Comparison of fracture surface and plane section analysis for ceramic grain size characterisation

A method has been developed to obtain quantitative information about grain size and shape from fractured surfaces of ceramic materials. One elaborated a routine to split intergranular and transgranular grains facets of ceramic fracture surfaces by digital image processing. A commercial ceramic (ALCOA A-16, Al2O3-1.5% of CrO) was used to test the proposed method. Microstructural measurements of grain shape and size taken from fracture surfaces have been compared through descriptive statistics of distributions, with the corresponding measurements from polished and etched surfaces. The agreement between results, with the expected bias on grain size values from fractures, obtained for both types of surfaces allowed to infer that this new technique can be used to extract the relevant microstructural information from fractured surfaces, thus minimising the time consuming steps of sample preparation. (C) 2003 Elsevier Ltd. All rights reserved.

Improving methods in gap ecology: Revisiting size and shape distributions using a model selection approach

Questions: We assess gap size and shape distributions, two important descriptors of the forest disturbance regime, by asking: which statistical model best describes gap size distribution; can simple geometric forms adequately describe gap shape; does gap size or shape vary with forest type, gap age or the method used for gap delimitation; and how similar are the studied forests and other tropical and temperate forests? Location: Southeastern Atlantic Forest, Brazil. Methods: Analysing over 150 gaps in two distinct forest types (seasonal and rain forests), a model selection framework was used to select appropriate probability distributions and functions to describe gap size and gap shape. The first was described using univariate probability distributions, whereas the latter was assessed based on the gap area-perimeter relationship. Comparisons of gap size and shape between sites, as well as size and age classes were then made based on the likelihood of models having different assumptions for the values of their parameters. Results: The log-normal distribution was the best descriptor of gap size distribution, independently of the forest type or gap delimitation method. Because gaps became more irregular as they increased in size, all geometric forms (triangle, rectangle and ellipse) were poor descriptors of gap shape. Only when small and large gaps (> 100 or 400m2 depending on the delimitation method) were treated separately did the rectangle and isosceles triangle become accurate predictors of gap shape. Ellipsoidal shapes were poor descriptors. At both sites, gaps were at least 50% longer than they were wide, a finding with important implications for gap microclimate (e.g. light entrance regime) and, consequently, for gap regeneration. Conclusions: In addition to more appropriate descriptions of gap size and shape, the model selection framework used here efficiently provided a means by which to compare the patterns of two different types of forest. With this framework we were able to recommend the log-normal parameters μ and σ for future comparisons of gap size distribution, and to propose possible mechanisms related to random rates of gap expansion and closure. We also showed that gap shape varied highly and that no single geometric form was able to predict the shape of all gaps, the ellipse in particular should no longer be used as a standard gap shape. © 2012 International Association for Vegetation Science.

Honey Ants (Genus Myrmecocystus) Macroecology: Effect of Spatial Patterns on the Relationship between Worker Body Size and Geographic Range Size

Macroecology evaluates the partitioning of physical space and resources among organisms through correlation among ecological variables, such as geographical range size and shape, body size, and population density, measured at large geographical and taxonomic scales. In this article, we analyzed the spatial patterns in worker body size and geographic range size for the 27 described species of honey ants, genus Myrmecocystus Wesmael, in the United States and Mexico, and especially the relationship between these 2 variables after statistically removing their spatial patterns. The 2 variables are correlated, but also displayed significant spatial patterns, as detected by trend surface and spatial autocorrelation analyses. After removing these spatial effects, worker body size and geographic range size were still positively correlated. The relationship, therefore, is not a consequence of spatial effects and it does follow Brown's model, which predicts that the geographic range size will have a positive slope on body size. In this model, the lower population densities caused by foraging activities and local territorial competition are associated with a large geographic range, avoiding stochastic extinction. Although this constraint in local population density does not necessarily hold for small organisms such as insects that could achieve high densities even in very small areas and patchy habitats, it may hold for social insects, especially ants, because of the local competition among colonies.

A method for the digital image analysis of ceramic grains based on shape factor segmentation

A very simple and robust method for ceramics grains quantitative image analysis is presented. Based on the use of optimal imaging conditions for reflective light microscopy of bulk samples, a digital image processing routine was developed for shading correction, noise suppressing and contours enhancement. Image analysis was done for grains selected according to their concavities, evaluated by perimeter ratio shape factor, to avoid consider the effects of breakouts and ghost boundaries due to ceramographic preparation limitations. As an example, the method was applied for two ceramics, to compare grain size and morphology distributions. In this case, most of artefacts introduced by ceramographic preparation could be discarded due to the use of perimeter ratio exclusion range.

The synergistic effects of Nb/Mn and Sb/Mn on the microstructure and electrical characteristics of BaTiO3 based ceramics

The microstructure and dielectric properties of Nb-Mn or Sb-Mn codoped BaTiO3 compositions were investigated. Starting ceramics powders were prepared by Pechini method. The composites were sintered at 1310°C and 1330°C in an air atmosphere for two hours. The microstructure and compositional investigations were done with SEM equipped with EDS. Two distinguish microstructure regions are observed in Nb/0.05Mn doped BaTiO 3 ceramics sintered at low temperature. The first, large one, with grain sizes from 5-40 μm and the second region with small grain sizes from 1 to 5 μm. Sintering at higher temperature, independent of Mn content, enables to achieve a uniform microstructure with grains less than 6 μm. In Sb/Mn doped ceramics, for both sintering temperatures, bimodal microstructures with fine grained matrix and grains up to 10 μm is formed. The highest value of permittivity at room temperature and the greatest change of permittivity in function of temperature are observed in Nb/0.01Mn doped ceramics compared to the same ones in Sb/Mn doped ceramics. The greatest shift of Curie temperature towards lower temperature has been noticed in Sb/Mn BaTiO3 ceramics compared to others samples. In all investigated samples the dielectric loss after initially large values at low frequency maintains a constant value for f>3 kHz.

