none

Pressureless-sintering of non-stoichiometric barium titanate (BaTiO3) powder of TiO2-excess compositions has been investigated. Crystalline phases were analysed by X-ray diffractometry. Attention has been paid to the analysis of the corresponding sintered microstructure by adopting scanning and transmission electron microscopy. Large plate-like grains grown abnormally containing {111} double twin lamellae are commonly found in low-temperature (1332oC) sintered BaTiO3, by presence of a liquid phase, or by twinning, or as discussed in this experiments by partial dislocations. Samples were sintered in air at 1250oC for 1¡B4 and 50 h. In this respect, the emphasis is discussed about the role of the partial dislocations in the early stage of twin formation. Both analytic dislocations exist on the {111} double twin lamellae within abnormal grain and the interface between abnormal grain and normal grain. In the experimental process, dislocation type with the Burgers vector ‹110› and ‹112› has been found except for the ‹111›. For the Burgers vector ‹110› in the perovskite structure, it is possible to envisage that edge dislocations with [100] Burgers vector can be dissociated in their climb plane ([100] ¡÷ 1/2[101] + 1/2[10 ]). Moreover, the perovskite structure has been deformed form ‹110› dislocation (perfect dislocation). Oppositely, the [112] Burgers vector has been formed both partial dislocation type and perfect dislocation type. For sintering at 50 h, we can conjecture the grain growth mold by Shockley or Frank partial dislocation affect on the macroscopic step. Experimental results show that Shockley and Frank partial dislocations have not been found on the {111} double twin lamellae.

Dynamic abnormal grain growth (DAGG) in commercial-purity molybdenum sheets was investigated through a series of tensile tests at temperatures between 1450°C and 1800°C. DAGG is abnormal grain growth (AGG) which requires the presence of concurrent plastic strain. Most AGG phenomena previously documented in the literature can be categorized as static abnormal grain growth (SAGG) because they occur during static annealing, sometimes following plastic strain, but do not occur during plastic deformation. The DAGG boundary migration rate is much faster than the SAGG boundary migration rate, and DAGG may be utilized to obtain large single crystals in the solid state. Dynamic abnormal grains were found to exhibit a crystallographic orientation preference with respect to the specimen geometry, generally described as derivative from a <101> fiber texture. DAGG was found to prefer growth on the surface of the specimen rather than the interior. The growth of dynamic abnormal grains, which initiated and grew during plastic straining, generally ceased when the application of plastic strain was removed. The DAGG boundary migration rate was found to be a direct function of plastic strain accumulation, regardless of the strain-rate. Therefore, it is hypothesized that the rapid boundary migration rate during DAGG results from an enhanced mobility of certain boundaries. A model is proposed based on the rate of boundary unpinning, as mediated by the emission of dislocations from pinning sites. / text

Dynamic abnormal grain growth (DAGG) is a phenomenon that produces abnormal grain growth at elevated temperatures during plastic deformation. It is distinct from classically studied static abnormal grain growth phenomena in that it only occurs during plastic deformation. Previous investigations of DAGG in a Mo sheet material produced using powder metallurgy techniques observed DAGG grains to grow more rapidly near the sheet surface than near the sheet center. This phenomenon is explored in the present study. A Mo sheet material produced using arc melting techniques is also studied to determine the morphology of DAGG grains. A preference for growth near the sheet center is observed in this material. The through-thickness variations in texture and grain size for both the arc-melted and powder-metallurgy Mo sheet materials are investigated. The preference for growth near the surface in the powder-metallurgy material is due to a through-thickness variation in grain size, with smaller grains near the surface and larger grains near the center. The preference for DAGG grain growth at the center of the arc-melted sheet material is because of very large grains that grow near the sheet surface. These large grains may be the product of multiple abnormal grains occurring near the sheet surface because of texture variation through the sheet thickness. Regardless, the DAGG grain cannot consume these large grains and leaves them as island grains decorating the region near the sheet surface. These results suggest that DAGG is driven primarily by grain boundary curvature. Microstructures that include DAGG grains are investigated with electron backscatter diffraction (EBSD). A new method to evaluate geometrically necessary dislocation densities using EBSD data is derived. DAGG grains are relatively undeformed compared to the polycrystalline microstructure. DAGG grains are not oriented either favorably or unfavorably for slip. Results of the analysis of the grain boundaries between DAGG grains and normal grains do not indicate any special character preference for these grain boundaries. / text

