the neutral sandwiches. The homeotypic compounds 3, 5, 6, 7 have open-framework structures built from the association by edge-sharing in two directions of parallel [UO5]4- chains of edge-shared UO7 pentagonal bipyramids and [Nb2O8]6- ribbons of two edge-shared NbO6 octahedra further linked by corners. In 3, 5 and 7, the mono-dimensional large tunnels created in the [001] direction by this arrangement can be considered as the association by rectangular faces of two columns of triangular face-shared trigonal prisms of uranyl oxygens. In 3 and 7, all the trigonal prisms are occupied by the alkaline metal, in 5, they are half-occupied. In 6, the polyhedral arrangement is more symmetric and the tunnels created in the [010] direction are built of face-sharing cubes of uranyl oxygens totally occupied by the Cs atoms. This last compound well illustrates the structure-directing effect of the conterion.
S. SurblŽ, S. Obbade , S. Saad, S. Yagoubi, C. Dion, F. Abraham, Journal of Solid State Chemistry 179 (2006) 3238-3251
E0159 - Mineralogical, crystallographic and morphological characteristics of natural kaolins from the Ivory Coast (West Africa)
Thirteen clay samples from four deposits in the Ivory Coast (West Africa) were studied using X-ray diffraction, thermogravimetric analysis and chemical analysis. Mineralogical, crystallographic and morphological characteristics of these samples are given. Kaolinite is the principal mineral but other minerals are present in small quantities: illite, quartz, anatase and iron oxides (oxides and oxyhydroxides). The crystallographic, morphological and surface characteristics are influenced by the presence of these impurities. In particular, the presence of iron oxides was associated with reduced structural ordering and thermal stability of kaolinite and increased specific surface area. These clays could be used in the ceramics industry to make tiles and bricks, and also in agronomy as supports for chemical fertilizers or for environmental protection by immobilising potentially toxic waste products.
J. Sei, F. Morato, G. Kra, S. Staunton, H. Quiquampoix, J.C. Jumas, J. Olivier-Fourcade, Journal of African Earth Sciences 46 (2006) 245-252
E0158 - Phase equilibria and phase transformations in the Ti-rich corner of the Fe-Ni-Ti system
While the main features of the Fe-Ni-Ti system are well known at low Ti content, literature review of the Ti-rich corner revealed inconsistencies between experimental reports. This investigation presents new experimental results, defined to remove the uncertainties concerning melting behavior and solid-state phase equilibria of the (Ni,Fe)Ti2 phase with the adjacent (Fe,Ni)Ti (B2, CsCl-type structure) and beta-Ti (A2, W-type) phases. Six samples have been prepared and examined by differential thermal analysis performed in yttria and alumina crucibles, and by scanning electron microscopy in the as-cast state as well as equilibrated at 900¡C.
P. Riani, G. Cacciamani, Y. Thebaut, J. Lacaze, Intermetallics 14 (2006) 1226-1230
E0157 - The nucleation and crystallization of fine grained leucite glass-ceramics for dental applications
Objectives. The aims of the study were to control the nucleation and crystal growth of selected aluminosilicate glass powders, to produce uniform leucite glass-ceramic microstructures consisting of fine (<1000 nm) grained leucite crystals. Methods. A starting glass composition of wt%; 64.2% SiO2, 16.1% Al2O3, 10.9% K2O, 4.3% Na2O, 1.7% CaO, 0.5% LiO2 and 0.4% TiO2 was heated in an electric furnace and later quenched to produce glasses. The glass powders were ball milled to two different particle sizes and heattreated using one and two-step crystallization heat treatments. Dta, Xrd, and Sem analyses was used to characterise and explore the crystallization kinetics of the glasses. Results. Selected heat treatments of the glass powders produced a uniform distribution of fine tetragonal leucite crystals (mean±S.D.) 0.1±0.2 µm2 in the glassy matrix, with minimal matrix microcraking in the glass-ceramics produced. The addition of a two-step heat treatment increased the leucite volume fraction in all instances. Significance. Selected crystallization heat treatments and powder particle sizes were used to control the leucite crystal size, distribution and volume fraction, in order to produce uniformly distributed ultra fine grained tetragonal leucite glass-ceramics for dental applications.
M.J. Cattell, T.C. Chadwick, J.C. Knowles, R.L. Clarke, D.Y.D. Samarawickrama, Dental Materials 22 ( 2006 ) 925-933
E0156 - Magnetically soft nanomaterials for high-temperature applications
Nanomaterials for high-temperature applications must meet two basic requirements: (i) very soft magnetic behaviour at elevated temperature, and (ii) stable properties at elevated temperature for a long time (application time). The latter requirement is related to thermal stability of nanocrystalline structure of these materials. The paper presents the current status of research in the field of magnetically soft nanocrystalline materials, highlighting the influence of alloy composition on magnetic properties and their stability at elevated temperatures during very long time annealing (several thousands of hours at temperature up to 550¡C). It was found that modification of the alloys allows to tailor their chemical composition and manufacturing process to particular application temperature requirements. FINEMETs are the most suitable materials for application at temperature, T, up to 300¡C, FINEMET modified by cobalt (Fe0.6Co0.4)73.5Cu1Nb3Si13.5B9 (at.%) for T = 300-350¡C, NANOPERM for T = 350-400¡C and HITPERM (Fe0.6Co0.4)86Hf7B6Cu1 for T = 400-550¡C.
