X-ray diffraction (XRD) profile fitting (Rietveld method) was used in this study to characterize the microstructure for seven microalloyed steels, which were produced through thermomechanical controlled processing (TMCP). Microstructure characterization was conducted through the strip thickness. The microstructural variables studied include subgrain size, dislocation density, texture index and weight percent of retained austenite. The subgrain size was also analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). The effects of processing parameters, including coiling temperature, cooling rate and alloying elements, on the microstructure were also investigated. It was found that decreasing the coiling temperature resulted in a finer subgrain size and higher dislocation densities. The texture index was observed to increase with decreasing coiling temperature. The subgrain size decreased and dislocation density increased as the amount of alloying elements (Ni, Mo and Mn) were increased. The amount of retained austenite increased at the strip center with increasing coiling temperature and increasing C and Ni content. / Materials Engineering

Este trabalho visa analisar a influência das taxas de resfriamento e temperatura no último passe de laminação a quente de fio máquina de um aço DIN 41Cr4 sobre a microestrutura obtida após a laminação e a sua correlação com aquela resultante do tratamento térmico de esferoidização. Foi avaliado a influência da microestrutura prévia de laminação nos tempos e taxa de resfriamento do tratamento térmico necessários para garantir adequada microestrutura do aço DIN 41Cr4. Foram aplicados conceitos de laminação termomecânica através da variação dos parâmetros: temperatura no último passe de laminação (acabador) e após o último passe de laminação (formador de espiras); velocidade das esteiras do “cooling conveyor” e consequente tempo de permanência das espiras sobre a região de ventiladores e alguns parâmetros no ciclo de tratamento térmico: tempo em patamar e taxa de resfriamento durante a produção de fio máquina redondo de bitolas entre 15,88mm e 16,15mm. A avaliação da resposta às variações impostas ao processo foi realizada através de análises metalográficas de microestrutura no material laminado e no material esferoidizado (grau de esferoidização), descarbonetação e de ensaios de propriedades mecânicas como dureza e tração. A partir dos resultados buscou-se determinar a influência dos parâmetros de laminação na microestrutura do material laminado e a influência desta na resposta ao tratamento térmico de esferoidização. Foram analisadas oito diferentes condições e os resultados mostraram que maiores taxas de resfriamento resultam em microestruturas mais refinadas proporcionando uma simplificação no tratamento térmico, atendendo as propriedades desejáveis no produto final (fio máquina redondo esferoidizado). / This work aims to analyze the influence of the cooling rate, the temperature of the finishing pass and at the coil-forming during hot rolling of DIN 41Cr4 steel wire rod on the microstructure and its influence on plateau times and cooling rate during the spheroidizing heat treatment. For this study thermomechanical rolling concepts were applied through the variation of some hot rolling parameters such as: temperature at the finishing pass and at the coils-former, the cooling conveyor belts velocity and some parameters in the heat treatment cycle: soak temperature and cooling rate during the production of round wire rod with 15,88 mm and 16,15 mm diameter. The evaluation response to changes imposed on the process was evaluated by metallographic analysis of microstructure in hot rolled and spheroidized material (spheroidizing degree), hardness, decarburization and tensile test. Eight rolling conditions and cooling rates were analyzed and results showed that higher cooling rates result in finer microstructures allowing a reduction in heat treatment time to achieve the desirable properties in the final product (spheroidized round wire rod).

