Microstructural, structural and dielectric properties of Er(3+)-modified BaTi(0.85)Zr(0.15)O(3) ceramics

The (micro)structural and electrical properties of undoped and Er(3+)-doped BaTi(0.85)Zr(0.15)O(3) ceramics were studied in this work for both nominal Ba(2+) and Ti(4+) substitution formulations. The ceramics were produced from solid-state reaction and sintered at 1400 degrees C for 3 h. For those materials prepared following the donor-type nominal Ba(1-x)Er(x)(Ti(0.85)Zr(0.15))O(3) composition, especially, Er(3+) however showed a preferential substitution for the (Ti,Zr)(4+) lattice sites. This allowed synthesis of a finally acceptor-like, highly resistive Ba(Ti,Zr,Er)O(3-delta)-like system, with a solubility limit below but close to 3 cat.% Er(3+). The overall phase development is discussed in terms of the amphoteric nature of Er(3+), and appears to mainly or, at least, partially also involve a minimization of stress effects from the ion size mismatch between the dopant and host cations. Further results presented here include a comparative analysis of the behavior of the materials` grain size, electrical properties and nature of the ferroelectric-to-paraelectric phase transition upon variation of the formulation and Er(3+) content. (C) 2008 Elsevier Ltd. All rights reserved.

Microstructural, structural and electrical properties of La(3+)-modified Bi(4)Ti(3)O(12) ferroelectric ceramics

Bi(4-x)La(x)Ti(3)O(12) (BLT) ceramics were prepared and studied in this work in terms of La(3+)-modified microstructure and phase development as well as electrical response. According to the results processed from X-ray diffraction and electrical measurements, the solubility limit (XL) of La(3+) into the Bi(4)Ti(3)O(12) (BIT) matrix was here found to locate slightly above x = 1.5. Further, La(3+) had the effect of reducing the material grain size, while changing its morphology from the plate-like form, typical of BIT ceramics, to a spherical-like one. The electrical results presented and discussed here also include the behavior of the temperature of the ferroelectric-paraelectric phase transition as well as the normal or diffuse and/or relaxor nature of this transition depending on the La(3+) content. (c) 2008 Elsevier Ltd. All fights reserved.

The influence of twinning on the hot working flow stress and microstructural evolution of magnesium alloy AZ31

The microstructural evolution during compression (at 350°C and a strain rate of 0.01s-1) was examined for magnesium alloy AZ31 received in the "as-cast" condition. It was revealed that at low strains, many twins are produced and dynamically recrystallized (DRX) grains form as a necklace along pre-existing grain boundaries. At higher strains, DRX stagnates, most likely due to the accommodation of deformation in the DRX fraction of the material. It was also observed that twin boundaries act as sites for the nucleation of DRX grains. The analysis was repeated for samples pre-compressed to a strain of 0.15 at room temperature prior to the hot deformation step. The idea of these additional tests was to increase the degree of twinning and therefore the density of sites for the nucleation of DRX. It was found that statically recrystallized (SRX) grains developed at the twins during heating to the test temperature. When these samples were deformed, the peak flow stress was reduced by approximately 20% and the development of DRX was enhanced. This can be attributed to the accelerated nucleation of DRX in the refined SRX structure.

Plastic flow properties and microstructural evolution in an ultrafine-grained Al-Mg-Si alloy at elevated temperatures

An AA6082 alloy was subjected to eight passes of equal channel angular pressing at 100 °C, resulting in an ultrafine grain size of 0.2 to 0.4 µm. The tensile deformation behavior of the material was studied over the temperature range of 100 °C to 350 °C and strain rate range of 10¯⁴ to 10¯¹ s¯¹. The evolution of microstructure under tensile deformation was investigated by analyzing both the deformation relief on the specimen surface and the dislocation structure. While extensive microshear banding was found at the lower temperatures of 100 °C to 150 °C, deformation at higher temperatures was characterized by cooperative grain boundary sliding and the development of a bimodal microstructure. Dislocation glide was identified as the main deformation mechanism within coarse grains, whereas no dislocation activity was apparent in the ultrafine grains.