T. Kulik, J. Ferenc, A. Kolano-Burian, X.B. Liang, M. Kowalczyk, Materials Science and Engineering A 449-451 (2007) 397-400
E0155 - High temperature behavior of ball-milled Al-Ni-Ce-Co alloys
Microstructure of ball-milled Al85Ni8Ce5Co2 powder indicates the formation of fine nanoparticles with some amorphous fraction. Thermal analysis revealed that the release of internal stress and grain growth is followed by the redistribution and possible melting of high solute concentration interfaces. In addition, mechanical properties of compacted powder specimens were also investigated.
A. RŽvŽsz, P. Henits, Zs. Kovacs, Journal of Alloys and Compounds 434-435 (2007) 424-427
E0154 - An investigation into fire protection and water resistance of intumescent nano-coatings
The objective of the paper is to develop nano-coatings that can provide good fire protection for the underlying substrate. The thermal degradation and fire resistance of nano-coatings have been investigated by differential thermal analysis (DTA), thermogravimetry (TG) and fire performance test. It is illustrated that nano-coatings can give an excellent fire resistance. The dispersion state and bonding of nano-SiO2 particles are characterized by the use of transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FT-IR). Water immersion test, fire performance test and mechanical test reveal that sodium silicate coating is vulnerable to water and hence fire resistance is severely damaged by water immersion, whereas nano-coatings demonstrate good water resistance and fire resistance even after water immersion.
Z. Wang, E. Han, W. Ke, Surface & Coatings Technology 201 (2006) 1528-1535
E0153 - Preparation of nanocrystalline Mn-Al-C magnets by melt spinning and subsequent heat treatments
Mn54Al44C2 ribbon samples have been prepared by melt spinning in a single-phase epsilon hexagonal disordered state and its exothermal transformation at around 500¡C into a tetragonal L10 type magnetic structure (t-phase) was followed by DTA, DSC, X-ray diffraction and thermomagnetic measurements. The metastable t-phase stabilized by carbon addition could be transformed reversibly into the epsilon-phase at around 800¡C, without decomposition into the stable Al8Mn5 and beta manganese phases. The almost constant Curie temperature obtained for partially transformed two-phase samples indicated a compositionally invariant transformation. By grinding the thin (25 µm) ribbon into sub-millimeter flakes, a bulk anisotropic magnet could be compacted by magnetic field oriented powder technology.
E. Fazakas, L.K. Varga, F. Mazaleyrat, Journal of Alloys and Compounds 434-435 (2007) 611-613
E0152 - Hydrothermal synthesis and characterization of a new zinc phosphate [Zn2.5(HPO4)2(PO4)][C6H10N2].5H2O
A new two-dimensional zinc phosphate, [Zn2.5(HPO4)2(PO4)][C6N2H10].5H2O (denoted in the following as ZnP-2AMP), with alternating inorganic and organic layers has been synthesized hydrothermally using 2-aminomethylpyridine (2AMP) as the structure-directing agent. This compound represents the first structure with a Zn/P ratio of 5/6. The structure of this compound, determined by single crystal X-ray diffraction, consists of anionic parallel [Zn2.5(HPO4)2(PO4)(H2O)2]2 sheets built up from ZnO4, ZnO2(H2O)4, PO4 and HPO4, alternating with thick slabs of organic molecules (C6H10N2)2+ and water molecules, the octahedral ZnO2(H2O)4 being enclosed in each [4^6 8^2 12^2] cage. The organic cations are linked to the anionic sheets through hydrogen bonds. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the partial attribution of phosphorus and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups. Additional characterization of the compound has also been performed by IR spectroscopy and TG-DTA analyses.
R. Kefi, C. Ben Nasr, F. Lefebvre, M. Rzaigui, Polyhedron 25 (2006) 2953-2958
E0151 - Magnetically soft nanomaterials for high-temperature applications
The paper summarizes the current status of research in the field of magnetically soft nanocrystalline materials especially highlighting the influence of alloy composition on structure and magnetic properties as well as their stability at elevated temperature during very long time annealing (several thousand hours at temperature up to 550¡C). Modification of the alloys allows to tailor their chemical composition and manufacturing process to particular application temperature requirements. FINEMET is the most suitable material for application at temperature up to 300¡C, FINEMET modified by cobalt (Fe0.6Co0.4)73.5Cu1Nb3Si13.5B9 for 300¡C<T < 350¡C, NANOPERM for 350¡C<T < 400¡C, and HITPERM (Fe0.6Co0.4)86Hf7B6Cu1 for 400¡C<T < 550¡C.
