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Chemical Homogeneity (chemical + homogeneity)
Selected AbstractsHigh-Zirconium-Content Nano-Sized Bimodal Mesoporous SilicasEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 13 2006David Ortiz de Zárate Abstract Silica-based nanoparticulated bimodal mesoporous materials with high Zr content (43 , Si/Zr , 4) have been synthesized by a one-pot surfactant-assisted procedure from a hydroalcoholic medium using a cationic surfactant (CTMABr = cetyltrimethylammonium bromide) as structure-directing agent, and starting from molecular atrane complexes of Zr and Si as hydrolytic inorganic precursors. This preparative technique allows optimization of the dispersion of the Zr guest species in the silica walls. The bimodal mesoporous nature of the final high surface area nano-sized materials is confirmed by XRD, TEM, and N2 adsorption,desorption isotherms. The small intraparticle mesopore system (with pore sizes around 2,3 nm) is due to the supramolecular templating effect of the surfactant, while the large mesopores (around 12,24 nm) have their origin in the packing voids generated by aggregation of the primary nanometric mesoporous particles. The basicity of the reaction medium seems to be a key parameter in the definition of this last pore system. The effects induced by the progressive incorporation of Zr atoms on the mesostructure have been examined, and the local environment of the Zr sites in the framework has been investigated by UV/Vis spectroscopy. Observations based on the consequences of post-treatments of the as-synthesized materials with HCl/ethanol mixtures corroborate that the atrane method leads to Zr-rich materials showing enhanced site accessibility and high chemical homogeneity throughout the pore walls. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006) [source] Synthesis of Nd-YAG material by citrate-nitrate sol-gel combustion route,ADVANCED ENGINEERING MATERIALS, Issue 4 2007L. Costa Polycrystalline, Neodymium doped, yttrium aluminum garnet Nd:YAG is a functional materials for solid-state lasers. The synthesis of Nd:YAG powders requires a strict control of the precursor reactivity and composition. Sol-gel citrate-based methods increase the chemical homogeneity and reactivity of the precursor powder. Calcination performed around 900,°C leads to the formation of pure YAG phase at temperatures much lower than the temperature required for the solid-state reaction (1600,°C). [source] Microwave-Hydrothermal Synthesis of Nanocrystalline Zirconia PowdersJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 11 2001Federica Bondioli Nanosized zirconium oxide (ZrO2) powders were prepared by adding NaOH to a zirconyl chloride aqueous solution under microwave-hydrothermal conditions. The obtained results showed that the tetragonal polymorph increased with increasing NaOH concentration in the starting solution and reached the maximum value by using 1M ZrOCl2. The microwave-assisted hydrothermal synthesis is expected to be able to process continuously, and may lead to energy savings because of rapid heating to temperature and increased kinetics of crystallization. This method is very simple and can lead to powders with desirable characteristics such as very fine size, narrow size distribution, and good chemical homogeneity. [source] Design of Ceramic Materials for Chemical Sensors: Effect of SmFeO3 Processing on Surface and Electrical PropertiesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2001Hiromichi Aono Perovskite-type SmFeO3 powders were prepared by the thermal decomposition of a heteronuclear complex, Sm(Fe(CN)6)·4H2O and by solid-state reaction between the corresponding single oxides, Sm2O3 and Fe2O3. The thermal decomposition behavior of the complex was studied by thermogravimetric analysis. X-ray diffractometry was used to investigate the structure of the products from the complex thermal decomposition and the formation of SmFeO3 from the oxide mixture. Powders prepared by both methods were used to deposit thick films onto alumina substrates with comb-type gold electrodes. The microstructure and chemical homogeneity of the film surfaces were investigated by scanning electron microscopy and Auger electron spectroscopy. Thick SmFeO3 single-phase films having a homogeneous elemental distribution on the surface were obtained when powder prepared by thermal