The use of Fe-30% Ni and Fe-30% Ni-Nb alloys as model systems for studying the microstructural evolution during the hot deformation of austenite

The development of physically-based models of microstructural evolution during thermomechanical processing of metallic materials requires knowledge of the internal state variable data, such as microstructure, texture, and dislocation substructure characteristics, over a range of processing conditions. This is a particular problem for steels, where transformation of the austenite to a variety of transformation products eradicates the hot deformed microstructure. This article reports on a model Fe-30wt% Ni-based alloy, which retains a stable austenitic structure at room temperature, and has, therefore, been used to model the development of austenite microstructure during hot deformation of conventional low carbon-manganese steels. It also provides an excellent model alloy system for microalloy additions. Evolution of the microstructure and crystallographic texture was characterized in detail using optical microscopy, X-ray diffraction (XRD), SEM, EBSD, and TEM. The dislocation substructure has been quantified as a function of crystallographic texture component for a variety of deformation conditions for the Fe-30% Ni-based alloy. An extension to this study, as the use of a microalloyed Fe-30% Ni-Nb alloy in which the strain induced precipitation mechanism was studied directly. The work has shown that precipitation can occur at a much finer scale and higher number density than hitherto considered, but that pipe diffusion leads to rapid coarsening. The implications of this for model development are discussed.

Effect of martensite morphology on low cycle fatigue behaviour of dual phase steels: Experimental and microstructural investigation

The low cycle fatigue (LCF) behaviour of a dual phase (DP) steel with different martensite morphologies has been investigated in the present work. DP steels with coarse martensite morphologies show inferior LCF life in comparison with fine martensite morphologies for all martensite volume fractions examined. It is suggested that this is be due to the development of larger local plastic strain concentrations in the ferrite with a coarser microstructure, compared to the finer microstructural morphology. Fatigue cracks were observed to initiate inside ferrite grains, and to preferentially propagate through the softer ferrite phase. The average sub-cell size was finer in samples with higher martensite volume fractions, but the sub-cell size was almost unaffected by the martensite morphology.

Effect of twinning on microstructural evolution during dynamic recrystallisation of hot deformed as-cast austenitic stainless steel

An as-cast austenitic stainless steel was hot deformed at 1173 K, 1223 K, and 1373 K (900 °C, 950 °C, and 1100 °C) to a strain of 1 with a strain rate of 0.5 or 5 s⁻¹. The recrystallised fraction is observed to be dependent on dynamic recrystallisation (DRX). DRX grains nucleated at the initial stages of recrystallization have similar orientation to that of the deformed grains. With increasing deformation, Cube texture dominates, mainly due to multiple twinning and grain rotation during deformation.

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.

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 SnO(2)center dot Co(3)O(4)center dot 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 phase T2Sn2O7 were observed with SEM in samples with 0.05, 0.10 and 0.25 mol% of Y2O3. The higher non-linearity (a = 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. (c) 2005 Published by Elsevier B.V.

From tin oxalate to (Fe, Co, Nb)-doped SnO(2): Sintering behavior, microstructural and electrical features

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Microstructural and Nonohmic Properties of ZnO center dot Pr6O11 CoO Polycrystalline System

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and characterization of non-oxide ceramic composites for mechanical and tribological applications

The main reasons for the attention focused on ceramics as possible structural materials are their wear resistance and the ability to operate with limited oxidation and ablation at temperatures above 2000°C. Hence, this work is devoted to the study of two classes of materials which can satisfy these requirements: silicon carbide -based ceramics (SiC) for wear applications and borides and carbides of transition metals for ultra-high temperatures applications (UHTCs). SiC-based materials: Silicon carbide is a hard ceramic, which finds applications in many industrial sectors, from heat production, to automotive engineering and metals processing. In view of new fields of uses, SiC-based ceramics were produced with addition of 10-30 vol% of MoSi2, in order to obtain electro conductive ceramics. MoSi2, indeed, is an intermetallic compound which possesses high temperature oxidation resistance, high electrical conductivity (21·10-6 Ω·cm), relatively low density (6.31 g/cm3), high melting point (2030°C) and high stiffness (440 GPa). The SiC-based ceramics were hot pressed at 1900°C with addition of Al2O3-Y2O3 or Y2O3-AlN as sintering additives. The microstructure of the composites and of the reference materials, SiC and MoSi2, were studied by means of conventional analytical techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (SEM-EDS). The composites showed a homogeneous microstructure, with good dispersion of the secondary phases and low residual porosity. The following thermo-mechanical properties of the SiC-based materials were measured: Vickers hardness (HV), Young’s modulus (E), fracture toughness (KIc) and room to high temperature flexural strength (σ). The mechanical properties of the composites were compared to those of two monolithic SiC and MoSi2 materials and resulted in a higher stiffness, fracture toughness and slightly higher flexural resistance. Tribological tests were also performed in two configurations disco-on-pin and slideron cylinder, aiming at studying the wear behaviour of SiC-MoSi2 composites with Al2O3 as counterfacing materials. The tests pointed out that the addition of MoSi2 was detrimental owing to a lower hardness in comparison with the pure SiC matrix. On the contrary, electrical measurements revealed that the addition of 30 vol% of MoSi2, rendered the composite electroconductive, lowering the electrical resistance of three orders of magnitude. Ultra High Temperature Ceramics: Carbides, borides and nitrides of transition metals (Ti, Zr, Hf, Ta, Nb, Mo) possess very high melting points and interesting engineering properties, such as high hardness (20-25 GPa), high stiffness (400-500 GPa), flexural strengths which remain unaltered from room temperature to 1500°C and excellent corrosion resistance in aggressive environment. All these properties place the UHTCs as potential candidates for the development of manoeuvrable hypersonic flight vehicles with sharp leading edges. To this scope Zr- and Hf- carbide and boride materials were produced with addition of 5-20 vol% of MoSi2. This secondary phase enabled the achievement of full dense composites at temperature lower than 2000°C and without the application of pressure. Besides the conventional microstructure analyses XRD and SEM-EDS, transmission electron microscopy (TEM) was employed to explore the microstructure on a small length scale to disclose the effective densification mechanisms. A thorough literature analysis revealed that neither detailed TEM work nor reports on densification mechanisms are available for this class of materials, which however are essential to optimize the sintering aids utilized and the processing parameters applied. Microstructural analyses, along with thermodynamics and crystallographic considerations, led to disclose of the effective role of MoSi2 during sintering of Zrand Hf- carbides and borides. Among the investigated mechanical properties (HV, E, KIc, σ from room temperature to 1500°C), the high temperature flexural strength was improved due to the protective and sealing effect of a silica-based glassy phase, especially for the borides. Nanoindentation tests were also performed on HfC-MoSi2 composites in order to extract hardness and elastic modulus of the single phases. Finally, arc jet tests on HfC- and HfB2-based composites confirmed the excellent oxidation behaviour of these materials under temperature exceeding 2000°C; no cracking or spallation occurred and the modified layer was only 80-90 μm thick.