T. Kulik, J. Ferenc, A. Kolano-Burian, X.B. Liang, M. Kowalczyk, Journal of Alloys and Compounds 434-435 (2007) 623-627
E0149 - Barium borosilicate glass - a potential matrix for immobilization of sulfate bearing high-level radioactive liquid waste
Borosilicate glass formulations adopted worldwide for immobilization of high-level radioactive liquid waste (HLW) is not suitable for sulphate bearing HLW, because of its low solubility in such glass. A suitable glass matrix based on barium borosilicate has been developed for immobilization of sulphate bearing HLW. Various compositions based on different glass formulations were made to examine compatibility with waste oxide with around 10 wt% sulfate content. The vitrified waste product obtained from barium borosilicate glass matrix was extensively evaluated for its characteristic properties like homogeneity, chemical durability, glass transition temperature, thermal conductivity, impact strength, etc. using appropriate techniques. Process parameters like melt viscosity and pour temperature were also determined. It is found that SB-44 glass composition (SiO2: 30.5 wt%, B2O3: 20.0 wt%, Na2O: 9.5 wt% and BaO: 19.0 wt%) can be safely loaded with 21 wt% waste oxide without any phase separation. The other product qualities of SB-44 waste glass are also found to be on a par with internationally adopted waste glass matrices. This formulation has been successfully implemented in plant scale.
C.P. Kaushik, R.K. Mishra, P. Sengupta, Amar Kumar, D. Das, G.B. Kale, Kanwar Raj, Journal of Nuclear Materials 358 (2006) 129-138
E0148 - Effect of Pb addition on ageing behavior of AZ91 magnesium alloy
The ageing behavior of AZ91 alloy containing 2 wt.% lead is investigated. The results show that addition of Pb suppresses the discontinuous precipitation and thereby slows down the ageing kinetics. Even though the peak hardness obtained for both alloys is almost same, the peak hardness reaches after 2400 min for Pb added alloy against 900 min for the base alloy. The presence of Pb in solid solution might have inhibited the diffusion of Al and Mg atoms, which is essential for the formation, and growth of discontinuous precipitation in this alloy.
A. Srinivasan, U.T.S. Pillai, B.C. Pai, Materials Science and Engineering A 452-453 (2007) 87-92
E0147 - Influence of expandable graphite on fire resistance and water resistance of flame-retardant coatings
Expandable graphite (EG) coating and ammonium polyphosphate-pentaerythritol-melamine (APP-PER-MEL) coating were prepared. Thermal degradation and char formation of the coatings were investigated by differential thermal analysis (DTA), thermogravimetry (TG), X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The results have shown that the anti-oxidation and fire-resistant properties of expandable graphite coating containing EG with size of 74 lm are better than those of APP-PER-MEL coating. The static immersion test was applied to study water resistance of the coatings, and the fire protection test and mechanical test were used to analyse heat insulation and mechanical properties of coatings before and after water immersion. The fire-resistant and mechanical properties of APP-PER- MEL coating were severely damaged by water immersion, whereas EG coating containing 8.5% EG with size of 74 lm could retain the good fire resistance even after 500 h water immersion.
Z. Wang, E. Han, W. Ke, Corrosion Science 49 (2007) 2237-2253
E0146 - Proof of the ISS-concept for LTA and FAU membranes and their characterization by extended gas permeation studies
Molecular sieve membranes are expected to separate molecules by size and shape provided that the intercrystalline defect transport is negligible. However, in the case of a non-negligible mass transport through the grain boundaries in the polycrystalline zeolite layer, the separation properties of the membrane become influenced by both the regular and defective transport. Nevertheless, also in this case proper separation performance is found due to adsorptive and/or diffusive interactions of the mixture components with the membrane. In a previous report [M. Noack, P. Kšlsch, A. Dittmar, M. Stšhr, G. Georgi, R. Eckelt, J. Caro, Micropor. Mesopor. Mater. 97 (2006) 88] the concept of crystal intergrowth supporting substances (ISS) was demonstrated. The charge neutralization of the negatively charged crystal surfaces of a growing MFI membrane by the positively charged ISS molecules improves the crystal intergrowth and results in a higher permeation selectivity. LTA and FAU membranes can separate water-organic mixtures in an excellent way but they fail in shapeselective gas separations. Therefore, many attempts were made to improve the separation properties of LTA and FAU membranes for gases. Zeta potential measurements on the Al-rich zeolite crystals LTA and FAU show a strong negative surface charge like it was found in [Noack et al., 2006] for MFI. In this work LTA and FAU multi-layer membranes were prepared by using an ISS. These membranes were characterized by SEM, XRD, permporosimetry, single gas permeation in combination with different probe molecules for the selective blocking of the micro and mesopore system. The results are discussed on the basis of pore condensation or pore narrowing according to the Kelvin and Halsey equations. Repeated strong de-watering of the hydrophilic LTA and FAU membranes have changed the membrane structure.
M. Noack, P. Kšlsch, A. Dittmar, M. Stšhr, G. Georgi, M. Schneider, U. Dingerdissen, A. Feldhoff, J. Caro, Microporous and Mesoporous Materials 102 (2007) 1-20
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- 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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