decomposition of the complex was used for deposition, even when the powder was fired at low temperature (800°C). Surface chemical analysis was performed by X-ray photoelectron spectroscopy (XPS). The O 1s XPS line was deconvoluted into two peaks, attributed to adsorbed oxygen (Oad) and oxygen in the lattice (Olattice). Quantitative analysis showed that the surface coverage of iron, expressed as Fe/(Fe + Sm), was larger for the films prepared using the solid-state reacted powder. Although the Olattice/(Fe + Sm) atomic ratio was not influenced by the processing procedures (and, thus, by iron surface coverage), the amount of Oad decreased with increasing iron surface coverage. A model of the SmFeO3 surface was used to determine that the outermost layer of the perovskite-type SmFeO3 prepared from the complex consisted mainly of samarium ions that could each bond four adsorbed oxygen ions. A single oxygen ion could adsorb onto an iron ion, and therefore, the content of adsorbed oxygen was lower for the film prepared from the solid-state reacted powders, which showed larger iron surface coverage. Electrical conductance measurements, performed with increasing temperature in different gaseous environments, confirmed these findings. Higher conductances and lower activation energies were observed for the films with larger samarium surface coverage. [source] Cloud-Point Pressure Curves of Ethene/Poly[ethylene- co -((meth)acrylic acid)] MixturesMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 4 2003Michael Buback Abstract Ethene-methacrylic acid (MAA) and ethene-acrylic acid (AA) copolymers of narrow polydispersity and high chemical homogeneity have been synthesized at acid unit copolymer contents up to 9 mol-% within a continuously operated stirred tank reactor at overall monomer conversions of about 2%. Cloud-point pressures (CPPs) of mixtures of 3 wt.-% copolymer in ethene (E) have been measured in an optical high-pressure cell at pressures and temperatures up to 3,000 bar and 260,°C, respectively. The CPP weakly increases with acid copolymer content up to about 3.5 mol-%. Toward higher acid contents, the CPP is strongly enhanced, in particular at the lower edge of the experimental temperature range at around 200,°C. This increase in CPP is more pronounced for the AA than for the MAA systems. The data suggest that hydrogen-bonding interactions are operative in the pressurized E/poly(E- co -(M)AA) mixtures at temperatures of 260,°C and perhaps even above. E-AA and E-MAA copolymers with acid contents of about 5.6 mol-% have also been completely methyl-esterified to yield the associated methyl esters. The CPPs of the resulting E-methyl acrylate and E-methyl methacrylate copolymers in mixtures with E are significantly below the CPPs of the corresponding E/poly(E- co -(M)AA) systems. Cloud-point pressure vs temperature curves for several E/poly(E- co -methacrylic acid) systems. The subscripts denote copolymer content in mol-%. A cloud-point pressure curve for E/polyethylene (PE) is included for comparison. [source] Verallgemeinerungsfähige Merkmale und Besonderheiten des SprühkompaktierensMATERIALWISSENSCHAFT UND WERKSTOFFTECHNIK, Issue 1 2003K. Bauckhage Sprayforming; Modelling Microstructure; Geometry Abstract Dadurch, daß beim Sprühkompaktieren die schnelle Erstarrung und Abkühlung des Materials das Ausmaß von Entmischungen eindämmen, können Makroseigerungen unterbunden und Anreicherungen an den Korngrenzen deutlich verringert werden. Ferner wird das Risiko der Lunker- und Warmrißbildung durch den Impuls des Massetransportes während des Kompaktiervorganges stark reduziert. Dies bedeutet, daß solche Materialien, die bspw. beim Gießen zu starker Seigerung neigen und besonders anfällig für die Lunkerbildung und/oder Warmrißbildung sind sowie bei Umformverfahren zur Zeilenbildung von Carbiden, Nitriden oder Sulfiden neigen, mit Hilfe des Sprühkompaktierens im Freiformverfahren mit großen Abmaßen chemisch homogen und fehlerfrei herstellbar werden. Ein besonderes Merkmal sprühkompaktierter Deposits ist ihr feines Gefüge und ihre vergleichsweise hohe Duktilität. Die Besonderheiten des neuartigen Urformverfahrens werden anhand von Beispielen erläutert. Characteristic Features and Specific Qualifications of the Sprayforming Process to be Generalized The solidification and cooling process of spray formed materials predominates the extent of any