935 resultados para Microstructure evolution
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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.
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The aim of this work is to characterize a metallic slurry (Al-4.5%Cu) flow during thixoforming of an automotive valve. The necessary globular structure was obtained by first inoculating the alloy with TIBAL (5%Ti, 1%B, Al - rest) at 750.0°C, and then reheating to a state between liquidus and solidus prior to thixoforming. Two metallic slurries, with a solid phase of approximately 86.1 and 78.2 percent, were used to generate different experimental flow patterns during the thixoforming process. The flow of the material into the die was observed for total, and partial displacement (2.7, 5.4, 7.5mm) of the punch. The first displacement shows formation of the valve rod. The patterns at each step of displacement of the punch were preserved by quenching in water, thus revealing the profile of the die fill and microstructural evolution. Degeneration of the globular phase was observed along the piece thixoextruded. Thixoextrusion forces versus time curves were generated for partial and full displacement of the punch. Porosity was visible along the billet prior to thixoforming. However, some areas show that the porosity gradually decreased to zero as the thixoextrusion pressure increased. Turbulent, transient and laminar flow are analyzed in this work.
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In order to reduce the cost of Al-Sc alloys and maintain their mechanical properties, the microstructure and mechanical properties of Al-0.24 wt% Sc-0.07 wt% Yb in comparison with Al-0.28 wt% Sc alloys were studied. The aging behaviour, precipitate morphologies, precipitate coarsening and precipitation hardening of both alloys were investigated. The average diameter and the size distribution of nanoscale Al3Sc and Al-3(Sc,Yb) precipitates at various aging conditions were measured. Transmission electron microscopy (TEM) and high-resolution TEM were used to deeply understand the precipitate evolution. A maximum hardness around 73 (HV30) was obtained with a precipitate diameter from 4.3 to 5.6 nm for both alloys. (c) 2014 Elsevier B.V. All rights reserved.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Fatigue life in metals is predicted utilizing regression analysis of large sets of experimental data, thus representing the material’s macroscopic response. Furthermore, a high variability in the short crack growth (SCG) rate has been observed in polycrystalline materials, in which the evolution and distributionof local plasticity is strongly influenced by the microstructure features. The present work serves to (a) identify the relationship between the crack driving force based on the local microstructure in the proximity of the crack-tip and (b) defines the correlation between scatter observed in the SCG rates to variability in the microstructure. A crystal plasticity model based on the fast Fourier transform formulation of the elasto-viscoplastic problem (CP-EVP-FFT) is used, since the ability to account for the both elastic and plastic regime is critical in fatigue. Fatigue is governed by slip irreversibility, resulting in crack growth, which starts to occur during local elasto-plastic transition. To investigate the effects of microstructure variability on the SCG rate, sets of different microstructure realizations are constructed, in which cracks of different length are introduced to mimic quasi-static SCG in engineering alloys. From these results, the behavior of the characteristic variables of different length scale are analyzed: (i) Von Mises stress fields (ii) resolved shear stress/strain in the pertinent slip systems, and (iii) slip accumulation/irreversibilities. Through fatigue indicator parameters (FIP), scatter within the SCG rates is related to variability in the microstructural features; the results demonstrate that this relationship between microstructure variability and uncertainty in fatigue behavior is critical for accurate fatigue life prediction.