nÃo hà / Os aÃos maraging sÃo materiais de ultra-alta resistÃncia que tem grande importÃncia tecnolÃgica devida sua aplicaÃÃo nos setores nuclear e bÃlico. Devido suas aplicaÃÃes de responsabilidade, à necessÃrio compreender como se comportam as propriedades plÃsticas desses materiais, pois a literatura carece de informaÃÃes sobre o comportamento mecÃnico dos aÃos Mar350 e de liga desenvolvida Mar350*. Esse trabalho investigou como a diferentes nÃveis de deformaÃÃo à frio influenciam as propriedades de anisotropia plÃstica de ambos materiais. Foram realizadas deformaÃÃes a frio nos nÃveis de 50, 70 e 80% por laminaÃÃo e apÃs foram realizados recozimentos a 900ÂC por 1h variando-se a taxa de resfriamento, resfriado-se as amostras em Ãgua, ao ar e ao forno atà a temperatura ambiente. Os resultados das anÃlises metalogrÃficas mostraram que os materiais nÃo sofrem alteraÃÃes morfolÃgicas nos grÃos com a variaÃÃo de taxa de resfriamento, mas sofrem um coalescimento nas deformaÃÃes de 50 e 70%. As amostras do aÃo Mar350 laminadas a frio em 80% mostraram um ultra-refino de grÃo e a precipitaÃÃo de uma fase intermetÃlica enquanto as amostras do aÃo Mar350* mostraram um refino grÃo quando comparado Ãs demais condiÃÃes para o mesmo aÃo, mas sem sofre um endurecimento significativo. As mediÃÃes de textura mostraram com o evoluir da deformaÃÃo à frio hà uma tendÃncia de âlimpezaâ da textura apresentado mais intensa a fibra γ. As mediÃÃes de microtextura mostram que algumas para a maioria das condiÃÃes estudadas a presenÃa da componente cubo girado menos intensa γ, componentes estas que poderiam ser a justificativa para o afastamento de ΔR de zero e os menores valores de Rm. / The maraging steels are ultra - high strength materials that has great technological importance due its application in military and nuclear sectors . Because its applications, it is necessary to understand how the plastic properties of these materials behave, because the literature lacks information on the mechanical behavior of steel the Mar350 and alloy redeveloped Mar300 . This study investigated how different levels of cold deformation influence the properties of plastic anisotropy of both materials . Cold deformation were carried out on levels of 50, 70 and 80% by rolling and after was made annealing were the materials carried out at 900  C for 1h varying the rate of cooling, the samples were cooled in water , air and the furnace until the room temperature. The results of metallographic analysis showed that the materials do not undergo morphological changes in the grains by varying the cooling rate, but some coarsening undergo a deformation in 50 and 70%. The samples of cold rolled steel Mar350 80% showed an ultra- grain refinement and precipitation of an intermetallic phase while the samples of steel Mar350* showed grain refining compared to the other conditions for the same steel, but without undergoes a significant hardening. The texture measurements showed the evolution of the cold deformation there is a tendency to cleanup texture appears more intense γ fiber . The measurements show that some microtexture for most conditions studied the presence of other components less intense outside the fiber γ , these components that could be the reason for the displacement of ΔR zero.

Les alliages aluminium-silicium sont les alliages d’aluminium de moulage les plus couramment employés en raison de leur faible poids, de leurs caractéristiques mécaniques et de leur fluidité. Leurs propriétés mécaniques, en particulier leur résistance, peuvent être améliorées par l’affinage des grains et la modification des précipités de silicium. Par contre, la précipitation de composés intermétalliques riches en fer, comme la phase dite beta, a un effet néfaste sur la tenue en traction et la ductilité de ces alliages. Bien que diverses méthodes aient été proposées pour atténuer les effets de la phase beta, la compréhension des mécanismes de sa croissance pourrait s’avérer utile pour réduire ses effets néfastes. L’objectif de cette étude est d’établir la relation entre la vitesse de refroidissement et les caractéristiques microstructurales des alliages Al-Si hypoeutectiques. Dans une pièce coulée réelle, la vitesse de refroidissement locale peut grandement changer d’un point à l’autre du fait de la géométrie de la pièce mais aussi du fait des paramètres de coulée. Les variations de vitesse de refroidissement affectent le processus de solidification, et ceci est rendu évident par les changements des températures caractéristiques des courbes de refroidissement enregistrées en différents endroits d’une pièce. Les relations entre ces températures caractéristiques et la taille des grains et la modification du silicium eutectique sont présentées. Cette étude a aussi porté sur l’effet de la vitesse de refroidissement sur la morphologie de la phase beta dans le cas d’un alliage ternaire Al-Fe-Si. La croissance de la phase beta a été caractérisée par tomographie post-mortem et in-situ. Enfin, certains écarts par rapport aux caractéristiques de solidification usuelles, telles que la précipitation en écriture chinoise de la phase beta et la formation de rosettes, ont été observés et sont discutés. / Aluminum-silicon alloys are the most common aluminum casting alloys produced due to their fluidity characteristic and mechanical and light weight properties. However, there are several issues concerning application of Al-Si hypoeutectic alloys such as strength, which may be improved by refining grain size of the alloy and modifying silicon precipitates. Furthermore, precipitation of Fe-bearing intermetallics such as the so-called beta phase has a detrimental effect on tensile and ductility properties of Al-Si hypoeutectic alloys. Although various methods have been proposed to mitigate the effect of beta phase, the understanding of the mechanism of growth may be useful to reduce its detrimental effects. The objective of this study is to establish the relationship between the cooling rate and morphology features in Al-Si hypoeutectic alloys. In real casting condition, cooling rate is one of the factors that is not easy to predict, because it is related to the geometry of the parts and to the casting process itself. Changes in cooling rate affect the solidification process, and this is made apparent by the changes in the characteristic temperatures of cooling curves recorded in different locations of a part. The relation between these characteristic temperatures and grain size and eutectic silicon modification are presented. Furthermore, the present study also includes the effect of cooling rate on the morphology of beta phase in the case of a ternary Al-Fe-Si alloy. An attempt to characterize the growth of beta phase was performed through post-mortem and in-situ tomography. In addition, some variations from usual solidification features such as script monoclinic phase and rosettes were observed and are discussed.

