A necessidade de trabalhos em altas temperaturas exige o desenvolvimento de materiais com elevada resistência química e mecânica em temperaturas que podem chegar próximas ao seu ponto de fusão. Em especial, os materiais empregados devem apresentar bom comportamento em fluência, de modo a suportar a combinação de altas tensões e altas temperaturas com o mínimo de deformação. O presente trabalho visa caracterizar a superliga MAR-M247, fornecida pela empresa Açotécnica, em condições de fluência para a produção de rotores empregados em turbocompressores automotivos. Os trabalhos são divididos em duas etapas. Na primeira estuda-se a melhor combinação de tratamentos térmicos de solubilização e envelhecimento, chegando à condição de solubilização por 5 horas a 1250?C e envelhecimento por 20 horas a 980?C. Um trabalho de outro aluno (SILVA, 2011) realiza o mesmo estudo para uma variação da superliga MAR-M247 em que o tântalo é totalmente substituído por nióbio. Neste caso, a melhor condição de tratamento é solubilização a 1260?C por 8 h seguida de envelhecimento duplo por 5 h a 880?C e 20 h a 780?C. Na segunda etapa, os materiais dos dois trabalhos, nas melhores condições de tratamento para cada um, são testados em condições de fluência a 850?C a 370, 390, 410 e 430 MPa. A superliga convencional apresenta os maiores valores de vida em fluência enquanto a modificada apresenta os maiores valores de ductilidade. A análise de fratura dos materiais ensaiados a 390 e 430 MPa mostra a presença massiva de carbonetos em toda a extensão da microestrutura, apresentando, em muitos casos, uma morfologia de \"escrita chinesa\". Apesar disso, todas as amostras apresentam grande quantidade de vazios, indicando que sua nucleação e crescimento são os responsáveis pela fratura do material. / The needing for high temperature work claim for new materials capable of maintain high strength and good corrosion resistance at temperatures that could reach values near their melting point. Such materials must be creep resistant to withstand high levels of tension and temperature. The aim of this work is the characterization of MAR-M247 under creep conditions for the production of automotive turbocharger rotors made by Açotécnica. The work is split in two steps. In the first one, the material is studied to find the best conditions for solution and ageing heat treatments. The result is a solution treatment at 1250?C for 5 h followed by aging at 980?C for 20 h. A work made by another student (SILVA, 2011) makes the same with a modification of MAR-M247 in which tantalum is completely substituted for niobium. The best condition for this case is a solution treatment at 1260?C for 8 h and a double aging treatment at 880?C for 5 h and 780?C for 20 h. At the second part of the work, both the materials are tested under creep conditions at 850?C with 370, 390, 410 and 430 MPa. The conventional superalloy shows the highest values for creep strength and the modified superalloy shows the highest ductility. Fracture surfaces for 390 and 430 MPa showed brittle carbides with \"chinese script\" morphology. Conversely, holes are present on all four materials what shall mean that its nucleation and growth was the most probably fracture path.

The increasing technological need to push service conditions of structural materials to higher temperatures has motivated the development of several alloy systems. Among them, superalloys are an excellent candidate for high temperature applications because of their ability to form coherent ordered precipitates, which enable the retention of high strength close to their melting temperature. The accelerated kinetics of solute diffusion, with or without an added component of mechanical stress, leads to coarsening of the precipitates, and results in microstructural degradation, limiting the durability of the materials. Hence, the coarsening of precipitates has been a classical research problem for these alloys in service. The prolonged hunt for an alternative of nickel base superalloys with superior traits has gained hope after the recent discovery of Co-Al-W based alloys, which readily form high temperature g precipitates, similar to Ni base superalloys. In the present study, coarsening behavior of g precipitates in Co-10Al-10W (at. %) has been carried out at 800°C and 900°C. This study has, for the first time, obtained critical coarsening parameters in cobalt-base alloys. Apart from this, it has incorporated atomic scale compositional information across the g/g interfaces into classical Cahn-Hilliard model for a better model of coarsening kinetics. The coarsening study of g precipitates in Ni-14Al-7 Cr (at. %) has shown the importance of temporal evolution of the compositional width of the g/g interfaces to the coarsening kinetics of g precipitates. This study has introduced a novel, reproducible characterization method of crystallographic study of ordered phase by coupling of orientation microscopy with atom probe tomography (APT). Along with the detailed analysis of field evaporation behaviors of Ni and Co superalloys in APT, the present study determines the site occupancy of various solutes within ordered g precipitates in both Ni and Co superalloys. This study has explained the role of structural and compositional gradients across the precipitates (g)/matrix (g) interfaces on the coarsening behavior of coherent precipitates in both Ni and Co-base superalloys. The observation of two interfacial widths, one corresponding to a structural order-disorder transition, and the other to the compositional transition across the interface, raises fundamental questions regarding the definition of the interfacial width in such systems. The comparative interface analysis in Co and Ni superalloy shows significant differences, which gives insights to the coarsening behaviors of g precipitates in these alloys. Hence, the principal goal of this work is to compare and contrast the Co and Ni superalloys and also, to accommodate atomic scale information related to transitions across interfaces to coarsening models for a better practical applicability of coarsening laws to various alloys.