segregation and separation process, which is conducive to avoid macro-segregation and to diminish concentration of alloying components at the grain boundaries. The risk of coarse porosity or of hot cracking is reduced significantly by the momentum of the mass flow during spray deposition. This means that those materials which e.g. during the casting process tend to establish strong segregation effects and cavities and/or hot cracks as well as those which tend to create filaments of carbides, nitrides or sulphides during rolling can be generated by the spray forming process in large dimensions with chemical homogeneity and without any of those defects. A characteristic feature of spray formed materials is the fine equiaxed grain structure and the high ductility. Specific features of this new free forming process will be discussed. [source] Petrology of Martian meteorite Northwest Africa 998METEORITICS & PLANETARY SCIENCE, Issue 5 2008Allan H. TREIMAN This 456-gram, partially fusion-crusted meteorite consists of (by volume) ,75% augite (core composition Wo39En39Fs22), ,9% olivine (Fo35), ,7% plagioclase (Ab61An35) as anhedra among augite and olivine, ,3.5% low-calcium pyroxenes (pigeonite and orthopyroxene) replacing or forming overgrowths on olivine and augite, ,1% titanomagnetite, and other phases including potassium feldspar, apatite, pyrrhotite, chalcopyrite, ilmenite, and fine-grained mesostasis material. Minor secondary alteration materials include "iddingsite" associated with olivine (probably Martian), calcite crack fillings, and iron oxide/hydroxide staining (both probably terrestrial). Shock effects are limited to minor cataclasis and twinning in augite. In comparison to other nakhlites, NWA 998 contains more low-calcium pyroxenes and its plagioclase crystals are blockier. The large size of the intercumulus feldspars and the chemical homogeneity of the olivine imply relatively slow cooling and chemical equilibration in the late- and post-igneous history of this specimen, and mineral thermometers give subsolidus temperatures near 730 °C. Oxidation state was near that of the QFM buffer, from about QFM-2 in earliest crystallization to near QFM in late crystallization, and to about QFM + 1.5 in some magmatic inclusions. The replacement or overgrowth of olivine by pigeonite and orthopyroxene (with or without titanomagnetite), and the marginal replacement of augite by pigeonite, are interpreted to result from late-stage reactions with residual melts (consistent with experimental phase equilibrium relationships). Apatite is concentrated in planar zones separating apatite-free domains, which suggests that residual magma (rich in P and REE) was concentrated in planar (fracture?) zones and possibly migrated through them. Loss of late magma through these zones is consistent with the low bulk REE content of NWA 998 compared with the calculated REE content of its parent magma. [source] ROMAN WINDOW GLASS: A COMPARISON OF FINDINGS FROM THREE DIFFERENT ITALIAN SITESARCHAEOMETRY, Issue 2 2010R. ARLETTI Thirty-three samples of window glass and five glass lumps coming from three Italian archaeological sites,the Suasa excavations (Ancona, settled from the third century bc to the fifth to sixth centuries ad), the Roman town of Mevaniola (Forlì-Cesena, settled from the Imperial Age up to the fourth century ad) and Theodoric's Villa of Galeata (Forlì-Cesena, settled from the sixth century ad onwards),were analysed to track the changes in the chemical composition and manufacturing technology of window glass through the centuries. The aims of this study were: (1) to establish the origin of the raw materials; (2) to verify the chemical homogeneity among samples coming from different sites and/or produced using different techniques; and (3) to sort the samples into the compositional groups of ancient glass. The analysis of all the chemical variables allowed two groups to be distinguished: (a) finds from Mevaniola and Suasa; and (b) finds from Galeata. All the samples had a silica,soda,lime composition, but the analysis of minor elements,in particular, of Fe, Mn, and Ti,made it possible to split the samples into two groups, with the higher levels of these elements always found in the Galeata samples (HIMT glass). In conclusion, it can be asserted that the main differences between the samples are related to their chronology. [source] | ||||||||||