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The Variscan basement of Northern Apennines (Northern Italy) is a polymetamorphic portion of continental crust. This thesis investigated the metamorphic history of this basement occurring in the Cerreto Pass, in the Pontremoli well, and in the Pisani Mountains. The study comprised fieldwork, petrography and microstructural analysis, determination of the bulk rock and mineral composition, thermodynamic modelling, conventional geothermobarometry, monazite chemical dating and Ar/Ar dating of muscovite. The reconstructed metamorphic evolution of the selected samples allowed to define a long-lasting metamorphic history straddling the Variscan and Alpine orogenesis. Some general petrological issues generally found in low- to medium-grade metapelites were also tackled: (i) With middle-grade micaschist it is possible to reconstruct a complete P-T-D path by combining microstructural analysis and thermodynamic modelling. Prekinematic white mica may preserve Mg-rich cores related to the pre-peak stage. Mn-poor garnet rim records the peak metamorphism. Na-rich mylonitic white mica, the XFe of chlorite and the late paragenesis may constrain the retrograde stage. (ii) Metapelites may contain coronitic microstructures of apatite + Th-silicate, allanite and epidote around unstable monazite grains. Chemistry and microstructure of Th-rich monazite relics surrounded by this coronitic microstructure may suggest that monazite mineral was inherited and underwent partial dissolution and fluid-aided replacement by REE-accessory minerals at 500-600°C and 5-7 kbar. (iii) Fish-shaped white mica is not always a (prekinematic) mica-fish. Observed at high-magnification BSE images it may consist of several white mica formed during a mylonitic stage. Hence, the asymmetric foliation boudin is a suitable microstructure to obtain geochronological information about the shearing stage. (iv) Thermodynamic modelling of a hematite-rich metasedimentary rock fails to reproduce the observed mineral compositions when the bulk Fe2O3 is neglected or determined through titration. The mismatch between observed and computed mineral compositions and assemblage is resolved by tuning the effective ferric iron content by P-XFe2O3 diagrams.
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Digital light, fluorescence and electron microscopy in combination with wavelength-dispersive spectroscopy were used to visualize individual polymers, air voids, cement phases and filler minerals in a polymer-modified cementitious tile adhesive. In order to investigate the evolution and processes involved in formation of the mortar microstructure, quantifications of the phase distribution in the mortar were performed including phase-specific imaging and digital image analysis. The required sample preparation techniques and imaging related topics are discussed. As a form of case study, the different techniques were applied to obtain a quantitative characterization of a specific mortar mixture. The results indicate that the mortar fractionates during different stages ranging from the early fresh mortar until the final hardened mortar stage. This induces process-dependent enrichments of the phases at specific locations in the mortar. The approach presented provides important information for a comprehensive understanding of the functionality of polymer-modified mortars.
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The impact of polymer modification on the physical properties of cementitious mortars is investigated using a multimethod approach. Special emphasis is put on the identification and quantification of different polymer components within the cementitious matrix. With respect to thin-bed applications, particularly tile adhesives, the spatial distributions of latex, cellulose ether (CE), polyvinyl alcohol (PVA), and cement hydration products can be quantified. It is shown that capillary forces and evaporation induce water fluxes in the interconnected part of the pore system, which transport CE, PVA, and cement ions to the mortar interfaces. In contrast, the distribution of latex remains homogeneous. In combination with results from qualitative experiments, the quantitative findings allow reconstruction of the evolution from fresh to hardened mortar, including polymer film formation, cement hydration, and water migration. The resulting microstructure and the failure modes can be correlated with the final adhesive strength of the tile adhesive. The results demonstrate that skinning prior to tile inlaying can strongly reduce wetting properties of the fresh mortar and lower final adhesive strength.
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Plane strain simple shearing of norcamphor (C7H10O) in a see-through deformation rig to a shear strain of γ = 10.5 at a homologous temperature of Th = 0.81 yields a microfabric similar to that of quartz in amphibolite facies mylonite. Synkinematic analysis of the norcamphor microfabric reveals that the development of a steady-state texture is linked to changes in the relative activities of several grain-scale mechanisms. Three stages of textural and microstructural evolution are distinguished: (1) rotation and shearing of the intracrystalline glide planes are accommodated by localized deformation along three sets of anastomozing microshears. A symmetrical c-axis girdle reflects localized pure shear extension along the main microshear set (Sa) oblique to the bulk shear zone boundary (abbreviated as SZB); (2) progressive rotation of the microshears into parallelism with the SZB increases the component of simple shear on the Sa microshears. Grain-boundary migration recrystallization favours the survival of grains with slip systems oriented for easy glide. This is associated with a textural transition towards two stable c-axis point maxima whose skeletal outline is oblique with respect to the Sa microshears and the SZB; and (3) at high shear strains (γ > 8), the microstructure, texture and mechanism assemblage are strain invariant, but strain continues to partition into rotating sets of microshears. Steady state is therefore a dynamic, heterogeneous condition involving the cyclic nucleation, growth and consumption of grains.
