Commercial superalloys like Rene88DT are used in high temperature applications like turbine disk in aircraft jet engines due to their excellent high temperature properties, including strength, ductility, improved fracture toughness, fatigue resistance, enhanced creep and oxidation resistance. Typically this alloy's microstructure has L12-ordered precipitates dispersed in disordered face-centered cubic γ matrix. A typical industrially relevant heat-treatment often leads to the formation of multiple size ranges of γ¢ precipitates presumably arising from multiple nucleation bursts during the continuous cooling process. The morphology and distribution of these γ′ precipitates inside γ matrix influences the mechanical properties of these materials. Therefore, the study of thermodynamic and kinetic factors influencing the evolution of these precipitates and subsequent effects is both relevant for commercial applications as well as for a fundamental understanding of the underlying phase transformations. The present research is primarily focused on understanding the mechanism of formation of different generations of γ′ precipitates during continuous cooling by coupling scanning electron microscopy (SEM), energy filtered TEM and atom probe tomography (APT). In addition, the phase transformations leading to nucleation of γ′ phase has been a topic of controversy for decades. The present work, for the first time, gives a novel insight into the mechanism of order-disorder transformations and associated phase separation processes at atomistic length scales, by coupling high angle annular dark field (HAADF) - STEM imaging and APT. The results indicate that multiple competing mechanisms can operate during a single continuous cooling process leading to different generations of γ′ including a non-classical mechanism, operative at large undercoolings.

Nickel based superalloys have superior high temperature mechanical strength, corrosion and creep resistance in harsh environments and found applications in the hot sections as turbine blades and turbine discs in jet engines and gas generator turbines in the aerospace and energy industries. The efficiency of these turbine engines depends on the turbine inlet temperature, which is determined by the high temperature strength and behavior of these superalloys. The microstructure of nickel based superalloys usually contains coherently precipitated gamma prime (?) Ni3Al phase within the random solid solution of the gamma () matrix, with the ? phase being the strengthening phase of the superalloys. How the alloying elements partition into the and ? phases and especially in the site occupancy behaviors in the strengthening ? phases play a critical role in their high temperature mechanical behaviors. The goal of this dissertation is to study the site substitution behavior of the major alloying elements including Cr, Co and Ti through first principles based calculations. Site substitution energies have been calculated using the anti-site formation, the standard defect formation formalism, and the vacancy formation based formalism. Elements such as Cr and Ti were found to show strong preference for Al sublattice, whereas Co was found to have a compositionally dependent site preference. In addition, the interaction energies between Cr-Cr, Co-Co, Ti-Ti and Cr-Co atoms have also been determined. Along with the charge transfer, chemical bonding and alloy chemistry associated with the substitutions has been investigated by examining the charge density distributions and electronic density of states to explain the chemical nature of the site substitution. Results show that Cr and Co atoms prefer to be close by on either Al sublattice or on a Ni-Al mixed lattice, suggesting a potential tendency of Cr and Co segregation in the ? phase.

