In this study a series of novel Fe-based materials derived from a bulk metallic glass-forming composition was investigated to improve the ductility of this high-strength glassy alloy. The interplay between the factors chemistry, structure and resulting mechanical properties was analyzed in detail. It has been recognized that subtle modifications of the chemical composition (carbon addition) lead to appreciable changes in the phase formation, which occurs upon solidification (from a single-phase structure to composite materials). As a consequence, significant differences in the mechanical response of the particular samples have been observed. The materials developed here were fabricated by centrifugal casting. To explore the structure features of the as-cast cylinders, manifold experimental techniques (X-ray diffraction, optical, as well as electron microscopy) were employed. The occurrence of the numerous reflections on the X-ray diffraction patterns has confirmed the crystalline nature of the studied Fe-based alloy systems. The subsequent extensive research on their deformation behavior (Vickers hardness and room temperature compression tests) has revealed that, although the glass-forming ability of the investigated compositions is not high enough to obtain a glassy phase as a product of casting, excellent mechanical characteristics (high strength - comparable to that of the reference bulk metallic glass (BMG) - associated with good ductility) were achieved for the “composite-like” alloys. In contrast, the single phase cylinders, subjected to compressive loading, manifested an amazing capacity for plastic deformation – no failure occurred. The fracture motives developed during deformation of the “composite-structured” samples were studied by scanning electron microscopy. The main emphasis has been put on understanding the mechanisms of crack propagation. Owing to the structural complexity of the deformed samples, it was crucial to elucidate the properties of the individual compounds. Based on the obtained results it was concluded that the coexistence of a soft f.c.c. γ-Fe phase in combination with a hard complex matrix is responsible for the outstanding mechanical response of the tested composites. While the soft particles of an austenite contribute to the ductility (they hinder the crack propagation and hence, cause unequivocal strain-hardening), the hard constituents of the matrix phase yield the strength.

Orientadores: Amauri Garcia, Noé Cheung / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-16T22:32:29Z (GMT). No. of bitstreams: 1 Bertelli_Felipe_M.pdf: 6382019 bytes, checksum: 7bc62ea83b7e721ef82e5669d236559f (MD5) Previous issue date: 2010 / Resumo: Neste trabalho, o software ANSYS, baseado no Método dos Elementos Finitos, é adaptado para a simulação tridimensional do fluxo de calor no processo de refusão superficial a laser. A análise numérica é validada com resultados simulados por outros modelos existentes na literatura para casos de refusão superficial a laser de alumínio puro e com resultados simulados e experimentais de uma liga Al-5%Ni. Ensaios experimentais próprios foram realizados em amostras de uma liga Al-1,5%Fe, utilizando um laser à fibra dopado com Itérbio, com potência máxima disponível de 2 kW. Para efeito comparativo, as trilhas foram feitas variando-se valores de velocidade de deslocamento do feixe laser para um mesmo valor de potência. Observou-se que a microestrutura tanto do substrato quanto da zona tratada apresentou morfologia tipicamente celular. As microestruturas resultantes dos tratamentos a laser foram analisadas através de microscopia eletrônica de varredura, sendo observados espaçamentos celulares extremamente refinados na área tratada a laser refletindo no aumento significativo da dureza confirmado por ensaios de microdureza Vickers. Uma técnica de dissolução parcial das amostras tratadas a laser foi aplicada para evidenciar os intermetálicos no substrato e na região tratada a laser, mostrando a modificação da redistribuição dos intermetálicos no interior da poça fundida e dando indicações de aumento da resistência à corrosão na região tratada / Abstract: In this work, the software ANSYS, based on the Finite Element Method, is adapted to simulate the three-dimensional heat flux during the laser remelting surface treatment. The numerical analysis is validated against theoretical results furnished by other models from the literature for laser surface remelting of aluminum and against theoretical and experimental results of Al-5wt%Ni alloy samples. Laser remelting experiments with Al-1,5%wtFe samples have been carried out by using a 2kW Yb fiber laser. For comparative effects, the laser tracks were performed with different laser beam velocities for a fixed value of power. It was observed that both the substrate and the treated region had a typical cellular morphology. The microstructures resulting from the laser treatment were analyzed by using electron scanning microscopy and very refined cell spacing has been observed, which can induce a significant hardness increase confirmed by Vickers microhardness tests. A partial dissolution technique has been performed to foreground the intermetallics at the substrate and at the laser treated zone, showing the intermetallics redistribution inside the molten pool and giving indications of increased corrosion resistance on the treated region / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica

