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Cleavage fracture in ferritic steels can be defined as a sequence of few critical steps. At first nucleation of a microcrack takes place, often in a hard inclusion. This microcrack then propagates into the surrounding matrix material. The last obstacle before failure is the encounter of grain boundaries. If a microcrack is not arrested during any of those steps, cleavage takes place. Temperature plays an important role since it changes the failure mode from ductile to brittle in a narrow temperature interval. In papers A and B micromechanical models of the last critical phase are developed (cleavage over a grain boundary) in order to examine the mechanics of this phase. An extensive parameter study is performed in Paper A, where cleavage planes of two grains are allowed to tilt relative each other. It is there shown that triaxiality has a significant effect on the largest grain size that can arrest a rapidly propagating microcrack. This effect is explained by the development of the plastic zone prior to crack growth. The effect of temperature, addressed through a change in the visco-plastic response of the ferrite, shows that the critical grain size increases with the temperature. This implies that with an increasing temperature more cracks can be arrested, that is to say that less can become critical and thus that the resistance to fracture increases. Paper B shows simulations of microcrack propagation when the cleavage planes of two neighboring grains are tilted and twisted relatively each other. It is shown that when a microcrack enters a new grain, it first does it along primary cleavage planes. During further growth the crack front is protruded along the primary planes and lags behind along the secondary ones. The effect of tilt and twist on the critical grain size is decoupled with twist misorientation offering a greater resistance to propagation. Simulations of cracking of a particle and microcrack growth across an inclusion-matrix interface are made in Paper C. It is shown that the particle stress can be expressed by an Eshelby type expression modified for plasticity. The analysis of dynamic growth, results in a modified Griffith expression. Both findings are implemented into a micromechanics-based probabilistic model for cleavage that is of a weakest link type and incorporates all critical phases of cleavage: crack nucleation, propagation over particle-matrix interface and into consecutive grains. The proposed model depends on six parameters, which are obtained for three temperatures in Paper D using experimental data from SE(B) tests. At the lowest temperature, -30° , the model gives an excellent prediction of the cumulative failure probability by cleavage fracture and captures the threshold toughness and the experimental scatter. At 25º  and 55º  the model slightly overestimates the fracture probability. In Paper E a serie of fracture experiments is performed on half-elliptical surface cracks at 25º in order to further verify the model. Experiments show a significant scatter in the fracture toughness. The model significantly overestimates the fracture probability for this crack geometry. / QC 20100910

Submitted by Juliana Cristine de Sousa Teixeira (jullysousa@gmail.com) on 2018-05-18T20:34:21Z No. of bitstreams: 1 Tese de Mestrado_Juliana Cristine de Sousa Teixeira_Final.pdf: 5778909 bytes, checksum: 048e61d5039f6fe8cb5e93a20b68b791 (MD5) / Rejected by Pamella Benevides Gonçalves null (pamella@feg.unesp.br), reason: Solicitamos que realize correções na submissão seguindo as orientações abaixo: • A capa e a ficha catalográfica não são consideradas para contagem de páginas. a paginação deve aparecer no canto superior direito a partir da introdução, realizei a contagem das páginas e seu trabalho deve com o número (17)*, após você precisa atualizar a numeração na ficha catalográfica, nas listas e no sumário • Referências. A palavra Referências deve ser centralizada, e não conter numeração de seção; As referencias devem ser justificadas, espaço simples com um espaço simples(enter) entre elas. • Será necessário revisar suas referências, logo, sobre a elaboração das referencias e citações favor solicitar ajuda com a bibliotecária Juciene (juciene@feg.unesp.br) ou consultar os modelos de referências nas diretrizes http://www.feg.unesp.br/Home/Biblioteca21/diretrizes-2016.pdf A identificação deve ser feita por letras maiúsculas, consecutivas seguidas de travessão e seus respectivos títulos. Exemplo: ANEXO A - Modelo de formulário Agradecemos a compreensão. on 2018-05-21T12:20:53Z (GMT) / Submitted by Juliana Cristine de Sousa Teixeira (jullysousa@gmail.com) on 2018-05-30T01:46:04Z No. of bitstreams: 1 Tese de Mestrado_Juliana Cristine de Sousa Teixeira_29052018.pdf: 5816923 bytes, checksum: 39d3338ac2cdd4e61f96dc8b8bde5084 (MD5) / Approved for entry into archive by Pamella Benevides Gonçalves null (pamella@feg.unesp.br) on 2018-06-11T12:25:10Z (GMT) No. of bitstreams: 1 teixeira_jcs_me_guara.pdf: 6341115 bytes, checksum: 44f465e9d11d884cc4f765165da772f7 (MD5) / Made available in DSpace on 2018-06-11T12:25:10Z (GMT). No. of bitstreams: 1 teixeira_jcs_me_guara.pdf: 6341115 bytes, checksum: 44f465e9d11d884cc4f765165da772f7 (MD5) Previous issue date: 2018-04-06 / O ensaio de queda de peso DWTT (Drop Weigth Tear Test) é um método amplamente utilizado pela indústria de óleo e gás para determinar a capacidade de um material em impedir a propagação de uma trinca. Esse método foi desenvolvido pelo Battelle Memorial Institute, e é realizado em conformidade com a especificação API RP 5L3 "Práticas Recomendadas para a Condução de Testes de Queda de Peso". Com o desenvolvimento dos aços ARBL, o comportamento dos aços vem mostrando algumas particularidades resultantes do processamento termomecânico, e por esse motivo, podem não apresentar o mesmo comportamento à fratura que aços mais antigos, como delaminações ou inclusões não metálicas. Atualmente são propostos dois tipos de entalhe, sendo o tipo prensado, obtido pela estampagem de uma matriz na amostra, e o tipo Chevron, que deve ser usinado. A correlação entre ambos os entalhes pode ser realizada apenas para a análise da porcentagem da superfície dúctil da fratura. Outros tipos de correlação como energia absorvida para impacto, não são recomendados, uma vez que a concentração de tensão para o entalhe Chevron é muito maior, facilitando o rompimento da amostra, enquanto que o entalhe prensado demanda maior energia, uma vez que possui maior encruamento na região. No presente trabalho foram realizados os levantamentos de curvas de temperatura de transição dúctil e frágil (TTDF) do material base do tubo com dimensões de 762 mm x 38,1 mm de aço carbono com grau API X60, através da análise da porcentagem de fratura dúctil resultante cujo os resultados se mostraram equivalentes tanto para o entalhe Prensado como Chevron; energia absorvida pela leitura do equipamento de DWTT com cutelo instrumentado, apresentando resultados não comparativos, sendo necessário maior energia para fraturar um CP com entalhe Prensado e menor energia para fraturar um CP com entalhe usinado Chevron; e expansão lateral, resultante das amostras para ambos os tipos de entalhes, cujo os resultados possuem similaridade, entretanto não equivalentes. Para correlacionar a energia absorvida, também foi realizada a TTDF por ensaio de impacto (CVN), contudo a correção não foi possível, devido ao tamanho da amostra ser distinta ao DWTT / The Drop Weigth Tear Test (DWTT) is a method widely used by the oil and gas industry to determine the ability of a material to prevent the propagation of a crack. This method was developed by the Battelle Memorial Institute, and is performed in accordance with API RP 5L3 "Drop-Weight Tear Tests on Line Pipe" specification. With the development of ARBL steels, the behavior of steels has shown some particularities resulting from thermomechanical processing, and for this reason, they may not present the same fracture behavior as older steels, such as delamination or nonmetallic inclusions. Currently two types of notch are proposed, being the type pressed, obtained by the stamping of a matrix in the sample, and the type Chevron, that must be machined. The correlation between both notches can be performed only for the analysis of the percentage of the ductile surface of the fracture. Other types of correlation as energy absorbed for impact are not recommended, since the stress concentration for the Chevron notch is higher, facilitating the rupture of the sample, while the notched press demands greater energy, since it has greater hardening in the region. In the present study, the ductile and brittle transition temperature (TTDF) curves of the base material of the pipe with dimensions of 762 mm x 38.1 mm of carbon steel with API grade X60 were carried out, through the analysis of the percentage of ductile fracture resulting whose results were shown to be equivalent for both notch: Pressed and Chevron; energy absorbed by reading DWTT equipment with instrumented cleaver, presenting non-comparative results, requiring greater energy to fracture a sample with notched Press and lower energy to fracture a sample with Chevron machined notch; and lateral expansion, resulting from the samples for both types of notches, whose results have similarity, however not equivalent. In order to correlate absorbed energy, TTDF was also performed by impact test (CVN), however correction was not possible, because the sample size was distinct from DWTT

