EXAFS and XRD Study of the Structural Evolution during Isothermal Sintering of SnO2 Xerogels

The formation of an ordered (crystalline) phase during isothermal sintering of SnO2 monolithic xerogels, at 200, 250, 300, 400, 500, 600 and 700°C, has been analyzed by the combined use of EXAFS and XRD techniques. For the desiccated gel (110°C), EXAFS results show the formation of small microcrystallites with the incipient cassiterite structure. Between 110 and 250°C, the dehydratation reaction leads to an amorphization evidenced by a decrease of the long and short range crystallographic order. It is due to fissure formation in the xerogel network. For higher temperatures, a continuous coagulation of the crystallites occurs, leading to grain growth. Grain and pore growth obeys the same kinetic relation, so that the microstructure grows by simple enlargement while its morphology is static.

LiNbO3 thin films prepared from a polymeric precursor method

LiNbO3 thin films were prepared from polymeric precursor method by dip coating. The precursor films, deposited on Si(111) substrates, were heat-treated from 400°C to 900°C in order to study the heat treatment influence on the crystallinity and microstructure of the final film. The X-ray diffraction patterns showed, in particular, that these films crystallize at low temperature (450°C) and present no preferential orientation. The scanning electron microscopy studies showed that the film microstructure is strongly influenced by the annealing temperature. © 1997 Trans Tech Publications.

Electrical properties of the SnO2-based varistor

The non-linear electrical properties of CoO-doped and Nb205-doped SnO2 ceramics were characterized. X-ray diffraction and scanning electron microscopy indicated that the system is single phase. The electrical conduction mechanism for low applied electrical field was associated with thermionic emission of the Schottky type. An atomic defect model based on the Schottky double-barrier formation was proposed to explain the origin of the potential barrier at the ceramic grain boundaries. These defects create depletion layers at grain boundaries, favouring electron tunnelling at high values of applied electrical field. © 1998 Chapman & Hall.

The influence of crystallization route on the SrBi2Nb2O9 thin films

Polycrystalline SrBi2Nb2O9-layered ferroelectric thin films were synthesized on Pt/Ti/SiO2/Si substrate using the polymeric precursors solution. The dip-coated films were specular and crack-free and crystallized during firing at 700 °C. Single-, double-, and triple-layered films were obtained by several dips in the deposition solution, and the influence of crystallization between each dip was studied. Microstructure and morphological evaluation were followed by grazing incident x-ray diffraction (GIXRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Multilayered films obtained using the intermediate-crystallized layer route present a dense microstructure with spherical grains, with a preferential orientation in the 〈215〉 direction; films obtained using the intermediate-amorphous layer route are polycrystalline and present elongated grains around 250 nm in size.

Influence of heat treatment on LiNbO3 thin films prepared on Si(111) by the polymeric precursor method

The effects of heat-treatment temperature on LiNbO3 thin films prepared by the polymeric precursor method were investigated. The precursor solution was deposited on Si(111) substrates by dip coating. X-ray diffraction and thermal analyses revealed that the crystallization process occurred at a low temperature (420 °C) and led to films with no preferential orientation. High-temperature treatments promoted formation of the LiNb3O8 phase. Scanning electron microscopy, coupled with energy dispersive spectroscopy analyses, showed that the treatment temperature also affected the film microstructure. The surface texture - homogeneous, smooth, and pore-free at low temperature - turned into an `islandlike' microstructure for high-temperature treatments.

Preparation and characterization of BaBi2Nb2O9(BBN) ceramics synthetized by polymeric precursors method

Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.

Effect of thermal treatment on the morphology of PLZT thin films prepared from polymeric precursor method

Lead lanthanum zirconate titanate (PLZT) thin films with (9/65/35) stoichiometry were prepared by dip coating from polymeric precursor method. The films deposited on silicon (100) substrates, were thermally treated from 450° to 700°C for 6 hours in order to study the influence of thermal treatment on the crystallinity, microstructure, grain size and roughness of the final film. X-ray diffraction results showed that PLZT phase crystallizes at low temperature (500°C) and present preferential orientation. It was observed by scanning electron microscopy (SEM) that it is possible to obtain dense thin films at temperatures around 650°C. The atomic force microscopy (AFM) studies showed that the grain size and roughness are strongly influenced by the annealing temperature.

The influence of the sintering system on PMN properties

PMN powder samples with PbO excess of 0, 1,2 and 3% were submitted to the pressing and sintering at 1200°C for 4h with a heating rate of 3°C/min. A new sintering system, developed at our laboratories, was used. It allows obtaining more information on the sintering process. The sintered samples in the new system were compared to sintered samples in the C system. The microstructure, dielectric properties and the effect of the PbO excess in different sintering systems were compared. The N system permitted to obtain a ceramic with better properties, such density, dielectric constant and very homogeneous microstructure.

