O presente trabalho visa avaliar a degradação microestrutural e variações nas propriedades mecânicas do aço 1,25Cr-0,5Mo após de 25 anos de uso em um sistema de tubulações de distribuição de vapor operando sob condições de alta pressão (10 MPa) em temperaturas elevadas (510ºC). Nesse sistema de tubulações, após 21 anos de operação, detectou-se uma trinca seguida de vazamento em uma região de concentração de tensões em um dos coletores de condensado. Desde então, tem-se monitorado por ensaios não destrutivos, a presença de trincas neste sistema. Com base nesses ensaios, em alguns testes acelerados de fluência e em análises metalográficas, foi efetuada a substituição programada de todos os coletores em outubro de 2006. A análise metalográfica de dois coletores substituídos, de um trecho de tubo e de uma curva removidos após 25 anos de operação mostra estágios avançados de degradação da microestrutura acompanhada de processo de fluência. Neste contexto, os principais objetivos deste trabalho foram concentrados nas caracterizações microestrutural e mecânica de amostras coletadas do trecho reto de tubulação, curvas e coletores. Para tanto, um conjunto de amostras foi submetido aos tratamentos térmicos de revenido e normalização seguido de revenido para avaliar a capacidade de regeneração microestrutural e mecânica. As amostras foram submetidas aos ensaios de tração à temperatura ambiente e a 510°C, ensaio de dureza e ensaio de impacto charpy antes e após os tratamentos térmicos. O trabalho foi complementado pela determinação dos principais micromecanismos de fratura. / The aim of this work is to evaluate the microstructural degradation and the mechanical properties variation of a 1.25Cr-0.5Mo steel pipeline steam after nearly 25 years of operation at 510°C and loaded by internal pressure of 10 MPa. A failure occurred after 21 years of operation caused by a crack in a stress concentration area in one of the \"T\" components of this pipe. Since then, non destructive tests have been done to evaluate the damage growth. Based on these inspections, creep tests and microstructural replication all the \"T\" components were planned to be replaced in 2006. The metallographic analysis in two \"T\" components, a piece of pipe and an elbow removed 25 years of operation shows high microstructural degradation followed by creep process. In this context, the main objective of this work was the microstructure and mechanical properties characterization of the \"T\" components, the piece of pipe and the elbow. According to this, some samples were tempered and normalized-andtempered to evaluate the capability of microstructure and mechanical regeneration. These samples were tried by stress-rupture tests on ambient and 510°C temperature, hardness tests and charpy V-notch tests, before and after heat treatments. The analyses were supplement by the determination of the principal fracture mechanisms present.

O presente trabalho visa avaliar a degradação microestrutural e variações nas propriedades mecânicas do aço 1,25Cr-0,5Mo após de 25 anos de uso em um sistema de tubulações de distribuição de vapor operando sob condições de alta pressão (10 MPa) em temperaturas elevadas (510ºC). Nesse sistema de tubulações, após 21 anos de operação, detectou-se uma trinca seguida de vazamento em uma região de concentração de tensões em um dos coletores de condensado. Desde então, tem-se monitorado por ensaios não destrutivos, a presença de trincas neste sistema. Com base nesses ensaios, em alguns testes acelerados de fluência e em análises metalográficas, foi efetuada a substituição programada de todos os coletores em outubro de 2006. A análise metalográfica de dois coletores substituídos, de um trecho de tubo e de uma curva removidos após 25 anos de operação mostra estágios avançados de degradação da microestrutura acompanhada de processo de fluência. Neste contexto, os principais objetivos deste trabalho foram concentrados nas caracterizações microestrutural e mecânica de amostras coletadas do trecho reto de tubulação, curvas e coletores. Para tanto, um conjunto de amostras foi submetido aos tratamentos térmicos de revenido e normalização seguido de revenido para avaliar a capacidade de regeneração microestrutural e mecânica. As amostras foram submetidas aos ensaios de tração à temperatura ambiente e a 510°C, ensaio de dureza e ensaio de impacto charpy antes e após os tratamentos térmicos. O trabalho foi complementado pela determinação dos principais micromecanismos de fratura. / The aim of this work is to evaluate the microstructural