Orientador: Amauri Garcia / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica / Made available in DSpace on 2018-08-14T11:35:39Z (GMT). No. of bitstreams: 1 Cante_ManuelVenceslau_D.pdf: 12795296 bytes, checksum: bd8bf91fcf479b66a28e7e3d6b5f7090 (MD5) Previous issue date: 2009 / Resumo: O desenvolvimento de microestruturas otimizadas durante o processo de solidificação são de fundamental importância nas propriedades e desempenho de produtos acabados baseados em ligas metálicas. Neste estudo é analisada a cinética envolvida no processo de solidificação, seus efeitos nos parâmetros macro e microestruturais e a sua conseqüente influência nas propriedades mecânicas. Com esse intuito, ligas hipoeutéticas do sistema binário são estudadas Al-Ni por meio de experimentos de solidificação vertical ascendente sob regime transitório de condução de calor. Os espaçamentos dendríticos primários (?1) e secundários(?2) foram medidos ao longo de todos os lingotes para cada uma das ligas analisadas e correlacionados com as variáveis térmicas de solidificação. Uma abordagem teórico-experimental é utilizada na determinação quantitativa de tais variáveis térmicas: coeficiente de transferência de calor na interface metal/molde, velocidade de deslocamento da isoterma liquidus, gradientes térmicos, taxa de resfriamento e tempo local de solidificação. Os dados experimentais referentes à solidificação das ligas são confrontados com os principais modelos teóricos de crescimento dendrítico da literatura. Este estudo aborda, também, a influência do teor de soluto nos espaçamentos dendríticos para as ligas estudadas. Do ponto de vista macroestrutural, verifica-se que a transição colunar/equiaxial (TCE) ocorre para ligas hipoeutéticas Al-Ni para uma taxa crítica de resfriamento de 0,16 K/s. Por ensaios de tração as propriedades mecânicas das ligas do sistema Al-Ni são correlacionadas com parâmetros da micro-estrutura dendrítica resultante do processo de solidificação. Verifica-se que os limites de escoamento e de resistência à tração crescem com o aumento da concentração de soluto e decrescem com o aumento dos espaçamentos dendríticos, ?1 e ?2. O alongamento específico, por outro lado, mostra-se independente da composição e do arranjo dendrítico. Para a liga Al-5%Ni foi também realizado um estudo de solidificação rápida por refusão da superfície a laser para análise das variações microestruturais e de dureza entre as áreas não tratadas e tratadas superficialmente. / Abstract: The development of optimized microstructures during the solidification stage of processing is of fundamental importance to the mechanical properties and to the performance of finished products of metallic alloys. In this study the kinetics of solidification and its effects on macro and microstructural parameters, as well as the consequent influence on the final mechanical properties are analyzed. Hypoeutectic Al-Ni alloys are studied by upward unidirectional solidification experiments under transient heat flow conditions. Primary (?1) and secondary (?2) dendrite arm spacings are measured along the castings for all alloys analyzed and correlated with transient solidification thermal variables. A combined theoretical/ experimental approach is used to quantitatively determine such thermal variables, i.e., transient metal/mold heat transfer coefficients, tip growth rates, thermal gradients, tip cooling rates and local solidification time. The experimental data concerning the Al-Ni alloys solidification are compared to the main predictive dendritic models from the literature and the dependence of dendrite arm spacing on the alloy solute content is also analyzed. From the macrostructural point of view, it is found that the CET occurs for a critical value of cooling rate of about 0.16 K/s for hypoeutectic Al-Ni alloys.With a view to correlate mechanical properties to dendrite arm spacings, tensile testings were carried out. It is found that the ultimate tensile strength and the yield strength increase with increasing alloy solute content and with decreasing primary and secondary dendrite arm spacings. In contrast, the elongation is found to be independent of both alloy composition and dendritic arrangement. For the Al 5%Ni alloy a rapid solidification study is carried out by using laser surface remelting in order to permit microstructural and microhardness variations throughout the resulting treated and untreated zones, to be analysed. / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

No description available.