Experimental analysis and FE Modeling of Aluminium alloys Microstructural Evolution in Extrusion

Extrusion is a process used to form long products of constant cross section, from simple billets, with a high variety of shapes. Aluminum alloys are the materials most processed in the extrusion industry due to their deformability and the wide field of applications that range from buildings to aerospace and from design to automotive industries. The diverse applications imply different requirements that can be fulfilled by the wide range of alloys and treatments, that is from critical structural application to high quality surface and aesthetical aspect. Whether one or the other is the critical aspect, they both depend directly from microstructure. The extrusion process is moreover marked by high deformations and complex strain gradients making difficult the control of microstructure evolution that is at present not yet fully achieved. Nevertheless the evolution of Finite Element modeling has reached a maturity and can therefore start to be used as a tool for investigation and prediction of microstructure evolution. This thesis will analyze and model the evolution of microstructure throughout the entire extrusion process for 6XXX series aluminum alloys. Core phase of the work was the development of specific tests to investigate the microstructure evolution and validate the model implemented in a commercial FE code. Along with it two essential activities were carried out for a correct calibration of the model beyond the simple research of contour parameters, thus leading to the understanding and control of both code and process. In this direction activities were also conducted on building critical knowhow on the interpretation of microstructure and extrusion phenomena. It is believed, in fact, that the sole analysis of the microstructure evolution regardless of its relevance in the technological aspects of the process would be of little use for the industry as well as ineffective for the interpretation of the results.

The development of stylolites, from small-scale heterogeneities to multi-scale roughness

Stylolites are rough paired surfaces, indicative of localized stress-induced dissolution under a non-hydrostatic state of stress, separated by a clay parting which is believed to be the residuum of the dissolved rock. These structures are the most frequent deformation pattern in monomineralic rocks and thus provide important information about low temperature deformation and mass transfer. The intriguing roughness of stylolites can be used to assess amount of volume loss and paleo-stress directions, and to infer the destabilizing processes during pressure solution. But there is little agreement on how stylolites form and why these localized pressure solution patterns develop their characteristic roughness.rnNatural bedding parallel and vertical stylolites were studied in this work to obtain a quantitative description of the stylolite roughness and understand the governing processes during their formation. Adapting scaling approaches based on fractal principles it is demonstrated that stylolites show two self affine scaling regimes with roughness exponents of 1.1 and 0.5 for small and large length scales separated by a crossover length at the millimeter scale. Analysis of stylolites from various depths proved that this crossover length is a function of the stress field during formation, as analytically predicted. For bedding parallel stylolites the crossover length is a function of the normal stress on the interface, but vertical stylolites show a clear in-plane anisotropy of the crossover length owing to the fact that the in-plane stresses (σ2 and σ3) are dissimilar. Therefore stylolite roughness contains a signature of the stress field during formation.rnTo address the origin of stylolite roughness a combined microstructural (SEM/EBSD) and numerical approach is employed. Microstructural investigations of natural stylolites in limestones reveal that heterogeneities initially present in the host rock (clay particles, quartz grains) are responsible for the formation of the distinctive stylolite roughness. A two-dimensional numerical model, i.e. a discrete linear elastic lattice spring model, is used to investigate the roughness evolving from an initially flat fluid filled interface induced by heterogeneities in the matrix. This model generates rough interfaces with the same scaling properties as natural stylolites. Furthermore two coinciding crossover phenomena in space and in time exist that separate length and timescales for which the roughening is either balanced by surface or elastic energies. The roughness and growth exponents are independent of the size, amount and the dissolution rate of the heterogeneities. This allows to conclude that the location of asperities is determined by a polimict multi-scale quenched noise, while the roughening process is governed by inherent processes i.e. the transition from a surface to an elastic energy dominated regime.rn