Orientador: Marcelo dos Santos Pereira / Resumo: O ensaio de queda de peso DWTT (Drop Weigth Tear Test) é um método amplamente utilizado pela indústria de óleo e gás para determinar a capacidade de um material em impedir a propagação de uma trinca. Esse método foi desenvolvido pelo Battelle Memorial Institute, e é realizado em conformidade com a especificação API RP 5L3 "Práticas Recomendadas para a Condução de Testes de Queda de Peso". Com o desenvolvimento dos aços ARBL, o comportamento dos aços vem mostrando algumas particularidades resultantes do processamento termomecânico, e por esse motivo, podem não apresentar o mesmo comportamento à fratura que aços mais antigos, como delaminações ou inclusões não metálicas. Atualmente são propostos dois tipos de entalhe, sendo o tipo prensado, obtido pela estampagem de uma matriz na amostra, e o tipo Chevron, que deve ser usinado. A correlação entre ambos os entalhes pode ser realizada apenas para a análise da porcentagem da superfície dúctil da fratura. Outros tipos de correlação como energia absorvida para impacto, não são recomendados, uma vez que a concentração de tensão para o entalhe Chevron é muito maior, facilitando o rompimento da amostra, enquanto que o entalhe prensado demanda maior energia, uma vez que possui maior encruamento na região. No presente trabalho foram realizados os levantamentos de curvas de temperatura de transição dúctil e frágil (TTDF) do material base do tubo com dimensões de 762 mm x 38,1 mm de aço carbono com grau API X60, através da análise da porce... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The Drop Weigth Tear Test (DWTT) is a method widely used by the oil and gas industry to determine the ability of a material to prevent the propagation of a crack. This method was developed by the Battelle Memorial Institute, and is performed in accordance with API RP 5L3 "Drop-Weight Tear Tests on Line Pipe" specification. With the development of ARBL steels, the behavior of steels has shown some particularities resulting from thermomechanical processing, and for this reason, they may not present the same fracture behavior as older steels, such as delamination or nonmetallic inclusions. Currently two types of notch are proposed, being the type pressed, obtained by the stamping of a matrix in the sample, and the type Chevron, that must be machined. The correlation between both notches can be performed only for the analysis of the percentage of the ductile surface of the fracture. Other types of correlation as energy absorbed for impact are not recommended, since the stress concentration for the Chevron notch is higher, facilitating the rupture of the sample, while the notched press demands greater energy, since it has greater hardening in the region. In the present study, the ductile and brittle transition temperature (TTDF) curves of the base material of the pipe with dimensions of 762 mm x 38.1 mm of carbon steel with API grade X60 were carried out, through the analysis of the percentage of ductile fracture resulting whose results were shown to be equivalent for both notch: ... (Complete abstract click electronic access below) / Mestre

Pour des intérêts technologiques, la compréhension des mécanismes de déformation des nano-structures est essentielle afin d'éviter que la relaxation des contraintes ne génère des défauts aux conséquences parfois catastrophiques. De plus, dans les nano-objets semi-conducteurs, les expériences montrent une transition fragile-ductile qui dépend de la taille des systèmes : ils sont ductiles pour des dimensions inférieures à quelques centaines de nanomètres, fragiles au-delà. Nous avons abordé ce problème via des calculs de dynamique moléculaire pour simuler des tests de déformation de nano-fils, et nous avons choisi le silicium comme prototype de matériau semi-conducteur. Nous avons dans un premier temps analysé des grandeurs mesurables comme les coefficients d'élasticité et la limite d'élasticité en fonction de différents paramètres, et montré notamment que la limite d'élasticité diminue quand la hauteur du nano-fil augmente. L'analyse à l'échelle atomique des systèmes déformés nous a permis de décomposer le comportement global des nano-fils en mécanismes élémentaires ; nous avons