One of the main sources of energy in this modern world is the gas turbine.  They reach extremely high working temperatures at peak capacity and hence require materials that can withstand the same.  Nickel-based superalloys have been widely used as working materials due to their various high-temperature properties, which help protect them from oxidation, corrosion,  and  creep.  This  high-temperature  strength  is  provided by the  gamma  prime (γ′)  phase  for  most  nickel-based  alloys.  This  study  deals  with understanding  the  effect of the mean γ′ phase size affected by different times and temperatures.  Different trial alloys have undergone different primary ageing cycles, followed by a subsequent secondary ageing  cycle.  Further,  the  mean  gamma  prime size  calculated  using  Image-Pro  coupled with  a  probability  density  function  for the mean  size  showed  significant  γ′  coarsening. Different temperatures and holding times also allowed for significant growth of secondary gamma prime structures.  These structures were found to impact the mean gamma prime size calculations significantly with their influence on the mechanical properties remaining unknown.  However, the mean gamma prime size remains similar to what was desired. / En av de viktigaste energikällorna i denna moderna värld är gasturbinen. De når extremt höga arbetstemperaturer vid toppkapacitet och kräver därför material som klarar av den höga temperaturen. Nickelbaserade superlegeringar har använts i stor utsträckning som material på grund av deras olika högtemperaturegenskaper, som hjälper till att skydda dem från oxidation, korrosion och krypning. Denna högtemperaturs hållfasthet uppnås från gamma prim-fasen (γ′) för de flesta nickelbaserade legeringar. Denna studie handlarom att förstå effekten av den genomsnittliga γ′-fasstorleken som påverkas av olika tider och temperaturer. Olika legeringar har genomgått olika primära åldringscykler, följt av en sekundär åldringscykel. Vidare visade den genomsnittliga gamma-prim storleken som beräknades med Image-Pro tillsammans med en sannolikhets densitetfunktion för medelstorleken av γ′ förgrovning. Olika temperaturer och hålltider möjliggjorde också betydande tillväxt av sekundära gamma-primstrukturer. Dessa strukturer visade sig påverka beräkningarna av den genomsnittliga gamma-primstorleken och egenskaperna av de mekaniska egenskaperna förblir okända. Den genomsnittliga gamma-primstorleken blir liknande det som var önskvärt.

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In sub-millimeter sheets of wrought H-X750 Nickel-base superalloy, aluminum-rich coatings are bonded to matrix with a vapor phase aluminization process. If an appropriate amount of aluminum is bonded to matrix with homogenization treatment, the resulting diffusion couple will diffuse into coherent (g/g’) heterogeneous phases creating matrix that is both precipitation and solid solution strengthened. The diffusional mechanisms for solid solution mass transport involved with the growth and dispersion of bonded aluminum-rich coatings in the aluminization process only differ from the no external mass flow homogenization process with annealing treatment in that the boundary conditions are different. In each case these forces that activate diffusion at the macroscopic level are connected to the activation energies of random walks of atoms on a wide scale at the angstrom level. An overview of wrought Nickel-base superalloy is presented. Starting with thin sheets the alloy will be aluminized and homogenized. The research from this study will determine the parameters for the movement of the phase boundaries, mass transport, and the time variant concentration fields for both the aluminization and homogenization processes. This is predictable for both single dimension fluxes assuming the interdiffusivities and fluxes at the phase boundaries are known. Because mass-transport is related to the movement of the phase boundaries through density, an investigation into the less dense aluminum-rich coatings and resultant matrix is also included.

L'alliage N19 est un superalliage base nickel, élaboré par métallurgie des poudres, qui a été développé récemment en vue d'une application pour disques de turbine aéronautique. L'objectif de cette étude est d'optimiser la microstructure de cet alliage en agissant sur les paramètres de traitements thermiques pour améliorer les propriétés mécaniques de l'alliage. Une bonne compréhension des relations entre les paramètres de traitements thermiques et la microstructure, d'une part, et, des relations entre la microstructure et les propriétés mécaniques, d'autre part, est donc nécessaire. De nombreux traitements thermiques ont été appliqués à l'alliage N19 pour évaluer l'effet de la température de mise en solution, des conditions de refroidissement et de la température de revenu sur la taille de grains, et sur la taille et la distribution des précipités gamma prime. L'observation des microstructures en microscopie électronique à balayage et en transmission a permis d'évaluer l'effet des différentes étapes du traitement thermique sur les caractéristiques microstructurales de l'alliage. L'effet de ces modifications microstructurales sur la vitesse de propagation de fissure en fatigue-fluage à 650°C a été étudié. Les résultats de ces essais de propagation de fissure en fatigue-fluage ont été analysés à l'aide d'essais de comportement en fatigue-relaxation. Une synthèse des différentes propriétés mécaniques de l'alliage en fonction des paramètres de traitements thermiques et des caractéristiques microstructurales a été proposée. / The N19 alloy is a powder metallurgy nickel-based superalloy which has recently been developed for aircraft engine turbine disks. The aim of this study is to optimize the N19 microstructure through the adjustment of the heat treatment parameters in order to enhance the mechanical properties of this alloy. A good understanding of the relationships between the heat treatment parameters and the microstructure, and between the microstructure and the mechanical properties is required. Numerous heat treatments were applied to the alloy to investigate the effect of the solutionizing temperature, the cooling path, and the ageing temperature on the grain size, and on the gamma prime precipitates size and distribution. The observation of the microstructures using scanning electron microscopy and transmission electron microscopy supports the analysis of the heat treatment parameters effects on the microstructural features of the alloy. The effect of the microstructural modifications on the creep fatigue crack growth rate at 650°C was studied. The results of the creep fatigue crack growth tests were analyzed using cyclic stress-relaxation tests. A synthesis of the various mechanical properties of the alloy according to the heat treatment parameters and microstructural features is proposed.