Materiais com fases intermetálicas têm sido avaliados para aplicações estruturais em altas temperaturas devido à baixa massa específica e interessantes propriedades de resistência mecânica e resistência à oxidação de vários compostos. As ligas de Ti são reconhecidas pela sua excelente combinação de alta-resistência, baixa massa específica e alta resistência à corrosão. Tendo em vista a importância de estudos em temperaturas na faixa de 700 a 1000 oC para futuras aplicações, avaliou-se neste trabalho as relações de fases do sistema Ti-Si-B na região rica em Ti nesta faixa de temperatura. Sabendo-se que a utilização de técnicas de solidificação rápida permite a obtenção de ligas com maior homogeneidade química e microestruturas finas, utilizou-se a técnica \"splat-cooling\" de solidificação rápida para produção das amostras, no sentido de obter microestruturas de equilíbrio em tempos e temperaturas menores nos tratamentos térmicos. As técnicas de microscopia, difração de raios X, análise térmica e dureza foram utilizadas para caracterização dos materiais. O processo de solidificação rápida (\"splat cooling\") promoveu refinamento de microestrutura e formação de fase amorfa em diversas composições de liga com temperaturas de início de cristalização (Tx) na faixa de 524 a 641oC. Foram confirmadas a estabilidade das fases αTi, Ti6Si2B e Ti3Si a 700oC e 1000oC. Os valores de dureza dos discos solidificados rapidamente ficaram na faixa de 434 HV a 1207 HV. / Materials with intermetallic phases have been evaluated for structural applications at high temperatures due to low specific mass and attractive mechanical properties as high-strength and oxidation resistance of various compounds. Ti alloys are recognized for their excellent combination of high-strength, low specific mass and high oxidation resistance. About future applications, studies at temperatures ranging from 700 to 1000 oC are important, we evaluated in this work the phase relationships of the system Ti-Si-B in the Ti-rich region in this temperature range. Knowing that the use of rapid solidification techniques results in alloys with higher chemical homogeneity and fine microstructure, the \"splat-cooling\" technique was used to produce the samples, in order to obtain stable microstructures in lower times and temperatures at the heat treatment. Microscopy, X-ray diffraction, thermal analysis and hardness measurement techniques were used for the materials characterization. The rapid solidification - splat cooling promoted the refinement of microstructure and even the formation of amorphous phase in the microstructure of materials with initial temperatures of crystallization (Tx) in the range from 524 to 641oC. We confirmed the stability of the phases αTi, Ti6Si2B and Ti3Si at 700oC and 1000oC. The hardness of the rapidly solidified discs were in the range of 434 HV to 1207 HV.

