The influence of yttrium on a typical SnO2 varistor system: Microstructural and electrical features

The influence of yttrium oxide, Y2O3, on the microstructure development of the SnO2·Co3O4·Nb2O5 typical varistor system was studied with scanning (SEM) and transmission (TEM) electron microscopies. The different phases present in the studied samples were characterized through XRD, EDS and selected area diffraction patterns (SAD). Particles of Co2SnO4 were observed with TEM in every sample, whereas clusters of the pyrochlore phaseY2Sn2O7 were observed with SEM in samples with 0.05, 0.10 and 0.25 mol% ofY2O3. The higher non-linearity (α = 16) was achieved with the addition of 0.05 mol% of Y2O3. The influence of the secondary phases on the electrical properties is also addressed in this work.Fil: Parra, Rodrigo. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Maniette, Y.. Universidade Estadual Paulista Julio de Mesquita Filho; BrasilFil: Varela, J. A.. Universidade Estadual Paulista Julio de Mesquita Filho; BrasilFil: Castro, Miriam Susana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentin

Mechanochemical synthesis of PZT powders

PZT ceramic powders were successfully prepared from the mixture of PbO, ZrO2 and TiO2 by mechanochemical synthesis in a planetary ball mill, under different milling conditions. Phase evolution during synthesis was monitored by X-ray diffraction analysis. Intensive milling resulted in formation of the nanocrystalline, perovskite PZT powders after 1 h of milling. This is a significant improvement in comparison to milling conditions reported by other authors. Depending on milling parameters the presence of some other phases, such as unreacted ZrO2, was also detected in some samples. The changes in powder size and morphology due to intensive milling, were determined by SEM and TEM, while BET analysis was used to determine specific surface area of the powders. Conclusions about processes taking place during mechanochemical synthesis of PZT powders were made based on the results of characterization. (C) 2002 Elsevier B.V. B.V. All rights reserved

High spatial resolution semi-automatic crystallite orientation and phase mapping of nanocrystals in transmission electron microscopes

International audienceA semi-automatic technique for the mapping of nanocrystal phases and orientations in a transmission electron microscope (TEM) is described. It is based primarily on the projected reciprocal lattice geometry, but also utilizes the intensity of reflections that are extracted from precession-enhanced electron diffraction spot patterns of polycrystalline materials and multi-material composites. At the core of the method, experimental (precession-enhanced) electron diffraction spot patterns are cross correlated with pre-calculated templates for a set of model structures. The required hardware facilitates a scanning-precession movement of the primary electron beam on the polycrystalline and/or multi-material sample and can be interfaced to any newer or older mid-voltage TEM. The software that goes with this hardware is so flexible in its intake of experimental data that it can also create crystallite orientation and phase maps of nanocrystals from the amplitude part of Fourier transforms of high resolution TEM images. Experimentally obtained crystallite orientation and phase maps are shown for a clausthalite nanocrystal powder sample, polycrystalline aluminum and copper films, fine-grained palladium films, as well as MnAs crystallites that are partly embedded in a GaAs wafer. Comprehensive open-access and commercial crystallographic databases that may provide reference data in support of the nanocrystal phase identification process of the software are briefly mentioned. (C) 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinhei

Improvement of the Mo/TiO2-Al2O3 catalyst by the control of the sol-gel synthesis

Traditional hydrotreating catalysts are constituted by molybdenum deposited on Al2O3 promoted by nickel and phosphorous. Several studies have shown that TiO2-Al2O3 mixed oxides are excellent supports for the active phases. Results concerning the preparation, characterization and testing of molybdenum catalyst supported on titania-alumina are presented. The support was prepared by sol-gel route using titanium and aluminum isopropoxides, the titanium one chelated with acetylacetone (acac) to promote similar hydrolysis ratio for both the alcoxides. The effect of nominal molar ratio [Ti]/[Ti+Al] on the microstructural features of nanometric particles was analyzed by X-Ray Diffraction, N-2 Adsorption Isotherms and Transmission Electron Microscopy. The catalytic activity of Mo impregnated supports was evaluated using the thiophene hydrodesulfurization at different temperatures and atmospheric pressure. The pores size distribution curve moves from the micropores to the mesopores by increasing the Ti contents, allowing the fine tuning of average size from 2.5 to 6 nm. Maximal (367 m(2).g(-1)) and minimal (127 m(2).g(-1)) surface area were found for support containing [Ti]/[Ti+Al] ratio equal to 0.1 and 1, respectively. The good mesopore texture of alumina-titania support with [Ti]/[Ti+Al] molar ratio between 0.3 and 0.5 was found particularly valuable for the preparation of well dispersed MoS2 active phase, leading to HDS catalyst with somewhat higher activity than that prepared using a commercial alumina support

Development of metal - SiO2 nanocomposites in a single-step process by the polymerizable complex method

This work presents the synthesis and characterization of SiO2:metal (Ni, Co, Ag, and Fe) nanocomposites processed by the polymerizable complex method. The polymeric precursor solutions obtained were characterized by means of FT-Raman and C-13 NMR spectroscopy. The results show the formation of a hybrid polymer with carbon and silicon in the macromolecule chain and the transition metal cation arrested within this polymeric chain. The nanocomposites are formed during the controlled polymeric precursor pyrolysis. The reduction of the metal cation is promoted by the CO/CO2 atmosphere resulting from the pyrolysis of the organic material. Microstructural characterization, performed by TEM and X-ray diffraction (XRD), showed that the nanocomposites are formed by metal nanoparticles embedded in a amorphous matrix formed by SiO2 and carbon. In the SiO2:Fe system, Fe3C was also detected by XRD

Microstructural and morphological analysis of pure and Ce-doped tin dioxide nanoparticles

Structural morphological studies in pure and Ce-doped tin dioxide nanoparticles with high stability against particle growth were performed in samples, obtained using the polymeric precursor method and prepared at different annealing temperatures. A Ce-rich surface layer was used to control the particle size and stabilize SnO2 against particle growth. The formation of this segregated layer can contribute to a decreased surface energy, acting in the driving force, or reducing the surface mobility. Only the cassiterite SnO2 phase was observed below 1000 degreesC and a secondary phase (CeO2) was observed for the Ce-doped SnO2 at temperatures higher than 1000 degreesC, when de-mixing process occurs. The evolution of crystallite size, microstrain and morphology of the nanoparticles with annealing temperatures was investigated by X-ray diffraction (XRD), associated to Rietveld refinements, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). (C) 2002 Elsevier B.V. Ltd. All rights reserved