ainsi montré que la nucléation d'une première dislocation est à l'origine de l'ensemble des comportements, ductiles et fragiles. Après cette nucléation initiale, le comportement global du nano-fil est déterminé par la compétition entre la nucléation d'autres dislocations et l'ouverture de cavités. Finalement, nous avons essayé d'estimer quantitativement les degrés de ductilité et de fragilité des nano-fils en analysant l'énergie relaxée pendant le régime plastique par ces deux mécanismes élémentaires, et de rationaliser ainsi le rôle de la taille du système sur la transition fragile-ductile. / For technological interest, the understanding of the deformation mechanisms at the nano-scale is essential in order to prevent stress relaxation mechanisms that could lead to defects formation and/or to catastrophic failure. Furthermore, recent experimental findings showed in semiconductor nano-objects, a size dependent brittle to ductile transition: they are ductile below a few hundreds of nanometers, brittle above that scale. To investigate this behavior, we have used molecular dynamics as a tool to simulate deformation tests of nanowires and we have used silicon as a prototypical semiconductor material. First we analyzed a number of measurable quantities such as the elasticity coefficients and the elasticity limit with respect to various parameters and we found that the elasticity limit decreases when the length of the nanowire increases. An analysis of the atomic structure of the deformed systems allowed us to decompose the overall mechanical behavior of the nanowires into elementary mechanisms; we thus showed that the nucleation of a first dislocation was systematically at the origin of ductility and brittleness. After the initial dislocation nucleation, the competition between further dislocation nucleation events and cavities opening, determine the overall mechanical behavior of the nanowire. Finally, we tried to estimate quantitatively the degree of ductility and brittleness of the nanowires by analyzing the amount of energy released by those two elementary mechanisms during the plastic regime and we rationalized the role of the size of the deformed systems on the brittle to ductile transition.

Pt-aluminide (PtAl) coatings form an integral part of thermal barrier coating (TBC) systems that are applied on Ni-based superalloy components operating in the hot sections of gas turbine engines. These coatings serve as a bond coat between the superalloy substrate and the ceramic yttrium stabilized zirconia (YSZ) coating in the TBC system and provide oxidation resistance to the superalloy component during service at high temperatures. The PtAl coatings are formed by the diffusion aluminizing process and form an integral part of the superalloy substrate. The microstructure of the PtAl coatings is heavily graded in composition as well as phase constitution. The matrix phase of the coating is constituted of the B2-NiAl phase. Pt, in the coating, is present as a separate PtAl2 phase as well as in solid solution in B2-NiAl. The oxidation resistance of the PtAl bond coat is derived from the B2-NiAl phase. At high temperatures, Al from the B2-NiAl phase forms a regenerative layer of alumina on the coating surface which, thereby, lowers the overall oxidation rate of the superalloy substrate. The presence of Pt is beneficial in improving the adherence of the alumina scale to the surface and thereby enhancing the oxidation resistance of the coating. However, despite its excellent oxidation resistance, the B2-NiAl being an intermetallic phase, renders the PtAl coating brittle and imparts it with a high brittle-to-ductile-transition-temperature (BDTT). The PtAl coating, therefore, remains prone to cracking during service. The penetration of these cracks into the substrate is known to degrade the strain tolerance of the components. Evaluation of the mechanical behavior of these coatings, therefore, becomes important from the point of views of scientific understanding as well as application of these coatings in gas turbine engine components. Studies on the mechanical behavior of coatings have been mostly carried on coated bulk superalloy specimens. However, since the coating is brittle and the superalloy substrate more ductile when compared to the coating, the results obtained from these studies may not be representative of the coating. Therefore, it is imperative that the mechanical behavior of the coating in stand-alone condition, i.e. the free-standing coating specimen without any substrate attached to it, be evaluated for ascertaining the true mechanical