Microstructural segmentation of 3D images of alsphalt specimen using Matlab engine

En este proyecto se ha desarrollado un código de MATLAB para el procesamiento de imágenes tomográficas 3D, de muestras de asfalto de carreteras en Polonia. Estas imágenes en 3D han sido tomadas por un equipo de investigación de la Universidad Tecnológica de Lodz (LUT). El objetivo de este proyecto es crear una herramienta que se pueda utilizar para estudiar las diferentes muestras de asfalto 3D y pueda servir para estudiar las pruebas de estrés que experimentan las muestras en el laboratorio. Con el objetivo final de encontrar soluciones a la degradación sufrida en las carreteras de Polonia, debido a diferentes causas, como son las condiciones meteorológicas. La degradación de las carreteras es un tema que se ha investigado desde hace muchos años, debido a la fuerte degradación causada por diferentes factores como son climáticos, la falta de mantenimiento o el tráfico excesivo en algunos casos. Es en Polonia, donde estos tres factores hacen que la composición de muchas carreteras se degrade rápidamente, sobre todo debido a las condiciones meteorológicas sufridas a lo largo del año, con temperaturas que van desde 30° C en verano a -20° C en invierno. Esto hace que la composición de las carreteras sufra mucho y el asfalto se levante, lo que aumenta los costos de mantenimiento y los accidentes de carretera. Este proyecto parte de la base de investigación que se lleva a cabo en la LUT, tratando de mejorar el análisis de las muestras de asfalto, por lo que se realizarán las pruebas de estrés y encontrar soluciones para mejorar el asfalto en las carreteras polacas. Esto disminuiría notablemente el costo de mantenimiento. A pesar de no entrar en aspectos muy técnicos sobre el asfalto y su composición, se ha necesitado realizar un estudio profundo sobre todas sus características, para crear un código capaz de obtener los mejores resultados. Por estas razones, se ha desarrollado en Matlab, los algoritmos que permiten el estudio de los especímenes 3D de asfalto. Se ha utilizado este software, ya que Matlab es una poderosa herramienta matemática que permite operar con matrices para realización de operaciones rápidamente, permitiendo desarrollar un código específico para el tratamiento y procesamiento de imágenes en 3D. Gracias a esta herramienta, estos algoritmos realizan procesos tales como, la segmentación de la imagen 3D, pre y post procesamiento de la imagen, filtrado o todo tipo de análisis microestructural de las muestras de asfalto que se están estudiando. El código presentado para la segmentación de las muestras de asfalto 3D es menos complejo en su diseño y desarrollo, debido a las herramientas de procesamiento de imágenes que incluye Matlab, que facilitan significativamente la tarea de programación, así como el método de segmentación utilizado. Respecto al código, este ha sido diseñado teniendo en cuenta el objetivo de facilitar el trabajo de análisis y estudio de las imágenes en 3D de las muestras de asfalto. Por lo tanto, el principal objetivo es el de crear una herramienta para el estudio de este código, por ello fue desarrollado para que pueda ser integrado en un entorno visual, de manera que sea más fácil y simple su utilización. Ese es el motivo por el cual todos estos algoritmos y funciones, que ha sido desarrolladas, se integrarán en una herramienta visual que se ha desarrollado con el GUIDE de Matlab. Esta herramienta ha sido creada en colaboración con Jorge Vega, y fue desarrollada en su proyecto final de carrera, cuyo título es: Segmentación microestructural de Imágenes en 3D de la muestra de asfalto utilizando Matlab. En esta herramienta se ha utilizado todo las funciones programadas en este proyecto, y tiene el objetivo de desarrollar una herramienta que permita crear un entorno gráfico intuitivo y de fácil uso para el estudio de las muestras de 3D de asfalto. Este proyecto se ha dividido en 4 capítulos, en un primer lugar estará la introducción, donde se presentarán los aspectos más importante que se va a componer el proyecto. En el segundo capítulo se presentarán todos los datos técnicos que se han tenido que estudiar para desarrollar la herramienta, entre los que cabe los tres temas más importantes que se han estudiado en este proyecto: materiales asfálticos, los principios de la tomografías 3D y el procesamiento de imágenes. Esta será la base para el tercer capítulo, que expondrá la metodología utilizada en la elaboración del código, con la explicación del entorno de trabajo utilizado en Matlab y todas las funciones de procesamiento de imágenes utilizadas. Además, se muestra todo el código desarrollado, así como una descripción teórica de los métodos utilizados