Secondary abnormal grain growth (SAGG) during sintering of barium titanate has been explained in terms of twin plane re-entrant edge (TPRE) growth mechanism by {111} double twin lamellae. But during sintering of Ti-excess barium titanate, {111} double twins lamellae are observed with out SAGG. In our group, Lin founded that when combine two different Ba/Ti ratio of powder to sintering above the eutectic temperature, the SAGG is observed in the interface between two different powders. Therefore, this thesis consists of three major researches: (a) {111} double twin, (b) Ba/Ti ratio, (c) liquid phase. In the experiment, we follow Lin¡¦s experiment to sinter the specimen contain with SAGG. And in this specimen, it can observe the specimen divided into three type of growth grain: (a) top surface with normal grain growth (NGG), (b) intermediate layer with abnormal grain growth (AGG), (c) bottom layer with secondary abnormal grain growth. It can all observed {111} double twin in these three different type of layer. This result confirmed that SAGG are not induced by TPRE growth mechanism. Then we used SEM/EDS to analysis the Ba/Ti ratio in the different type of grain growth layer. The Ba/Ti ratio in this analysis is not differing in NGG, AGG and SAGG. Therefore, we used OM, SEM, TEM to observe the grain boundary and triple grain junction in NGG, AGG and SAGG. It can observe that only the grain boundary and triple grain junction in SAGG are complete wetting. The experimental results shows that the grain growth behavior controlled by the liquid phase wetting degree.

Dynamic abnormal grain growth (DAGG) is a phenomenon by which single crystals up to centimeters in length are produced at elevated temperature during the application of strain. DAGG was previously demonstrated in commercial-purity molybdenum (Mo) materials. This is the first investigation to confirm DAGG in another material, tantalum (Ta). Previous experiments initiated and propagated DAGG using constant true-strain rate tensile tests, but this study demonstrates that DAGG can also occur under constant true-stress tensile conditions. A Mo material was tested under constant true stress, and two Ta materials were tested under constant true-strain rate. The effects of temperature, stress, strain rate, initial microstructure and texture on tensile test data and the resulting microstructures are examined. The microstructures of the Ta materials are analyzed using electron backscatter diffraction (EBSD) data to quantify the orientation, deformation, grain boundary character, and slip properties of the DAGG grains and unconsumed microstructure. The DAGG grains were found to be relatively undeformed compared to the unconsumed microstructure following DAGG and to not be oriented favorably, or unfavorably, for slip. The grain boundaries between DAGG grains in one Ta material were found to commonly have [sigma]3 character. This was likely due to a strong initial <111>-fiber texture. Previous investigations of DAGG in Mo indicated that DAGG grains commonly grow along the surface of the specimen, but this was not observed with significant frequency in Ta. Results suggest that the distance the DAGG grain boundary travels is proportional to the accumulated strain during DAGG, and the velocity of the DAGG grain boundary is proportional to the applied strain rate but is not related to the orientation of the DAGG grain or its slip properties. / text

Static abnormal grain growth (SAGG) was studied in Al-Mg alloy AA5182 sheet by varying four processing parameters: deformation temperature, strain rate, annealing temperature, and annealing time. SAGG is a secondary recrystallization process related to geometric dynamic recrystallization (GDRX) and requires both deformation at elevated temperature and subsequent static annealing. A minimum temperature is required for both SAGG and GDRX. Recrystallized grains only develop at strains larger than the critical strain for SAGG, [epsilon]SAGG. The size of the recrystallized grains is inversely related to and controlled by the density of SAGG nuclei, which increases as local strain increases. The results of this study suggest that SAGG is controlled by two thermally-activated mechanisms, dynamic recovery and recrystallization. During deformation, dynamic recovery increases as deformation temperature increases or strain rate decreases, increasing the critical strain for SAGG. SAGG is subject to an incubation time that decreases as annealing temperature increases. SAGG can produce grains large enough to reduce yield strength by 20 to 50 percent. The results of this study suggest strategies for avoiding SAGG during hot-metal forming operations by varying processing conditions to increase [epsilon]SAGG. / text