Les implants de corps humain biocompatibles à base de Ti de faible module de Young et sans élèments toxiques sont développés dans deux régimes de matériaux, les alliags cristallins à base de Ti-Nb(-Sn) et les alliages amorphes à base de Ti -Fe -Si. Une série d'alliages à base de Ti-Nb(-Sn) a été synthétisée par une aspiration coulée par la moule de cuivre et soumis à différents traitements thermiques (refroidissement du four ou trempe à l'eau). La microstructure, les propriétés thermiques et mécaniques des échantillons traités telles que la coulée et la chaleur ont été étudiées. On montre que l'addition de Sn augmente la stabilité de la phase β. Les modules de Young de ces alliages ont été également mesurés avec des mesures par ultrasons. Les alliages Ti74Nb26 trempés à l'eau avaient le plus faible module de Young. L'addition de Sn a peu d'impact sur le module de Young des alliages Ti-Nb. Les alliages amorphes à base de Ti- Fe-Si ont été synthétisés par filage à l'état fondu. La capacité de formation des verres, les propriétés thermiques et les propriétés de corrosion des alliages à base de Ti- Fe-Si ont été étudiées. La composition vitreuse a été conçue en fonction de la règle de l'eutectique profond. On a constaté que la région la plus proche du point eutectique ternaire(Ti65Fe30Si5) est une région quasi-cristalline icosaédrique, tandis que le côté plus raide (Si côté riche) de ce point eutectique ternaire est la région de formation de verre. L'effet de L'addition élémentaire mineur (Ge, Pd, Zr) sur la capacité de formation de verre des alliages à base de Ti- Fe-Si a été également étudié. L'observation in situ d'amorphisation des alliages vitreux Ti40Zr10Cu34Pd14Sn2 en faisceau synchrotron a été effectuée. L'alliage a été vitrifié avec succès dans un appareil à sustentation aérodynamique. / The Ti-based biocompatible human body implants of low Young's modulus and without toxic elements are developed in two regime of materials, crystalline Ti-Nb(-Sn) based alloys and amorphous Ti-Fe-Si based alloys. A series of Ti-Nb(-Sn) alloys were synthesized by copper mould suction casting and subjected to different heat treatments (furnace cooling or water quenching). The microstructure, thermal and mechanical properties of the as-cast and heat treated samples were investigated. It is shown that the addition of Sn increases the stability of the β phase. The Young's moduli of these alloys were also measured by ultrasonic measurements. Water-quenched Ti74Nb26 alloy was found to exhibits the lowest Young's modulus. Sn addition has little impact on the Young's moduli of the TiNb alloys. The Ti-Fe-Si based amorphous alloys were synthesized by melt spinning. The glass forming ability, thermal properties and corrosion properties of Ti-Fe-Si based alloys were investigated. The glassy compositions were designed according to the deep eutectic rule. It was found that the region near ternary eutectic point (Ti65Fe30Si5) is an icosahedral quasicrystal forming region, whereas the steeper side (Si rich side) of this ternary eutectic point is the glass forming region. Effect of minor elemental addition (Ge, Pd, Zr) on glass forming ability of the Ti-Fe-Si based alloys was also studied. The in situ observation of amorphization of Ti40Zr10Cu34Pd14Sn2 glassy alloy in synchrotron beam was conducted. The alloy was successfully vitrified in an aerodynamic levitation apparatus.