Este trabalho visa analisar a influência das taxas de resfriamento e temperatura no último passe de laminação a quente de fio máquina de um aço DIN 41Cr4 sobre a microestrutura obtida após a laminação e a sua correlação com aquela resultante do tratamento térmico de esferoidização. Foi avaliado a influência da microestrutura prévia de laminação nos tempos e taxa de resfriamento do tratamento térmico necessários para garantir adequada microestrutura do aço DIN 41Cr4. Foram aplicados conceitos de laminação termomecânica através da variação dos parâmetros: temperatura no último passe de laminação (acabador) e após o último passe de laminação (formador de espiras); velocidade das esteiras do “cooling conveyor” e consequente tempo de permanência das espiras sobre a região de ventiladores e alguns parâmetros no ciclo de tratamento térmico: tempo em patamar e taxa de resfriamento durante a produção de fio máquina redondo de bitolas entre 15,88mm e 16,15mm. A avaliação da resposta às variações impostas ao processo foi realizada através de análises metalográficas de microestrutura no material laminado e no material esferoidizado (grau de esferoidização), descarbonetação e de ensaios de propriedades mecânicas como dureza e tração. A partir dos resultados buscou-se determinar a influência dos parâmetros de laminação na microestrutura do material laminado e a influência desta na resposta ao tratamento térmico de esferoidização. Foram analisadas oito diferentes condições e os resultados mostraram que maiores taxas de resfriamento resultam em microestruturas mais refinadas proporcionando uma simplificação no tratamento térmico, atendendo as propriedades desejáveis no produto final (fio máquina redondo esferoidizado). / This work aims to analyze the influence of the cooling rate, the temperature of the finishing pass and at the coil-forming during hot rolling of DIN 41Cr4 steel wire rod on the microstructure and its influence on plateau times and cooling rate during the spheroidizing heat treatment. For this study thermomechanical rolling concepts were applied through the variation of some hot rolling parameters such as: temperature at the finishing pass and at the coils-former, the cooling conveyor belts velocity and some parameters in the heat treatment cycle: soak temperature and cooling rate during the production of round wire rod with 15,88 mm and 16,15 mm diameter. The evaluation response to changes imposed on the process was evaluated by metallographic analysis of microstructure in hot rolled and spheroidized material (spheroidizing degree), hardness, decarburization and tensile test. Eight rolling conditions and cooling rates were analyzed and results showed that higher cooling rates result in finer microstructures allowing a reduction in heat treatment time to achieve the desirable properties in the final product (spheroidized round wire rod).

As velocidades críticas de resfriamento necessárias à obtenção de percentuais definidos de martensita, presentes em amostras de aços temperados em óleo, foram determinadas por meio de curvas de resfriamento. As amostras constituíram-se de barras de aço AISI 4140 e 8640 com seções circulares de 25,4; 38,1 e 50,8 mm e barras quadradas com 25,4 e 38,1 mm de lado e comprimento igual a 5 vezes o diâmetro ou lado. Visando-se à obtenção de padrões de comparação para essas velocidades, foram também obtidas as curvas em U das durezas ao longo das seções transversais das barras e as curvas Jominy desses aços. Os resultados apresentaram boa coerência, o que garantiu a eficiência do processo. Os resultados concernentes ao teor específico de 50% de martensita foram comparados com os obtidos a partir de equações constantes na literatura. As equações não se mostraram diretamente adequadas, requerendo a obtenção de um fator de correção, que uma vez obtido mostrou-se eficiente na adequação dos valores empíricos de velocidade crítica aos determinados por meio das curvas de resfriamento. / The criticaI cooling velocities necessary to obtaining specific contents of martensite, present in test specimens of hardened steels in oil, were evaluated by means of cooling curves. The samples were constituted of bars of AISI 4140 and 8640 steels with 25,4; 38,1 and 50,8 mm diameter and squared bars with 25,4 and 38,1 mm in side by 5 times the diameter or side long. Aiming at obtaining comparison patterns for those velocities, they were also obtained the curves in U of the hardness along the traverse sections of the bars and the Jominy curves of those steels. The results presented good agreement, what guaranteed the efficiency of the process. The concerning results achieving a 50 pct martensitic microstructure were compared with those obtained from equations presented in the literature. The equations did not show good approaches, requesting the determination of a correction factor, that once obtained it was shown efficient in the adaptation of the empirical values of critical velocities to those determined by means of the cooling curves.