<p>This master’s thesis work is a study of oxidation and degradation of nickel-base alloys at high temperatures. The materials studied are designed for use in critical gas turbine components such as turbine blades and vanes. Some of the alloys are used today, whereas others have not yet entered commercial application. In order to maximize the efficiency of gas turbines, there is an ambition to maximize the operating temperatures. There is therefore a demand for materials which can withstand the damage mechanisms active at high temperatures. Among these damage mechanisms are oxidation and microstructural degradation.</p><p>To investigate the oxidation resistance of 7 different monocrystalline and polycrystalline alloys, samples have been exposed isothermally in still air at temperatures between 850 and 1000°C, for exposure times of up to 20000h. Two of the alloys were also exposed cyclically at 950°C. Oxidation during the heat treatment resulted in significant weight changes, which were measured after each cycle for cyclically exposed samples and after completed heat treatment for isothermally exposed samples. The weight change data was used to evaluate the relative oxidation resistance of the alloys. The ranking of the alloys with respect to oxidation resistance was generally in agreement with the oxidation resistance predicted by a simple consideration of the Cr and Al contents of the alloys. However, the single-crystal alloy PWA1483 displayed better oxidation resistance than predicted from its chemical composition.</p><p>Metallographic analysis of the samples indicated that the oxide scales formed consisted of several different types of oxides. The oxide scales were mainly composed of Cr2O3 and Al2O3. Fragments of the oxide scales spalled off, primarily during cooling but also in some cases during the long-term heat treatments. Spalling of the oxide scale accelerated the oxidation process, since the ability of the oxide scale to impede diffusion decreased with its decrease in thickness. Oxidation caused depletion of Al and thereby local dissolution of the aluminum-rich γ′ particles, which are of vital importance to the mechanical properties of the material. A γ′ depleted zone thereby formed underneath the oxide scale. In this zone nitrides and needle-like particles, believed to be topologically close packed μ phase, precipitated during heat treatment. Recrystallization in the depletion zone was observed in some of the monocrystalline materials. MC carbides (M=metal) present in the virgin material decomposed during heat treatment and M23C6 carbides were formed. The γ′ particles coarsened during heat treatment, which resulted in decreased hardness. The hardness decreased with exposure temperature up to 950°C, as expected due to the increased coarsening rate. At 1000°C an unexpected increase in hardness was observed for all sample materials except one. A possible explanation for this hardness increase is redistribution of γ′, by dissolution of γ′ during heat treatment and reprecipitation during cooling as much finer particles. A fine dispersion of γ′ is expected to contribute more to the hardness than a corresponding volume of γ′ in the form of larger particles. For some of the sample series, clear correlations between hardness and γ′ particle size or exposition time were found. These relationships could potentially be used to estimate the exposure temperature of service-exposed material.</p><p>A numerical model was implemented in Matlab to describe the process of oxide growth and spalling, cycle by cycle. The model was successfully adapted to experimental data from the cyclic oxidation measurements. The general applicability of the model to cyclic oxidation data at different temperatures and cycle frequencies was not investigated. At long times of cyclic exposure, the net weight loss of the samples could be well approximated as a linear function of the number of cycles. However, during the last few cycles the amount of oxide spalled in each cycle suddenly decreased. This change in spallation behavior was mainly observed for the samples cooled in air between every cycle and to a much smaller extent for the samples cooled in water. The proposed explanation is that spalling occurred preferentially at a weak subscale interface and that the spalling propensity decreased with decreasing area of this weak interface. The deviating results of the last few cycles were not included in the modeling of the cyclic oxidation process.</p>