Experiments on the production of porous metallic materials were performed on Fe-base and Al-base alloys. The method involves dissolution of gases in the liquid state and solidification at various cooling rates. The alloy compositions were selected to induce solidification of primary particles intended to control the pore distribution. For the Fe-base alloys, nitrogen was introduced into the melt by dissolution of chromium nitride powder. Fe-Cr-Mn-Si-C alloys featuring M7C3 carbide particles were selected. For the Al-base alloys, hydrogen gas was dissolved into the melt by decomposition of water vapor. Al-Ti and Al-Fe alloys featuring primary Al3Ti and Al3Fe intermetallic particles, respectively, were considered. In the Fe-base alloys, a homogeneous distribution of gas pores through the specimens’ volume was obtained at high cooling rate (water quenching) and after introduction of external nucleating agents. In the case of the Al-base alloys, a good pore distribution was observed at all cooling rates and without addition of nucleating agents. Calculations of the variation of nitrogen (respectively hydrogen) solubility based on Wagner interaction parameters suggest that pore nucleation and growth occur during precipitation of the primary particles (M7C3 carbides, Al3Ti or Al3Fe intermetallics), due to composition changes in the melt and resultant supersaturation with gas atoms. Microscopic analyses revealed that the primary particles control the pore growth in the melt and act as barriers between adjacent pores, thereby preventing pore coalescence and promoting a fine pore distribution. Uniaxial compression testing of the porous Al-Ti and Al-Fe materials showed the typical compressive behavior of cellular metals. Further work is needed to improve the quality and reproducibility of the porous structures which can possibly be used in energy absorption or load-bearing applications. As a corollary result of the quenching of hypereutectic Fe-Cr-Mn-Si-C alloys in the experiments of synthesis of porous metals, a homogeneous featureless structure was observed in some parts of the samples, instead of the equilibrium structure of M7C3 and eutectic phases. Subsequent investigations on rapid solidification of Fe-base alloys at various alloy compositions and cooling rates led to the formation of a single-phase structure for the composition Fe-8Cr-6Mn-5Mo-5Si-3.2C (wt.%), at relatively low cooling rates (≈103 K/s) and for large sample dimensions (2.85 mm). The single phase, which is likely to be the hcp ɛ-phase, was found to decompose into a finely distributed structure of bainite and carbides at ≈600 °C. The annealed structure showed very high hardness values (850 to 1200 HV), which could be exploited in the development of high-strength Fe-base materials. / QC 20100809

In the present study, the powder metallurgy was evaluated as a technique to produce high performance Al &amp / #8211 / 8Fe &amp / #8211 / 1.7V &amp / #8211 / 7.9Si (wt%) alloys for elevated temperature applications and the role of powder particle size range and extrusion ratio in the microstructural and mechanical properties of the extruded alloys was investigated. For this purpose, an air atomization method was employed to produce powders of the high temperature alloy and after that the produced powders were sieved and cold compacted. The compacted billets were subsequently hot extruded at 450 &amp / #8211 / 480 &deg / C. Five selected ranges of powders which were different in particle size (&amp / #8722 / 2000+212 &amp / #956 / m, &amp / #8722 / 212+150 &amp / #956 / m, &amp / #8722 / 150+106 &amp / #956 / m, &amp / #8722 / 106+90 &amp / #956 / m, and &amp / #8722 / 90 &amp / #956 / m) and three different extrusion ratios (144:1, 81:1, and 26:1) were used in this study. In the first part of the thesis, microstructure and thermal stability of as &amp / #8211 / air atomized powders were described. &amp / #945 / &amp / #8211 / Al matrix and &amp / #945 / &amp / #8211 / Al13(Fe, V)3Si phases were characterized in all rapidly solidified powders by XRD. The fraction of the intermetallic phases was reduced as the powder particle size increased. DTA analysis revealed an exothermic reaction at 581 &deg / C in all alloy powders of different size fractions. In the second part of the study, the effect of powder particle size and extrusion ratio on microstructural and mechanical properties (at different temperatures) of the extruded alloys was investigated. The results showed that decrease in powder particle size and increase in extrusion ratio refined the microstructure and improved the mechanical properties. It was revealed that the effect of powder size was more evident than that of extrusion ratio. Remarkable increases in mechanical properties (e.g. 60.7% increase in ultimate tensile strength at 250 &deg / C) were observed as a result of rapid solidification process (atomization) and hot extrusion.