Optical and transport properties of rare-earth trivalent ions located at different sites in sol-gel SnO2

Photoluminescence and photo-excited conductivity data as well as structural analysis are presented for sol-gel SnO2 thin films doped with rare earth ions Eu3+ and Er3+, deposited by sol-gel-dip-coating technique. Photoluminescence spectra are obtained under excitation with various types of monochromatic light sources, such as Kr+, Ar+ and Nd:YAG lasers, besides a Xe lamp plus a selective monochromator with UV grating. The luminescence fine structure is rather different depending on the location of the rare-earth doping, at lattice symmetric sites or segregated at the asymmetric grain boundary layer sites. The decay of photo-excited conductivity also shows different trapping rate depending on the rare-earth concentration. For Er-doped films, above the saturation limit, the evaluated capture energy is higher than for films with concentration below the limit, in good agreement with the different behaviour obtained from luminescence data. For Eu-doped films, the difference in the capture energy is not so evident in these materials with nanoscocopic crystallites, even though the luminescence spectra are rather distinct. It seems that grain boundary scattering plays a major role in Eu-doped SnO2 films. Structural evaluation helps to interpret the electro-optical data. © 2010 IOP Publishing Ltd.

Influence of current density on crystalline structure and magnetic properties of electrodeposited Co-rich CoNiW alloys

The influence of current density, at the interval 5-100 mA cm-2, on the structural and magnetic properties of electrodeposited (Co 100-xNix)100-yWy alloys (x = 23-33.5 at. % Ni, y = 1.7-7.3 at. % W) was studied from a glycine-containing bath. W-content decreases with the increase of the current density magnitude. X-ray data have shown stabilization of hexagonal close packed, face centered cubic or a mixture of these structures by modulating the applied cathodic current density, for values lower than 50 mA cm-2. Two structural phase transitions were observed: one from hexagonal close packed to face centered cubic structural transition occurring for a current density of 20 mA cm -2, and another one, from cubic crystalline phase to amorphous state, which happens for values higher than 50 mA cm-2. These structural phase transitions seem to be associated with the W-content as well as average crystalline grain sizes that reduce with increasing the current density value. The grain size effect may explain the face centered cubic stabilization in Co-rich CoNiW alloys, which was initially assumed to be basically due to H-adsorption/incorporation. Magnetic properties of Co-rich CoNiW alloys are strongly modified by the current density value; as a result of the changes on the W-content and their structural properties© 2013 Elsevier B.V. All rights reserved.

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.

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.

Otimização das propriedades mecânicas por meio de modificações microestruturais em aços de baixo carbono

This paper discusses the formation of microstructures with different volume fractions, as an outcome of a specific heat treatment, with the following phases: ferrite, martensite, bainite and retained austenite. For the microstructure characterization it is developed a chemical etching that allows to distinguish the phases by optical microscopy. The evaluation of the mechanical properties is done based on the results of tensile and fatigue tests. The experimental results show that appropriate heat treatments can contribute to a significant improvement in the mechanical properties of the steel. In this process it is essential to control the fraction volume, morphology of the phases, and grain size.

Preparation of lanthanum doped Bi4Ti3O12 ceramics by the polymeric precursor method

Lanthanum-modified bismuth titanate, Bi4 - xLaxTi3O12 (BLT) ceramics, with x ranging from 0 to 0.75 were prepared by the polymeric precursor method. Orthorhombicity of the system is decreased with the increase of lanthanum content in the bismuth titanate (BIT) crystal lattice. No secondary phases were evident after lanthanum addition. Increasing lanthanum content causes a structural distortion in the bismuth titanate lattice. The shape of the grains is strongly influenced by the lanthanum added to the system. © 2005 Elsevier B.V. All rights reserved.

Grãos ultrafinos por laminação a morno e recozimento intercrítico

Grain refinement of low carbon steel via the warm deformation of martensite during torsion testing was investigated. At the beginning of straining, laths with high dislocation density were observed. After large deformations, a ferrite matrix with grain size close to 1μm and dispersed cementite particles were attained.

Methanol oxidation on PtRu/C electrocatalysts prepared by a microemulsion method

PtRu/C nanocatalysts were prepared by a microemulsion method using different values of water/surfactant molar ratio in order to get different particle sizes. Crystallite sizes and structural properties were determined by X-ray diffraction. Particle size and distribution were characterized by transmission electron microscopy and average composition was determined by energy dispersive X-ray analysis. Differential scanning calorimetry measurements indicated the presence of oxides in the as-prepared catalysts. The general electrochemical behavior was evaluated by cyclic voltammetry in 0.5 M sulfuric acid and the electrocatalytic activity towards the oxidation of methanol was studied in 0.5 M methanol acid solutions by potential sweeps and chronoamperometry. copyright The Electrochemical Society.