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Phases Present (phase + present)
Selected AbstractsA Study of the Influence of Composition on the Microstructural Properties of ZnO/Al2O3 Mixed Oxides,EUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 7 2009Shaojun Miao Abstract A series of ZnO/Al2O3 mixed oxide samples with varyingZn/Al ratio is prepared by coprecipitation, ageing, drying, and calcination. Samples are investigated in the state after drying and calcination. The applied methods include X-ray diffraction, solid-state 27Al magic-angle spinning nuclear magnetic resonance spectroscopy, transmission electron microscopy and thermogravimetric experiments coupled with evolved gas analysis. Phases present in the dried precursor samples include hydrozincite, zaccagnaite, and an unknown phase. After calcination zinc oxide and spinel can be found. All results indicate the substitution of Al ions for Zn ions in zinc oxide of zinc-rich samples. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Exciton,Exciton Annihilation in Mixed-Phase Polyfluorene FilmsADVANCED FUNCTIONAL MATERIALS, Issue 1 2010Paul E. Shaw Abstract Singlet,singlet annihilation is studied in polyfluorene (PFO) films containing different fractions of , -phase chains using time-resolved fluorescence. On a timescale of >15,ps after excitation, the results are fitted well by a time-independent annihilation rate, which indicates that annihilation is controlled by 3D exciton diffusion. A time-dependent annihilation rate is observed during the first 15,ps in the glassy phase and in the , -phase rich films, which can be explained by the slowdown of exciton diffusion after excitons reach low-energy sites. The annihilation rate in the mixed-phase films increases with increasing fraction of , -phase present, indicating enhanced exciton diffusion. The observed trend agrees well with a model of fully dispersed, -phase chromophores in the surrounding glassy phase with the exciton diffusion described using the line-dipole approximation for an exciton wavefunction extending over 2.5,nm. The results indicate that glassy and, -phase chromophores are intimately mixed rather than clustered or phase-separated. [source] High-resolution magic-angle spinning NMR for the identification of reaction products directly from thin-layer chromatography spotsMAGNETIC RESONANCE IN CHEMISTRY, Issue 10 2007Scott A. Bradley Abstract We have investigated the prospect of identifying organic reaction products directly from separated thin-layer chromatography (TLC) spots with high-resolution magic-angle spinning (HRMAS) NMR. The concept is to use the TLC spots for NMR analysis so that spectra can be obtained before the reaction is worked up, but without having to elute the product from the TLC stationary phase. Thus, the separated spot is scraped from the plate, transferred to an HRMAS sample rotor, and suspended with a deuterated solvent. Herein, we describe the effects of having the stationary phase present during NMR acquisition. Using a Varian 4 mm gHX Nanoprobe and rotenone as a test compound, we found that the presence of the stationary phase during NMR acquisition resulted in (i) a large, broad ,background' signal near 4.6 ppm and (ii) a decrease in the signal-to-noise ratio due to the adsorption of the product molecules to the adsorbent. However, both effects could be adequately and conveniently eliminated. The background signal was removed by using either a CPMG pulse sequence or chemical exchange. The adsorption was avoided by using a more polar solvent system. Finally, we found that spectra with good signal-to-noise ratio and resolution could be acquired in a matter of minutes even for cases of limited product concentration. Therefore, we believe the technique has value and provides the organic chemist with another option to obtain NMR data critical for structural elucidation or verification. Copyright © 2007 John Wiley & Sons, Ltd. [source] Mn and Si influence on the hyperfine properties of the fcc and hcp phases in the Fe,Mn and Fe,Mn,Si systemsPHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 6 2009Javier Martínez Abstract A study of the hyperfine properties of the fcc and hcp phases of the Fe,Mn and Fe,Mn,Si systems, performed on a systematic and accurate set of samples belonging to the 15 at% to 30 at% Mn and 0 at% to 12 at% Si composition ranges, is presented. The samples were characterized using Conversion Electron Mössbauer Spectroscopy. The evolution with the Mn and Si contents of the hyperfine parameters of both phases has been determined. A constancy of the isomer shift parameter of the hcp phase with both constituents of the alloy was observed. While constancy and a linear decrease of the isomer shift values of the fcc phase with Mn and Si, respectively, were determined. The magnetic hyperfine field of the fcc phase presents two different values depending on the Mn content in the binary system and a decrease with the addition of Si when the ternary alloy is considered. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Glass-to-Metal Seal Interfacial Analysis using Electron Probe Microscopy for Reliable Solid Oxide Fuel CellsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 4 2009Scarlett J. Widgeon The chemical compatibility between sealing glasses and interconnect materials for solid oxide fuel cells (SOFCs) has been studied in SOFC environments. Two borate-based glass compositions were sealed to interconnect materials, 441 stainless-steel (441SS) and Mn1.5Co1.5O4 -coated 441SS. The Mn1.5Co1.5O4 -coated 441SS coupons were analyzed as-received using X-ray diffraction (XRD) and electron probe microanalysis (EPMA) to obtain structural information and concentration profiles, respectively. The concentration profiles and the lack of Fe-containing phases present in the XRD spectrum show Fe is present throughout the coating, suggesting that Fe is partially substituted in the Mn1.5Co1.5O4 spinel. The glass,metal coupons were heat treated in air at 750°C for 500 h. The specimens were analyzed by EPMA and scanning electron microscope (SEM) to obtain images of the glass microstructure at the interface, to verify seal adherence, and to record concentration profiles across the glass,metal interface, with an emphasis on Cr. In total, four seal configurations were tested and analyzed, and in all cases the glasses remained well adhered to the metal and coating, and there was no microstructural evidence of new reaction phases present at the interface. There was slight diffusion of Cr from the 441SS into the sealing glasses, and Cr diffusion was hindered by the coating on the coated 441SS samples. [source] Microstructure and Creep Behavior of a Si3N4,SiC MicronanocompositeJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2009Monika Ka, iarová The microstructure and its influence on the creep behaviour of carbon derived Si3N4 -SiC micro/nanocomposite tested in bending at temperatures from 1200° to 1400°C in air has been studied. No phase and microstructure change after creep test implied that material is stable at tested temperature range. After creep test only partial crystallization of glassy intergranular phase has been observed. Creep parameters n close to 1, apparent activation energy around 350 kJ/mol together with TEM observation indicated that the main creep mechanisms is solution precipitation controlled by interface reaction in combination with grain boundary sliding caused by the amorphous intergranular phases present in microstructure. However, the grain boundary sliding is hindered by local SiC particles interlocking neighboring Si3N4 grains. [source] Ferric iron in SNC meteorites as determined by Mössbauer spectroscopy: Implications for martian landers and martian oxygen fugacityMETEORITICS & PLANETARY SCIENCE, Issue 12 2003M. Darby DYAR Also, considerable current effort is being made to understand the oxygen fugacity of martian magmas because of the effect of fO2 on mineral chemistry and crystallization processes. For these 2 reasons, the present study was conceived to acquire room temperature Mössbauer spectra of mineral separates and whole rock samples of 10 SNC meteorites. The results suggest that mineral identification using remote application of this technique will be most useful when the phases present have distinctive parameters arising from Fe in very different coordination polyhedra; for example, pyroxene coexisting with olivine can be discriminated easily, but opx versus cpx cannot. The MER goal of using Mössbauer spectroscopy to quantify the relative amounts of individual mineral species present will be difficult to satisfy if silicates are present because the lack of constraints on wt% FeO contents of individual silicate phases present will make modal calculations impossible. The remote Mössbauer spectroscopy will be most advantageous if the rocks analyzed are predominantly oxides with known stoichiometries, though these phases are not present in the SNCs. As for the detection of martian oxygen fugacity, no evidence exists in the SNC samples studied of a relationship between Fe3+ content and fO2 as calculated by independent methods. Possibly, all of the Fe3+ observed in olivine is the result of dehydrogenation rather than oxidation, and this process may also be the source of all the Fe3+ observed in pyroxene. The observed Fe3+ in pyroxene also likely records an equilibrium between pyroxene and melt at such low fO2 that little or no Fe3+ would be expected. [source] |