Submitted by Aelson Maciera (aelsoncm@terra.com.br) on 2017-04-18T17:39:37Z No. of bitstreams: 1 TeseJRMH.pdf: 6415770 bytes, checksum: 1bdc924884c63f0003dce6138a5d2b07 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-04-24T13:21:46Z (GMT) No. of bitstreams: 1 TeseJRMH.pdf: 6415770 bytes, checksum: 1bdc924884c63f0003dce6138a5d2b07 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-04-24T13:21:54Z (GMT) No. of bitstreams: 1 TeseJRMH.pdf: 6415770 bytes, checksum: 1bdc924884c63f0003dce6138a5d2b07 (MD5) / Made available in DSpace on 2017-04-24T13:51:09Z (GMT). No. of bitstreams: 1 TeseJRMH.pdf: 6415770 bytes, checksum: 1bdc924884c63f0003dce6138a5d2b07 (MD5) Previous issue date: 2016-10-19 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / A study was made of the synthesis and processing of magnetoelectric particulate composites of strontium barium niobate (SrxBa1-xNb2O6, or simply SBN) as a lead-free piezoelectric phase and nickel ferrite (NFO) as a magnetic phase. The specific objectives of this work were: (i) to obtain SBN (TBT) and NFO phases without impurities during the synthesis of the powders and the densification of the ceramic bodies; (ii) to produce SBN-NFO composites of 0–3 connectivity, i.e., with a highly homogeneous distribution of ferrite phase in the SBN matrix; and (iii) to ensure mechanical interphase coupling based on high densification, without the occurrence of anomalous SBN grain growth. The Sr0.61Ba0.39Nb206/NiFe2O4 biphasic system (SBN61/NFO) was prepared with molar ratios of 50/50, 70/30 and 80/20 by means of in situ chemical synthesis using the Pechini method. The objectives of this work included an analysis and proposal of phase formation during the in situ synthesis of SBN/NFO grain growth, with high chemical homogeneity, a low degree of NFO phase percolation, and 0–3 connectivity. composites. The synthesized powders were analyzed by Rietveld refinement of their X-ray diffraction patterns. This enabled the quantification of spurious phases and revealed the effect of reducing these phases and the abnormal grain growth resulting from the increased proportion of NFO phase. However, the secondary phases could only be determined based on the hypotheses put forward in the proposal of the phase formation model of the SBN/NFO system. This proposed phase formation model enabled us to understand why SBN and NFO phases can be formed simultaneously during in situ synthesis by the Pechini method, and also to conclude that the presence of precipitates during the formation of the polymeric resin may be the cause of spurious phases. This allowed us to propose changes in the synthesis step in order to eliminate possible precipitates, which actually resulted in the reduction of the secondary phases in the tests of the 70/30 system. After sintering, magnetoelectric composites were obtained with a relative density of ~96%, without abnormal grain growth, with high chemical homogeneity, a low degree of NFO phase percolation, and 0–3 connectivity. / Neste trabalho estudou-se a síntese e o processamento de compósitos magnetoelétricos particulados de niobato de estrôncio e bário (SrxBa1- xNb2O6 ou, simplesmente, SBN), como fase piezoelétrica livre de chumbo, e de ferrita de níquel (NFO), como fase magnética. Os objetivos específicos do trabalho foram: obtenção das fases SBN (TBT) e NFO como únicas do sistema, tanto durante a síntese dos pós, quanto na densificação dos corpos cerâmicos; produção de compósitos SBN-NFO com conectividade 0-3, ou seja, com alta homogeneidade da distribuição da fase ferrita em uma matriz de SBN; e garantia do acoplamento mecânico entre as fases, a partir de alta densificação e sem a ocorrência de crescimento anormal de grãos da fase SBN. Neste trabalho adotou-se a síntese in situ pelo método Pechini para a preparação do sistema bifásico Sr0,61Ba0,39Nb206/NiFe2O4 (SBN/NFO), nas proporções molares 50/50, 70/30 e 80/20. Análise e proposta de formação de fases durante a síntese in situ de compósitos SBN/NFO foram incluídas nos objetivos deste trabalho. Os pós dos compósitos sintetizados foram analisados por refinamento estrutural dos perfis de difração de raios X, pelo método de Rietveld, o que permitiu evidenciar quantitativamente a presença de fases espúrias e o efeito de redução dessas fases, e do consequente crescimento anormal de grãos, pelo incremento da proporção da fase NFO. Contudo, a determinação das fases secundárias só pode ser concluída a partir das hipóteses levantadas na proposta do modelo de formação de fases desse sistema. Além disso, esse modelo permitiu explicar porque é possível a formação simultânea das fases SBN e NFO pela síntese Pechini in situ, e também concluir que a presença de precipitados na etapa de formação da resina polimérica poderia ser a causa da ocorrência das fases espúrias. Com isso, pode-se propor alterações na etapa de síntese, com a intenção de se eliminar possíveis precipitados, o que realmente resultou, para os ensaios realizados no sistema 70/30, em redução das fases secundárias e compósitos magnetoelétricos, após sinterização, com densidade relativa ~96%, sem crescimento anormal de grãos, de elevada homogeneidade química, com baixo grau de percolação da fase NFO e conectividade 0-3. / FAPESP: 2008/04025-0 / FAPESP: 2012/24025-0 / CAPES: Procad 2013 - 3012/2014