Structural characterization of Li-MN doped powders prepared by Pechini's method

Pechini's method has been successfully used to prepare Li-doped MgNb2O6(MN) at short time and low temperature. It consists in the preparation of metal citrate solution, which is polymerized at 250°C to form a high viscous resin. This resin was burned in a box type furnace at 400°C/2h and ground in a mortar. Successive steps of calcination up to 900°C were used to form a crystalline precursor. SEM, DTA and XRD were used to characterize the powders. MN precursor powders containing from 0.1 to 5.0 mol% of LiNbO3 additive was prepared aiming better dielectric properties and microstructural characteristics of the PMN prepared from columbite route. SEM analysis showed that particles increased by sintering, forming large agglomerates. The surface area is also substantially reduced with the increase in additive amount above 1.0 mol%. In XRD pattern of the precursor material with 5.0 mol% of additive was observed the LiNbO3 phase of trigonal structure. XRD data were used for Rietveld refinement and a decrease in microstrain and pronounced increase in crystallite size with the increase of LiNbO3 were observed. It is in agreement with the particle morphologies observed by SEM analysis.

Elevated CO2 levels do not affect the shell structure of the bivalve Arctica islandica from the western Baltic

Shells of the bivalve Arctica islandica are used to reconstruct paleo-environmental conditions (e.g. temperature) via biogeochemical proxies, i.e. biogenic components that are related closely to environmental parameters at the time of shell formation. Several studies have shown that proxies like element and isotope-ratios can be affected by shell growth and microstructure. Thus it is essential to evaluate the impact of changing environmental parameters such as high pCO2 and consequent changes in carbonate chemistry on shell properties to validate these biogeochemical proxies for a wider range of environmental conditions. Growth experiments with Arctica islandica from the Western Baltic Sea kept under different pCO2 levels (from 380 to 1120 µatm) indicate no affect of elevated pCO2 on shell growth or crystal microstructure, indicating that A. islandica shows an adaptation to a wider range of pCO2 levels than reported for other species. Accordingly, proxy information derived from A. islandica shells of this region contains no pCO2 related bias.

The relationships between microstructure and crystal structure in zincite solid solutions

Single phase (Zn,Fe)(1-x) O zincite solid solution samples have been prepared by high temperature equilibration in air and in reducing atmospheres, followed by quenching to room temperature. The Fe2+/Fe3+ concentrations in the samples have been determined using wet chemical and XPS techniques. Iron is found to be present in zincite predominantly in the form of Fe3+ ions. The transition from an equiaxed grain morphology to plate-like zincite crystals is shown to be associated with increasing Fe3+ concentration, increasing elongation in < 001 > of the hexagonal crystals and increasing anisotropic strain along the c-axis. The plate-like crystals are shown to contain planar defects and zincite polytypes at high iron concentrations.

EBSD characterization of an ECAP deformed Nb single crystal

A niobium single crystal was subjected to equal channel angular pressing (ECAP) at room temperature after orienting the crystal such that [1 -1 -1] ayen ND, [0 1 -1] ayen ED, and [-2 -1 -1] ayen TD. Electron backscatter diffraction (EBSD) was used to characterize the microstructures both on the transverse and the longitudinal sections of the deformed sample. After one pass of ECAP the single crystal exhibits a group of homogeneously distributed large misorientation sheets and a well formed cell structure in the matrix. The traces of the large misorientation sheets match very well with the most favorably oriented slip plane and one of the slip directions is macroscopically aligned with the simple shear plane. The lattice rotation during deformation was quantitatively estimated through comparison of the orientations parallel to three macroscopic axes before and after deformation. An effort has been made to link the microstructure with the initial crystal orientation. Collinear slip systems are believed to be activated during deformation. The full constraints Taylor model was used to simulate the orientation evolution during ECAP. The result matched only partially with the experimental observation.

Influence of chemical interesterification on thermal behavior, microstructure, polymorphism and crystallization properties of canola oil and fully hydrogenated cottonseed oil blends

This work evaluated chemical interesterification of canola oil (CaO) and fully hydrogenated cottonseed oil (FHCSO) blends, with 20%, 25%, 30%, 35% and 40%(w/w) FHCSO content. Interesterification produced reduction of trisaturated and increase in monounsaturated and diunsaturated triacylglycerols contents, which caused important changes in temperatures and enthalpies associated with the crystallization and melting thermograms. It was verified reduction in medium crystal diameter in all blends, in addition crystal morphology modification. Crystallization kinetics revealed that crystal formation induction period and maximum solid fat content were altered according to FHCSO content in original blends and as a result of random rearrangement. Changes in Avrami constant (k) and exponent (n) indicated, respectively, that interesterification decreased crystallization rates and altered crystalline morphology. However, X-ray diffraction analyses showed randomization did not change the original crystalline polymorphism. The original and interesterified blends had significant predominance of beta` polymorph, which is interesting for several food applications. (C) 2009 Elsevier Ltd. All rights reserved.