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In this work, the microstructure of mortars made with an ordinary Portland cement and slag cement has been studied. These mortars were exposed to four different constant temperature and relative humidity environments during a 180-day period. The microstructure has been studied using impedance spectroscopy, and mercury intrusion porosimetry as a contrast technique. The impedance spectroscopy parameters make it possible to analyze the evolution of the solid fraction formation for the studied mortars and their results are confirmed with those obtained using mercury intrusion porosimetry. The development of the pore network of mortars is affected by the environment. However, slag cement mortars are more influenced by temperature while the relative humidity has a greater influence on the OPC mortars. The results show that slag cement mortars hardened under non-optimal environments have a more refined microstructure than OPC mortars for the studied environmental conditions.
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Typically, cognitive abilities of humans have been attributed to their greatly expanded cortical mantle, granular prefrontal cortex (gPFC) in particular. Recently we have demonstrated systematic differences in microstructure of gPFC in different species. Specifically, pyramidal cells in adult human gPFC are considerably more spinous than those in the gPFC of the macaque monkey, which are more spinous than those in the gPFC of marmoset and owl monkeys. As most cortical dendritic spines receive at least one excitatory input, pyramidal cells in these different species putatively receive different numbers of inputs. These differences in the gPFC pyramidal cell phenotype may be of fundamental importance in determining the functional characteristics of prefrontal circuitry and hence the cognitive styles of the different species. However, it remains unknown as to why the gPFC pyramidal cell phenotype differs between species. Differences could be attributed to, among other things, brain size, relative size of gPFC, or the lineage to which the species belong. Here we investigated pyramidal cells in the dorsolateral gPFC of the prosimian galago to extend the basis for comparison. We found these cells to be less spinous than those in human, macaque, and marmoset. (c) 2005 Wiley-Liss, Inc.
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The focus of this work is to develop and employ numerical methods that provide characterization of granular microstructures, dynamic fragmentation of brittle materials, and dynamic fracture of three-dimensional bodies.
We first propose the fabric tensor formalism to describe the structure and evolution of lithium-ion electrode microstructure during the calendaring process. Fabric tensors are directional measures of particulate assemblies based on inter-particle connectivity, relating to the structural and transport properties of the electrode. Applying this technique to X-ray computed tomography of cathode microstructure, we show that fabric tensors capture the evolution of the inter-particle contact distribution and are therefore good measures for the internal state of and electronic transport within the electrode.
We then shift focus to the development and analysis of fracture models within finite element simulations. A difficult problem to characterize in the realm of fracture modeling is that of fragmentation, wherein brittle materials subjected to a uniform tensile loading break apart into a large number of smaller pieces. We explore the effect of numerical precision in the results of dynamic fragmentation simulations using the cohesive element approach on a one-dimensional domain. By introducing random and non-random field variations, we discern that round-off error plays a significant role in establishing a mesh-convergent solution for uniform fragmentation problems. Further, by using differing magnitudes of randomized material properties and mesh discretizations, we find that employing randomness can improve convergence behavior and provide a computational savings.
The Thick Level-Set model is implemented to describe brittle media undergoing dynamic fragmentation as an alternative to the cohesive element approach. This non-local damage model features a level-set function that defines the extent and severity of degradation and uses a length scale to limit the damage gradient. In terms of energy dissipated by fracture and mean fragment size, we find that the proposed model reproduces the rate-dependent observations of analytical approaches, cohesive element simulations, and experimental studies.
Lastly, the Thick Level-Set model is implemented in three dimensions to describe the dynamic failure of brittle media, such as the active material particles in the battery cathode during manufacturing. The proposed model matches expected behavior from physical experiments, analytical approaches, and numerical models, and mesh convergence is established. We find that the use of an asymmetrical damage model to represent tensile damage is important to producing the expected results for brittle fracture problems.