This master's thesis deals with the effects of the cooling rate on the grain size of magnesium alloys based on Mg–Al (AZ91E) and Mg–Zr–RE (WE43B and Elektron21). The effects of the cooling rate are analyzed on samples of varying thickness for different cooling methods (forced–air–cooling, cooling into polymer, natural air cooling). We also evaluated the final microstructure, porosity, hardness, and mechanical properties for investment castings. Based on the evaluated grain sizes, we demonstrated a significant difference in the cooling rate influence on the grain size for the alloy AZ91E. Compared to Zirconium-based alloys (WE43B and Elektron21), for which the zirconium content influences grain size the most. For the alloys based on Mg–Zr–RE, it is possible to prefer casting conditions, without negative enlarging of the grain size.

Orientador: Frederico Ozanam Papa / Resumo: Durante o processo de criopreservação os espermatozoides de garanhões sofrem danos osmóticos que são irreversíveis. Mesmo utilizando-se as melhores técnicas de criopreservação, este processo ainda é prejudicial às células espermáticas sendo em média a taxa de sobrevivência espermática em torno de 50%. Além disso, ainda há uma porcentagem de espermatozoides sobreviventes portadores de danos subletais, fazendo com que seja limitada a capacidade de sobrevivência das células espermáticas após a descongelação e como consequência existe uma queda na fertilidade. Está bem estabelecido que os espermatozoides de diferentes garanhões domésticos variam significativamente em criosensibilidade, este fato pode estar relacionado com o efeito do crioprotetor, assim como pode ter relação com o tamanho molecular do crioprotetor penetrante e curva de refrigeração utilizada. Enquanto o glicerol continua a ser o crioprotetor mais comum para espermatozoides, existem fatores limitantes pelo seu uso, incluindo danos na membrana através de um efeito osmótico, sendo assim, as amidas têm sido estudas com o objetivo de minimizar os efeitos causados pelo glicerol durante o processo de criopreservação, por apresentarem melhor crioproteção da membrana das células espermáticas. Sendo assim, a proposta desse trabalho foi avaliar diferentes crioprotetores em diferentes curvas de refrigeração sobre a qualidade do sêmen equino. Para tanto, o estudo foi realizado para avaliar o efeito dos crioprotetores glicerol... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: During the cryopreservation process, sperm from stallions suffer osmotic damage that is irreversible. Even using the best cryopreservation techniques, this process is still harmful to sperm cells, with an average sperm survival rate of around 50%. In addition, there is still a percentage of surviving sperm with sublethal damage, causing the sperm cells' ability to survive after thawing to be limited and as a consequence there is a fall in fertility. It is well established that sperm from different domestic stallions vary significantly in cryosensitivity, this fact may be related to the effect of the cryoprotectant, as well as it may be related to the molecular size of the penetrating cryoprotectant and the cooling curve used. While glycerol remains the most common cryoprotectant for sperm, there are limiting factors for its use, including damage to the membrane through an osmotic effect, so amides have been studied with the aim of minimizing the effects caused by glycerol during cryopreservation process, as they present better cryoprotection of the sperm cell membrane. Thus, the purpose of this work was to evaluate different cryoprotectants in different refrigeration curves on the quality of equine semen. To this end, the study was carried out to evaluate the effect of cryoprotectants glycerol, methylformamide, dimethylformamide and dimethylacetamide in concentration at 5% in four refrigeration curves: 1°C/min-1, 0.25°C/min-1, 4°C/min-1 with stabilization at 5°C for 15min and... (Complete abstract click electronic access below) / Doutor

Friction stir welding (FSW) of HSLA steel commonly produces a hard zone (HZ) on the advancing side (AS) of the weld. Despite its detrimental effects on weld toughness, the mechanisms of its formation have not been thoroughly investigated and are not well understood. This paper investigates the various mechanisms in FSW believed to affect the weld HZ, namely: strain, strain-rate, peak temperature and cooling rate. Gleeble tests indicate that strain and strain rate have negligible effects on weld HZ with cooling rate and peak temperature as dominant effects. Jominy tests resulted in cooling rate having 270% greater influence than peak temperature on the formation of lath ferrite microstructures similar to what is observed in the HZ of FSW X65. Comparing weld HZ microstructures to Jominy tests, it is estimated that cooling rates on the AS of the weld are at least 150°C/s higher than the retreating side. Reducing the cooling rate on the AS will likely lead to an improved microstructure at the weld HZ.