response of the coating. Study of stand-alone bond coats involves complex specimen preparation techniques and challenging testing procedures. Therefore, reports on the evaluation of mechanical properties of stand-alone coatings are limited in open literature. Further, no systematic effort has so far been made to examine important aspects such as the effect of temperature and strain rate on the tensile behavior of these coatings. The deformation mechanisms associated with these bond coats have also not been reported in the literature. In light of the above, the present research study aims at evaluating the tensile behavior of free-standing PtAl coatings by the micro-tensile testing technique. The micro-tensile testing method was chosen for property evaluation because of its inherent ability to generate uniform strain in the specimen while testing, which makes the results easy to interpret. Further, since the technique offers the feasibility to test the entire graded PtAl coating in-situ, the results remain representative of the coating. Using the above testing technique, the tensile behavior of the PtAl coating has been evaluated at various temperatures and strain rates. The effect of strain rate on the BDTT of the coating has been ascertained. Further, the effect of Pt content on the tensile behavior of these coatings has also been evaluated. Attempts have been made to identify the mechanisms associated with tensile deformation and fracture in these coatings. The thesis is divided into nine chapters. Chapter 1 presents a brief introduction on the operating environment in gas turbine engines and the materials that are used in the hot sections of gas turbine engines. The degradation mechanisms taking place in the superalloy in gas turbine environments and the need for application of coatings has also been highlighted. The basic architecture of a typical thermal barrier coating (TBC) system applied on gas turbine engine components has been presented. The constituents of the TBC system, i.e. the ceramic YSZ coating, MCrAlY overlay as well as diffusion aluminide bond coats and, the various techniques adopted for the deposition of these coatings have been described in brief. Chapter 2 presents an overview of the literature relevant to this study. This chapter is divided into four sub-chapters. The formation of diffusion aluminide coatings on Ni-based superalloys has been described in the first sub-chapter. Emphasis has been laid on pack cementation process for the formation of the coatings. The fundamentals of pack aluminizing process, including the thermodynamic and kinetic aspects, have been mentioned in brief. The microstructural aspects of high activity and low activity plain aluminide and Pt-aluminide coatings have also been illustrated. The techniques applied for the mechanical testing of bond coats have been discussed in the second sub-chapter. The macro-scale testing techniques have been mentioned in brief. The small scale testing methods such as indentation, bend tests and micro-tensile testing have also been discussed in the context of evaluation of mechanical properties of bond coats. Since the matrix in the aluminide bond coats is constituted of the B2-NiAl phase, a description of the crystal structure and deformation characteristics of this phase including the flow behavior, ductility and fracture behavior has been mentioned in the third sub-chapter. In the fourth sub-chapter, reported literature on the tensile behavior and brittle-to-ductile-transition-temperature (BDTT) of diffusion aluminide bond coats has been discussed. In Chapter 3, details on experiments carried out for the formation of various coatings used in the present study and, their microstructural characterization, are provided. The method for extraction of stand-alone coating specimens and their testing is discussed. The microstructure and composition of the various coatings used in the present study are discussed in detail in Chapter 4. Unlike in case of bulk tensile testing, for which standards on the design of specimens exist, there are no standards available for the design of micro-tensile specimens. Therefore, as part of the present research work, a finite element method (FEM)-based study was carried out for ascertaining the dimensions of the specimens. The simulation studies predicted that failure of the specimens within the gage length can be ensured only when certain correlations between the dimensional parameters are satisfied. Further, the predictions from the simulation study were validated experimentally by carrying out actual testing of specimens of