degradation and the mechanical properties variation of a 1.25Cr-0.5Mo steel pipeline steam after nearly 25 years of operation at 510°C and loaded by internal pressure of 10 MPa. A failure occurred after 21 years of operation caused by a crack in a stress concentration area in one of the \"T\" components of this pipe. Since then, non destructive tests have been done to evaluate the damage growth. Based on these inspections, creep tests and microstructural replication all the \"T\" components were planned to be replaced in 2006. The metallographic analysis in two \"T\" components, a piece of pipe and an elbow removed 25 years of operation shows high microstructural degradation followed by creep process. In this context, the main objective of this work was the microstructure and mechanical properties characterization of the \"T\" components, the piece of pipe and the elbow. According to this, some samples were tempered and normalized-andtempered to evaluate the capability of microstructure and mechanical regeneration. These samples were tried by stress-rupture tests on ambient and 510°C temperature, hardness tests and charpy V-notch tests, before and after heat treatments. The analyses were supplement by the determination of the principal fracture mechanisms present.

Student Number : 9800022T - PhD thesis - School of Mechanical, Industrial and Aeronautical Engineering - Faculty of Engineering and the Built Environment / For many applications, it may be useful to be able to estimate creep properties of a material from simpler testing procedures such as tensile tests than the conventional creep testing procedures. Most alloys used for creep service conditions are in a hardened condition and thus tertiary creep, controlled by micro structural degradation, is dominant. The object of the study was to investigate a reasonably simple method for estimating the creep behavior of a low alloy 1% Cr, 0.25 % Mo steel from tensile yield data. The study involved performing of series of investigations, including age hardening, tensile and creep tests. Microstructural degradation was monitored from specimens held in a furnace for different times and temperatures, which were then tested in tension at room temperatures. Tensile tests were carried out at different temperatures and strain rates and the data used to determine material parameters for use in kinetic equations describing deformation. For comparison, creep curves were obtained from both creep tests and tensile tests results. Tests on furnace aged specimens were used to quantify softening due to material degradation and formulate a structure evolution and kinetic expressions used to determine creep curves. The modified equation by Dorn was used to determine the material parameters and to predict flow characteristics. Two sets of mechanisms were observed. At low temperature and high stress (above 550MPa) dislocation by glide mechanism was investigated. At higher temperatures and low stress (below 550MPa), some form of power law creep was observed. Glide mechanism was investigated and material parameters σ ) , n and activation volume v, were calculated. The calculated value of σ ) was assumed for both plastic deformation and the softening kinetics. A reasonably good estimate of the creep behavior of the low alloy steel used in this investigation in which tertiary creep dominates can be calculated from tensile yield stress values. Furthermore, the creep rate and recovery have similar stress dependences, with the stress and temperature dependence similar to that predicted by recovery theory. The value of activation energy observed for creep for this alloy is in line with the processes which could be related to self diffusion. In order to justify the significance of this study, four existing empirical models are discussed, highlighting their merits and demerits with respect to the models used in this study. These are θ-Projection, Damage Mechanics, Estrin-Mecking and the Internal Stress Methods. Generally, in this class of alloys, recovery process occurs under an effective stress (i.e. an applied stress less the internal stress). Thus the possibility of using tensile data obtained in this study in the internals stress model was explored. The model could replicate the one used in this study if the change in internal stress value o σ is assumed to be negligible. This could be assumed to be true for tensile data at high stresses and low temperature especially during secondary creep rate when the internal stress approximates to the applied stress and at short test durations.