[pt] Este trabalho consiste na caracterização da fase gama linha em superligas de níquel através do processamento e análise digital de imagens. Amostras de uma superliga de níquel foram submetidas a 10 tratamentos térmicos diferentes. Após o tratamento térmico, estas amostras foram preparadas para avaliação metalográfica e imagens da microestrutura foram adquiridas no microscópio eletrônico de varredura (MEV). A fase gama linha presente no material foi segmentada e posteriormente medida através do processamento digital de imagens. Foram analisadas 429 imagens, o que gerou medidas de mais de 225,000 partículas. Foi medida a fração de área ocupada pelas partículas de gama linha, a quantidade de partículas por imagem, a área de cada partícula e a razão de aspectos das partículas. Uma análise estatística dos resultados foi realizada. Os resultados mostraram menor concentração e maior tamanho de gama linha com o aumento da temperatura, conforme era esperado. O uso de análise digital de imagens permitiu obter medidas com altíssima confiabilidade, uma vez que a alta velocidade de análise permite uma amostragem muito superior às técnicas tradicionais de caracterização microestrutural. / [en] This study consists of the characterization of the gamma prime phase in nickel base superalloys using digital image processing and analysis. Samples of a nickel base superalloy were heat treated to 10 different temperatures. After the heat treatment cycle, the samples were prepared for metallographic evaluation and images of the microstructure were acquired using a scanning electron microscope (SEM). The gamma prime was segmented and measured using digital image processing methods. 429 images were analyzed, in which over 225000 particles were measured. The following parameters were obtained: area fraction of gamma prime, number of particles of gamma prime per image, area of each particle and the particles' feret ratio. An statistical analysis of the data was performed The results showed that the gamma prime fraction decreases and its size increases with temperature increase, as expected. The use of digital image analysis provided measurements with high accuracy, as the high speed of digital image analysis allowed sampling much superior to the traditional microstructural characterization methods.

Nickel-base superalloys have been emerged as materials for gas turbines used for jet propulsion and electricity generation. The strength of the superalloys depends mainly from an ordered precipitates of L12 structure, so called gamma prime (γ’) dispersed within the disorder γ matrix. The Ni-base alloys investigated in this dissertation comprise both model alloy systems based on Ni-Al-Cr and Ni-Al-Co as well as the commercial alloy Rene N5. Classical nucleation and growth mechanism dominates the γ’ precipitation process in slowed-cooled Ni-Al-Cr alloys. The effect of Al and Cr additions on γ’ precipitate size distribution as well as morphological and compositional development of γ’ precipitates were characterized by coupling transmission electron microscopy (TEM) and 3D atom probe (3DAP) techniques. Rapid quenching Ni-Al-Cr alloy experiences a non-classical precipitation mechanism. Structural evolution of the γ’ precipitates formed and subsequent isothermal annealing at 600 °C were investigated by coupling TEM and synchrotron-based high-energy x-ray diffraction (XRD). Compositional evolution of the non-classically formed γ’ precipitates was determined by 3DAP and Langer, Bar-on and Miller (LBM) method. Besides homogeneous nucleation, the mechanism of heterogeneous γ’ precipitation involving a discontinuous precipitation mechanism, as a function of temperature, was the primary focus of study in case of the Ni-Al-Co alloy. This investigation coupled SEM, SEM-EBSD, TEM and 3DAP techniques. Lastly, solute partitioning and enrichment of minor refractory elements across/at the γ/ γ’ interfaces in the commercially used single crystal Rene N5 superalloy was investigated by using an advantage of nano-scale composition investigation of 3DAP technique.

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