various dimensions. Details on the above mentioned aspects of specimen design are provided in Chapter 5. The PtAl coatings undergo brittle fracture at lower temperatures while ductile fracture occurs at higher temperatures. Further, the coatings exhibit a scatter in the yielding behavior at temperatures in the vicinity of BDTT. Therefore, the BDTT, determined as the temperature at which yielding is first observed in the stress-strain curves, may not be representative of the PtAl coatings. In Chapter 6, a method for the precise determination of BDTT of aluminide bond coats, based on the variation in the plastic strain to fracture with temperature, has been demonstrated. The BDTT determined by the above method correlated well with the variation in fracture surface features of the coating and was found representative of these coatings. In Chapter 7, the effect of temperature and strain rate on the tensile properties of a PtAl bond coat has been evaluated. The temperature and strain rate was varied between room temperature (RT)-1100°C and 10-5 s-1-10-1 s-1, respectively. The effect of strain rate on the BDTT of the PtAl bond coat has been examined. Further, the variation in fracture surface features and mechanism of fracture with temperature and strain rate are illustrated. The micro-mechanisms of deformation and fracture in the coating at different temperature regimes have also been discussed. The coating exhibited brittle-to-ductile transition with increase in temperature at all strain rates. The BDTT was strain rate sensitive and increased significantly at higher strain rates. Above BDTT, YS and UTS of the coating decreased and its ductility increased with increase in the test temperature at all strain rates. Brittle behavior occurring in the coating at temperatures below the BDTT has been attributed to the lack of operative slip systems in the B2-NiAl phase of the coating. The onset of ductility in the coating in the vicinity of BDTT has been ascribed to generation of additional slip systems caused by climb of dislocations onto high index planes. The coating exhibited two distinct mechanisms for plastic deformation as the temperature was increased from BDTT to 1100°C. For temperatures in the range BDTT to about 100°C above it, deformation was controlled by dislocations overcoming the Peierls-Nabarro barrier. Above this temperature range, non-conservative motion of jogs by jog dragging mechanism controlled the deformation. The transition temperature for change of deformation mechanism also increased with increase in strain rate. For all strain rates, fracture in the coating at test temperatures below the BDTT, occurred by initiation of cracks in the intermediate single phase B2-NiAl layer of the coating and subsequent inside-out propagation of the cracks across the coating thickness. Ductile fracture in the coating above the BDTT was associated with micro-void formation throughout the coating. The effect of Pt content on the tensile behavior of PtAl coating, evaluated at various temperatures ranging from room temperature (RT) to 1100°C and at a nominal strain rate of 10-3 s-1, is presented in Chapter 8. Irrespective of Pt content in the coating, the variation in tensile behavior of the coating with temperature remained similar. At temperatures below BDTT, the coatings exhibited linear stress-strain response (brittle behavior) while yielding (ductile behavior) was observed at temperatures above BDTT. At any given temperature, the elastic modulus decreased while the strength increased with increase in Pt content in the coating. On the other hand, the ductility of the coating remained unaffected with Pt content. The BDTT of the coating also increased with increase in Pt content in the coating. Addition of Pt did not affect the fracture mechanism in the coating. Fracture at temperatures below BDTT was caused by nucleation of cracks at the intermediate layer and their subsequent inside-out propagation. At high temperatures, fracture occurred in a ductile manner comprising void formation, void linkage and subsequent joining with cracks. The deformation sub-structure of the coating did not get affected with Pt incorporation. Short straight dislocations were observed at temperatures below BDTT, while, curved dislocations marked by jog formation were observed at temperatures above BDTT. The factors controlling fracture stress and strength in the PtAl coatings at various temperatures have also been assessed. The overall summary of the present research study and recommendations for future studies are presented in the last chapter, i.e. Chapter 9.