Inconel 738 (IN 738), like other precipitation-hardened nickel-base superalloys that contain a substantial amount of Al and Ti, is very difficult to weld due to its high susceptibility to heat-affected zone (HAZ) cracking during conventional fusion welding processes. The cause of this cracking, which is usually intergranular in nature, has been attributed to the liquation of various phases in the alloy, subsequent wetting of the grain boundaries by the liquid and decohesion along one of the solid-liquid interfaces due to on-cooling tensile stresses. To address the problem of liquation cracking in weldments, recent developments in welding research have resulted in supposedly exclusive solid-state friction joining processes, such as linear friction welding (LFW), for joining crack susceptible structural alloys. The objective of this work was therefore to investigate the weldability of the difficult-to-weld IN 738 superalloy by LFW and to analyze the resulting microstructural changes in the alloy due to the welding process. LFW was performed on Linear Friction Welding Process Development System (PDS) at the Aerospace Manufacturing Technology Centre of the Institute for Aerospace Research, National Research Council (NRC) of Canada. In order to study and decouple the effect of non-equilibrium thermal cycle and imposed compressive stress during the joining, physical simulation of the LFW process was performed by using Gleeble 1500-D Thermo-Mechanical Simulation System at the University of Manitoba. Detailed microstructural study of welded and Gleeble-simulated materials was carried out. Correlation between the simulated microstructure and that of the weldments was obtained, in that, a significant grain boundary liquation was observed in both the simulated specimens and actual weldments due to non-equilibrium reaction of second phase particles, including the strengthening gamma prime phase. These results show that in contrast to the general assumption of LFW being an exclusively solid-state joining process, intergranular liquation, caused by non-equilibrium phase reaction(s), occurred during the process. However, despite a significant occurrence of liquation in the alloy, no HAZ cracking was observed. Nevertheless, the result showed that crack-free welding by linear friction welding is not due to preclusion of grain boundary liquation as has been commonly assumed and reported. Instead, resistance to cracking can be related to the counter-crack-formation effect of the imposed strain and to a concept observed and reported for the first time in this work, which is strain-induced rapid solidification. Furthermore, microstructural evolution during joining cannot be understood without considering the concept of non-equilibrium liquation reaction and strain-induced rapid solidification of the metastable liquid, which are carefully elucidated in this thesis.

Inconel 738 (IN 738), like other precipitation-hardened nickel-base superalloys that contain a substantial amount of Al and Ti, is very difficult to weld due to its high susceptibility to heat-affected zone (HAZ) cracking during conventional fusion welding processes. The cause of this cracking, which is usually intergranular in nature, has been attributed to the liquation of various phases in the alloy, subsequent wetting of the grain boundaries by the liquid and decohesion along one of the solid-liquid interfaces due to on-cooling tensile stresses. To address the problem of liquation cracking in weldments, recent developments in welding research have resulted in supposedly exclusive solid-state friction joining processes, such as linear friction welding (LFW), for joining crack susceptible structural alloys. The objective of this work was therefore to investigate the weldability of the difficult-to-weld IN 738 superalloy by LFW and to analyze the resulting microstructural changes in the alloy due to the welding process. LFW was performed on Linear Friction Welding Process Development System (PDS) at the Aerospace Manufacturing Technology Centre of the Institute for Aerospace Research, National Research Council (NRC) of Canada. In order to study and decouple the effect of non-equilibrium thermal cycle and imposed compressive stress during the joining, physical simulation of the LFW process was performed by using Gleeble 1500-D Thermo-Mechanical Simulation System at the University of Manitoba. Detailed microstructural study of welded and Gleeble-simulated materials was carried out. Correlation between the simulated microstructure and that of the weldments was obtained, in that, a significant grain boundary liquation was observed in both the simulated specimens and actual weldments due to non-equilibrium reaction of second phase particles, including the strengthening gamma prime phase. These results show that in contrast to the general assumption of LFW being an exclusively solid-state joining process, intergranular liquation, caused by non-equilibrium phase reaction(s), occurred during the process. However, despite a significant occurrence of liquation in the alloy, no HAZ cracking was observed. Nevertheless, the result showed that crack-free welding by linear friction welding is not due to preclusion of grain boundary liquation as has been commonly assumed and reported. Instead, resistance to cracking can be related to the counter-crack-formation effect of the imposed strain and to a concept observed and reported for the first time in this work, which is strain-induced rapid solidification. Furthermore, microstructural evolution during joining cannot be understood without considering the concept of non-equilibrium liquation reaction and strain-induced rapid solidification of the metastable liquid, which are carefully elucidated in this thesis.