The impact of this work is that designers of lithium-ion battery components can employ the numerical methods presented herein to analyze the evolving electrode microstructure during manufacturing, operational, and extraordinary loadings. This allows for enhanced designs and manufacturing methods that advance the state of battery technology. Further, these numerical tools have applicability in a broad range of fields, from geotechnical analysis to ice-sheet modeling to armor design to hydraulic fracturing.
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Calcitic belemnite rostra are usually employed to perform paleoenvironmental studies based on geochemical data. However, several questions, such as their original porosity and microstructure, remain open, despite they are essential to make accurate interpretations based on geochemical analyses.This paper revisits and enlightens some of these questions. Petrographic data demonstrate that calcite crystals of the rostrum solidum of belemnites grow from spherulites that successively develop along the apical line, resulting in a “regular spherulithic prismatic” microstructure. Radially arranged calcite crystals emerge and diverge from the spherulites: towards the apex, crystals grow until a new spherulite is formed; towards the external walls of the rostrum, the crystals become progressively bigger and prismatic. Adjacent crystals slightly vary in their c-axis orientation, resulting in undulose extinction. Concentric growth layering develops at different scales and is superimposed and traversed by a radial pattern, which results in the micro-fibrous texture that is observed in the calcite crystals in the rostra.Petrographic data demonstrate that single calcite crystals in the rostra have a composite nature, which strongly suggests that the belemnite rostra were originally porous. Single crystals consistently comprise two distinct zones or sectors in optical continuity: 1) the inner zone is fluorescent, has relatively low optical relief under transmitted light (TL) microscopy, a dark-grey color under backscatter electron microscopy (BSEM), a commonly triangular shape, a “patchy” appearance and relatively high Mg and Na contents; 2) the outer sector is non-fluorescent, has relatively high optical relief under TL, a light-grey color under BSEM and low Mg and Na contents. The inner and fluorescent sectors are interpreted to have formed first as a product of biologically controlled mineralization during belemnite skeletal growth and the non-fluorescent outer sectors as overgrowths of the former, filling the intra- and inter-crystalline porosity. This question has important implications for making paleoenvironmental and/or paleoclimatic interpretations based on geochemical analyses of belemnite rostra.Finally, the petrographic features of composite calcite crystals in the rostra also suggest the non-classical crystallization of belemnite rostra, as previously suggested by other authors.
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This study aimed at evaluating whether human papillomavirus (HPV) groups and E6/E7 mRNA of HPV 16, 18, 31, 33, and 45 are prognostic of cervical intraepithelial neoplasia (CIN) 2 outcome in women with a cervical smear showing a low-grade squamous intraepithelial lesion (LSIL). This cohort study included women with biopsy-confirmed CIN 2 who were followed up for 12 months, with cervical smear and colposcopy performed every three months. Women with a negative or low-risk HPV status showed 100% CIN 2 regression. The CIN 2 regression rates at the 12-month follow-up were 69.4% for women with alpha-9 HPV versus 91.7% for other HPV species or HPV-negative status (P < 0.05). For women with HPV 16, the CIN 2 regression rate at the 12-month follow-up was 61.4% versus 89.5% for other HPV types or HPV-negative status (P < 0.05). The CIN 2 regression rate was 68.3% for women who tested positive for HPV E6/E7 mRNA versus 82.0% for the negative results, but this difference was not statistically significant. The expectant management for women with biopsy-confirmed CIN 2 and previous cytological tests showing LSIL exhibited a very high rate of spontaneous regression. HPV 16 is associated with a higher CIN 2 progression rate than other HPV infections. HPV E6/E7 mRNA is not a prognostic marker of the CIN 2 clinical outcome, although this analysis cannot be considered conclusive. Given the small sample size, this study could be considered a pilot for future larger studies on the role of predictive markers of CIN 2 evolution.