Tensile strength modelling is usually done to predict the mechanical properties of lamellargraphite iron considering microstructural features. This work attempts to create a simplifiedmodel incorporating cooling rate and solidification time without considering themicrostructural features. This model will save time and cost in industry with the presence of acommercially available software such as Magmasoft which simulates solidification time andcooling rate. A plate model was designed for this purpose as the test geometry to createvariation in solidification time and cooling rate. By altering fraction solid, thermalconductivity, specific heat capacity in Magmasoft, a good fit was created between simulatedcooling curve and experimental cooling curves. The experimental UTS data of samples fromthree moulds were investigated and a regression model was created using statistics toolMinitab. The effect of solidification time and alloying on the graphite length Lmax was studiedfor twelve samples from each mould. Quantification of the effect of cooling rate and alloyingon the pearlitic properties of grey iron like matrix microhardness, pearlite inter-lamellarspacing was also investigated in this work.The developed model has sixty three percent correlation and explains UTS well in terms ofsolidification time and cooling rate. Microhardness measurements show that there is an almostlinear relationship between the cooling rate and microhardness of the matrix structure.Microhardness data also provides an overview of the pearlite fineness/interlamellar spacing.Analysis of the outliers showed that the presence of free ferrite on a fully pearlitic structurereduces the UTS significantly. Comparison of the regression model obtained from this workwith previous work showed that, there is a reduction in the predicted strength with this model.The effort to identify the reason for this reduction was not successful and needs furtherinvestigation. Pearlite inter-lamellar spacing measurement was not accurate. The relationshipbetween pearlite interlamellar spacing and matrix microhardness needs to be investigated inthe future using a better technique for pearlite spacing measurement. This will be useful tounderstand the effect of cooling rate on pearlite spacing and consequently on the UTS of greycast iron. / Draghållfasthetsmodellering görs vanligtvis för att förutsäga de mekaniska egenskaperna av lamellärt grafitjärn. Detta arbete har försökt att skapa en förenklad modell som innehåller kylhastighet och stelningstid utan att överväga mikrostrukturella egenskaper. Modellen kommer att spara tid och kostnad i industrin tillsammans med kommersiellt tillgänglig mjukvara som Magmasoft som simulerar stelningstiden och kylningshastighet. En plattformig modell utformades för detta ändamål som testgeometrin för att skapa variation i stelningstid och kylningshastighet. Genom att ändra fraktion fast fas, termisk konduktivitet och specifik värmekapacitet i Magmasoft skapades en bra anpassning mellan simulerade och experimentella kylkurvor. Experimentella draghållfasthetsdata (UTS) för prover från tre gjutningar undersöktes och en regressionsmodell skapades med hjälp av statistikverktyg Minitab. Effekten av stelningstid och legeringshalt på grafitlängden Lmax studerades för tolv prover från varje form. Effekten av kylhastighet och legering på de perlitiska egenskaperna hos grått järn som matrismikrohårdhet och perlitlamellavstånd undersöktes också i detta arbete.  Den utvecklade modellen har sextiotre procent korrelation och förklarar UTS väl med avseende på stelningstid och kylningshastighet. Mikrohårdhetsmätningar visar att det finns ett nästan linjärt förhållande mellan kylhastigheten och mikrohårdheten hos matrisstrukturen. Mikrohårdhetsdata ger också en översikt över perlitens finhet/interlamellära avstånd. Analys av outliers visade att närvaron av fri ferrit på en fullständigt perlitisk struktur minskar UTS betydligt. Jämförelse av regressionsmodellen erhållen från detta arbete med tidigare arbete visade det att det finns en minskning av den förutsagda styrkan med denna modell. Ansträngningen att identifiera orsaken till denna minskning var inte framgångsrik och behöver ytterligare undersökas. Perlit mellan lamellär avståndsmätning var inte korrekt. Förhållandet mellan perlitens interlamellära avstånd och matrismikrohet måste undersökas i framtiden med hjälp av en bättre teknik för perlit-avståndsmätning. Detta kommer att vara användbart att förstå effekten av kylhastighet på perlitavståndet och följaktligen på UTS av grå gjutjärn