In modern turbine engines for propulsion and energy generation, thermal barrier coating (TBCs) protect hot-section blades and vanes, and play a critical role in enhancing reliability, durability and operation efficiency. In this study, thermal cyclic lifetime and microstructural degradation of electron beam physical vapor deposited (EB-PVD) Yttria Stabilized Zirconia (YSZ) with (Ni,Pt)Al bond coat and Hf- and/or Y- modified CMSX-4 superalloy substrates were examined. Thermal cyclic lifetime of TBCs was measured using a furnace thermal cycle test that consisted of 10-minute heat-up, 50-minute dwell at 1135C, and 10-minute forced-air-quench. TBC lifetime was observed to improve from 600 cycles to over 3200 cycles with appropriated Hf- and/or Y alloying of CMSX-4 superalloys. This significant improvement in TBC lifetime is the highest reported lifetime in literature with similar testing parameters. Beneficial role of reactive element (RE) on the durability of TBCS were systematically investigated in this study. Photostimulated luminescence spectroscopy (PL) was employed to non-destructively measure the residual stress within the TGO scale as a function of thermal cycling. Extensive microstructural analysis with emphasis on the YSZ/TGO interface, TGO scale, TGO/bond coat interface was carried out by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and scanning electron microscopy (STEM) as a funcion of thermal cycling including after the spallation failure. Focused ion beam in-situ lift-out (FIB-INLO) technique was employed to prepare site-specific TEM specimens. X-ray diffraction (XRD) and secondary ion mass spectroscopy (SIMS) were also employed for phase identification and interfacial chemical analysis. While undulation of TGO/bond coat interface (e.g., rumpling and ratcheting) was observed to be the main mechanism of degradation for the TBCs on baseline CMSX-4, the same interface remained relatively flat (e.g., suppressed rumpling and ratcheting) for durable TBCs on Hf- and/or Y-modified CMSX-4. The fracture paths changed from the YSZ/TGO interface to the TGO/bond coat interface when rumpling was suppressed. The geometrical incompatibility between the undulated TGO and EB-PVD YSZ lead to the failure at the YSZ/TGO interface for TBCs with baseline CMSX-4. The magnitude of copressive residual stress within the TGO scale measured by PL gradually decreased as a function of thermal cycling for TBCs with baseline CMSX-4 superalloy substrates. This gradual decrease corrsponds well to the undulation of the TGO scale that may lead to relaxation of the compressive residual stress within the TGO scale. For TBCs with Hf- and/or Y-modified CMSX-4 superalloy substrates, the magnitude of compressive residual stress within the TGO scale remained relatively constant throughout the thermal cycling, although PL corresponding to the stress-relief caused by localized cracks at the TGO/bond coat interface and within the TGO scale was observed frequently starting 50% of lifetime. A slightly smaller parabolic growth constant and grain size of the TGO scale was observed for TBCs with Hf- and/or Y- modified CMSX-4. Small monoclinic HfO2 precipitates were observed to decorate grain boundaries and the triple pointes within the alpha-Al2O3 scale for TBCs with Hf- and/or Y-modified CMSX-4 substrates. Segregation of Hf/Hf4+ at the TGO/bond coat interfaces was also observed for TBCs with Hf- and/or Y-modified CMSX-4 superalloys substrates. Adherent and pore-free YSZ/TGO interface was observed for TBCs with Hf- and/or Y-modified CMSX-4, while a significant amount of decohesion at the YSZ/TGO interface was observed for TBCs with baseline CMSX-4. The beta-NiAl(B2) phase in the (Ni,Pt)Al bond coat was observed to partially transform into gama prime-Ni3Al (L12) phase due to depletion of Al in the bond coat during oxidation. More importantly, the remaining beta-NiAl phase transformed into L10 martensitic phase upon cooling even though there was no significant difference in these phase transformations for all TBCs. Results from these microstructural observations are documented to elucidate mechanisms that suppress the rumpling of the TGO/bond coat interface, which is responsible for superior performance of EB-PVD TBCs with (Ni,Pt)Al bond coat and Hf- and/or Y-modified CMXS-4 superalloy.