A geração de novas fontes de energia limpa, segura e renovável por meio da fusão nuclear envolve importantes desafios tecnológicos, dentre eles a pesquisa, caracterização e a fabricação de materiais avançados para os futuros reatores de fusão nuclear. Os aços ferrítico-martensíticos de reduzida atividade radioativa, em especial a liga Eurofer-97, destacam-se por apresentar uma combinação única de propriedades para esta aplicação. O objetivo desta Tese de Doutorado é avaliar a estabilidade microestrutural deste aço recozido numa ampla faixa de temperaturas. Cálculos termodinâmicos e testes de dilatometria foram usados para determinar as temperaturas de transformação de fase. A estabilidade microestrutural foi estudada por meio de recozimentos isotérmicos entre 200 e 1350oC após laminação a frio com reduções de 40, 70, 80 e 90%. A avaliação da estabilidade mecânica do aço Eurofer-97 foi realizada por meio de medidas de dureza Vickers. As principais técnicas utilizadas para caracterização microestrutural foram microscopias eletrônica de varredura e de transmissão, tomografia por sonda atômica e medidas de magnetização DC. Tanto a textura como a microtextura foram determinadas por meio de medidas de difração de raios X e de elétrons retroespalhados (EBSD). Recuperação, recristalização primária e crescimento anormal de grão ocorrem neste material recozido abaixo de 800oC. Acima desta temperatura, a transformação martensítica ocorre alterando bastante a micoroestrutura. A cinética de crescimento anormal de grão é alterada pela quantidade de redução a frio previamente aplicada. A hipótese proposta para explicar o crescimento anormal de grãos neste material baseia-se principalmente na vantagem de tamanho adquirida pelos núcleos de recristalização primária com diferenças de orientação médias superiores a 45º em relação aos vizinhos. Neste caso, o crescimento anormal de grão é responsável por fortalecer as componentes {111} e {111}, {001} e {110}. Acima de 800oC a transformação martensítica prevalece elevando a dureza Vickers e randomizando a textura deste aço. As características do produto transformado dependem tanto da temperatura de austenitização quanto do tamanho incial do grão ferrítico. Os dados de composição química das partículas estáveis após recozimento em temperaturas inferiores a 800oC foram usados para validar os resultados dos cálculos termodinâmicos obtidos via Thermo-Calc. / Clean, safe, and renewable energy sources such as nuclear fusion comprise important technological challenges, including research, characterization and manufacture of advanced materials for future fusion reactors. Modified ferritic-martensitic steels with reduced radioactive activity (RAFM), especially Eurofer-97 steel, are among worldwide references in the nuclear field for their unique properties. The scope of this Thesis is to evaluate the microstructural (thermal) stability in ferritic-martensitic Eurofer-97 after annealing within a wide range of temperatures. Themodinamic calculations as well as dilatometric tests were used to determine the main phase transformation temperatures. The microstructural stability of this steel was followed by isothermal annealing between 200 and 1350°C after cold rolling to 40, 70, 80 and 90% reductions in thickness. The mechanical stability in the Eurofer-97 was assessed by Vickers microhardness measurements. Representative samples for each metallurgical condition were characterized by scanning electron microscopy, transmission electron microscopy, atom probe tomography, and DC-magnetization tests. Both texture and microtexture were evaluated by X-ray diffraction and electron backscattered diffraction (EBSD) techniques. Recovery, primary recrystallization, and abnormal grain growth (secondary recrystallization) processes have been observed at temperatures below 800°C. The amount of abnormally grown grains depends on the amount of previous cold rolling. The hypothesis for the most probable mechanism responsible for abnormal grain growth is based on the advantage size acquired by nuclei with misorientations above 45º surrounding their neighboring grains, even in regions where primary recrystallization was incomplete. The texture developed after abnormal grain growth has components belonging to ?- and ?-fibers with predominance of {111}, {111}, {100} e {110} components. The martensite transformation takes place when this steel is annealed above 800°C causing an increase of hardness, significant changes in microstructure, and texture weakening. The martensitic sructure depends very much on both austenitization temperature and initial austenitic grain size. The results of chemical analyses of stable particles present in samples annealed below 800oC were used to validate the thermodynamic calculations provided by Thermo-Calc.