para el pre-procesamiento y segmentación de las imagenes en 3D. En el capítulo 4, se mostrarán los resultados obtenidos en el estudio de una de las muestras de asfalto, y, finalmente, el último capítulo se basa en las conclusiones sobre el desarrollo de este proyecto. En este proyecto se ha llevado han realizado todos los puntos que se establecieron como punto de partida en el anteproyecto para crear la herramienta, a pesar de que se ha dejado para futuros proyectos nuevas posibilidades de este codigo, como por ejemplo, la detección automática de las diferentes regiones de una muestra de asfalto debido a su composición. Como se muestra en este proyecto, las técnicas de procesamiento de imágenes se utilizan cada vez más en multitud áreas, como pueden ser industriales o médicas. En consecuencia, este tipo de proyecto tiene multitud de posibilidades, y pudiendo ser la base para muchas nuevas aplicaciones que se puedan desarrollar en un futuro. Por último, se concluye que este proyecto ha contribuido a fortalecer las habilidades de programación, ampliando el conocimiento de Matlab y de la teoría de procesamiento de imágenes. Del mismo modo, este trabajo proporciona una base para el desarrollo de un proyecto más amplio cuyo alcance será una herramienta que puedas ser utilizada por el equipo de investigación de la Universidad Tecnológica de Lodz y en futuros proyectos. ABSTRACT In this project has been developed one code in MATLAB to process X-ray tomographic 3D images of asphalt specimens. These images 3D has been taken by a research team of the Lodz University of Technology (LUT). The aim of this project is to create a tool that can be used to study differents asphalt specimen and can be used to study them after stress tests undergoing the samples. With the final goal to find solutions to the degradation suffered roads in Poland due to differents causes, like weather conditions. The degradation of the roads is an issue that has been investigated many years ago, due to strong degradation suffered caused by various factors such as climate, poor maintenance or excessive traffic in some cases. It is in Poland where these three factors make the composition of many roads degrade rapidly, especially due to the weather conditions suffered along the year, with temperatures ranging from 30 o C in summer to -20 ° C in winter. This causes the roads suffers a lot and asphalt rises shortly after putting, increasing maintenance costs and road accident. This project part of the base that research is taking place at the LUT, in order to better analyze the asphalt specimens, they are tested for stress and find solutions to improve the asphalt on Polish roads. This would decrease remarkable maintenance cost. Although this project will not go into the technical aspect as asphalt and composition, but it has been required a deep study about all of its features, to create a code able to obtain the best results. For these reasons, there have been developed in Matlab, algorithms that allow the study of 3D specimens of asphalt. Matlab is a powerful mathematical tool, which allows arrays operate fastly, allowing to develop specific code for the treatment and processing of 3D images. Thus, these algorithms perform processes such as the multidimensional matrix sgementation, pre and post processing with the same filtering algorithms or microstructural analysis of asphalt specimen which being studied. All these algorithms and function that has been developed to be integrated into a visual tool which it be developed with the GUIDE of Matlab. This tool has been created in the project of Jorge Vega which name is: Microstructural segmentation of 3D images of asphalt specimen using Matlab engine. In this tool it has been used all the functions programmed in this project, and it has the aim to develop an easy and intuitive graphical environment for the study of 3D samples of asphalt. This project has been divided into 4 chapters plus the introduction, the second chapter introduces the state-of-the-art of the three of the most important topics that have been studied in this project: asphalt materials, principle of X-ray tomography and image processing. This will be the base for the third chapter, which will outline the methodology used in developing the code, explaining the working environment of Matlab and all the functions of processing images used. In addition, it will be shown all the developed code created, as well as a theoretical description of the methods used for preprocessing and 3D image segmentation. In Chapter 4 is shown the results obtained from the study of one of the specimens of asphalt, and finally the last chapter draws the conclusions regarding the development of this project.