Este trabalho tem como objetivo caracterizar as mudanças microestruturais durante o recozimento isotérmico de um fio de ferro trefilado a frio e de pureza comercial com ênfase no crescimento de grão. Os recozimentos foram realizados no intervalo de 823-1173 K por diversos tempos. As informações estatísticas do tamanho de grão foram obtidas por meio do método dos interceptos lineares. O mapeamento das orientações foi obtido por meio de difração de elétrons retroespalhados (EBSD). O material apresenta uma microestrutura ferrítica e totalmente recristalizada a partir de 873 K. Foram encontrados indícios de crescimento normal de grão a partir de 1023 K, porém este crescimento não evoluiu consideravelmente ao longo do tempo de tratamento. Os resultados obtidos a partir do método dos interceptos lineares demonstram que a distribuição de tamanho de grão segue uma curva próxima à log-normal. Nas amostras recozidas a partir de 1123 K, verificou-se a ocorrência de crescimento anormal de grão. O crescimento anormal de alguns grãos inicia-se na região central do fio, estendendo-se até uma região próxima à superfície do fio. Algumas modificações na dimensão da amostra e na atmosfera de recozimento foram realizadas a fim de se estudar a interação destas variáveis no desenvolvimento dos grãos anormais. Foram identificados indícios morfológicos de que o mecanismo para ocorrência de crescimento anormal foi o molhamento de contornos no estado sólido (solid-state wetting) que depois foram confirmados pelas análises de micro e mesotexturas. A análise de microtextura também revela que o material apresenta duas componentes preferenciais, as fibras || DT e || DT, onde DT é a direção axial de trefilação. A primeira orientação é a mais intensa, sendo que seu fortalecimento parece ser impulsionado pelo crescimento anormal de grão. A segunda é menos intensa e parece estar relacionada com as orientações dos grãos oriundos da recristalização primária. Aspectos teóricos e analíticos sobre o crescimento de grão são apresentados e associados aos resultados experimentais e à literatura. / This Dissertation aims follow the microstructural changes occurring during isothermal annealing of commercially-pure cold-drawn iron wire, with emphasys on grain growth phenomena. The grain size data were obtained by means of the linear intercept method. The orientations scanning were done by means of electron backscatter diffraction patterns (EBSD). Isothermal annealing was performed within the temperature range 823 - 1173 K for several times. The material displays full recrystallization at temperatures above 873 K. Normal grain growth was observed above 1023 K, although this growth did not evolve through longer annealing times. The results of the linear intercept method show the grain size distribution has a log-normal shape. For samples annealed above 1123 K, abnormal grain growth occurs. The first signs of secondary recrystallization appear close to the center of the wire, growing towards the surface. Changes in the wire diameter and annealing atmosphere were performed to assess the effect of these variables on abnormal grain growth. Results point out that abnormal grain growth is driven by solid-state wetting. These morphological observations were also confirmed by micro and mesotexture analyses. The microtexture also shows the presence of two major fiber texture components || WD and || WD, were WD is the axial wire-drawn direction. The first one is the most intense and its strengthening seems to be related with abnormal grain growth. The second one is weaker and it seems to be most related with small primary recrystallized grains. Theoretical and analytical features about grain growth are presented and discussed in light of literature and experimental results.