Les assiettes de fibrage utilisées pour la production de fibres de verre subissent d’importantes contraintes mécaniques, chimiques et thermiques. Par conséquent, cette pièce se dégrade et doit être périodiquement remplacée. Le but de ces travaux est d’augmenter la durée de vie des assiettes de fibrage en améliorant les propriétés mécaniques et chimiques des superalliages qui les constituent. Plus précisément, l’objectif de cette thèse est, dans un premier temps, d’améliorer les alliages utilisés pour le fibrage à 1000°C, puis dans un second temps, de trouver un superalliage pouvant fibrer à 1125°C. Ces travaux ont été menés sur deux familles de superalliages : base nickel et base cobalt. Les propriétés chimiques ont été caractérisées par des essais thermogravimétriques et les propriétés mécaniques par des essais de fluage flexion 3 points. Pour l’alliage base Ni, l’influence des éléments minoritaires subis, Mn et Si, a été étudiée. Les propriétés mécaniques de cet alliage ont fait, ensuite, l’objet d’essais d’amélioration par l’addition de titane, zirconium, tantale, hafnium et de niobium. L’addition d’aluminium a été aussi expérimentée mais ayant pour but d’améliorer les propriétés chimiques de l’alliage. Enfin, des études ont été aussi menées sur l’addition de métaux nobles (Pd et Ru) et de terres rares (Y, La et Ce). Concernant les superalliages base cobalt, l’étude s’est portée sur un alliage base Co qui a antérieurement montré de bonnes propriétés générales pour une utilisation à 1125°C et non à 1000°C. Des variantes avec une teneur abaissée en tantale, sans hafnium et sans tungstène ont été étudiées. Pour clore ces travaux, l’augmentation de la teneur en nickel et un traitement thermique ont été étudiés afin d’améliorer la résistance à l’oxydation de ce second alliage / The fiberizing spinners used to produce the glass fibers undergo sizable mechanical, chemical and thermal solicitations. Therefore, this piece is degraded and must be periodically replaced. The purpose of these works is to increase the lifetime of the fiberizing spinners by improving the mechanical and chemical properties of the superalloys that constitute them. More precisely, the objective of this thesis is, in the first time, to improve the alloys used to fiberize at 1000°C, and in a second time, to find a superalloy that can fiberize at 1125°C. These works are focused on two families of superalloys: nickel-based and cobalt-based. The chemical properties are characterized by the thermogravimetry tests and the mechanical properties by 3 points flexural creep tests. For the Ni-based alloy, the influences of unwanted minority elements, Mn and Si, were studied. The mechanical properties of this alloy are subject to improvement tests by the addition titanium, zirconium, tantalum, hafnium and niobium. The aluminium addition was also experimented but with the aim of improving the chemical properties of the alloy. Finally, the studies were also driven on the addition of noble metals (Pd and Ru) and of rare earths (Y, La and Ce). Concerning the cobalt-based superalloys, the study focused on an alloy which has previously shown good general properties to be used at 1125°C and no at 1000°C. The versius with a lowered content in tantalum, without tungsten and without hafnium were studied. To close this work, the increase of nickel and a heat treatment were studied in order to improve the oxidation resistance of this second alloy

Superligas à base de níquel vêm sendo extensivamente utilizadas em diversas aplicações nas indústrias devido ao excelente comportamento mecânico e anticorrosivo. No entanto, essas ligas possuem certas particularidades que levam à necessidade de desenvolvimento de técnicas de inspeção e caracterização metalúrgica, como forma de garantir a integridade estrutural dos componentes fabricados com essas ligas. Neste trabalho, a técnica de correntes parasitas foi aplicada à superligas à base de níquel com duas propostas distintas: 1) Em um primeiro momento foi realizado o estudo da evolução microestrutural da liga Inconel 718 durante o processo de envelhecimento através da combinação do ensaio por correntes parasitas, análise de difração de raios-X, análise metalográfica, medidas de dureza e tamanho de grão. As medidas foram realizadas em amostras submetidas a diferentes ciclos de tratamentos térmicos variando entre 620-1035°C. Os resultados mostraram que as diferentes microestruturas do Inconel 718 têm efeitos distintos na condutividade elétrica quando medidos através da técnica de correntes parasitas. A influência da microestrutura na condutividade pode ser mostrada sendo devido à competição de dois efeitos sobre o espalhamento de elétrons: a purificação da matriz e a morfologia, distribuição e tamanho dos precipitados. A combinação dos valores de dureza e condutividade elétrica provou ser uma forma rápida e prática de determinar o nível de envelhecimento da liga; 2) Em um segundo momento foi desenvolvido um processo de otimização de sensores através de modelagem por elementos finitos (MEF). Através de uma metodologia de otimização, os parâmetros de construção e operação de um sensor foram otimizados para inspeção de defeitos superficiais e subsuperficiais esperados em materiais cladeados com Inconel 625. O sensor com a geometria ótima foi construído e testado a fim de verificar a eficiência do processo de otimização. Uma ótima correlação entre os resultados numéricos e experimentais foi encontrada e o sensor ótimo se mostrou eficiente na inspeção de pequenos defeitos superficiais e subsuperficiais na liga Inconel 625 quando operado nas frequências apropriadas. / Nickel-based superalloys have been extensively used in various industries due to its unique mechanical and corrosion behavior. However, these alloys show particular characteristics which lead to the need for specific inspection and metallurgical characterization techniques in order to ensure the structural integrity of components manufactured from these alloys. In this work , the eddy current technique was applied to nickel-base superalloys with two aims: 1 ) Firstly, the microstructural evolution of Inconel 718 during aging processes has been studied through a combination of eddy current testing, X-ray diffraction analysis, metallography, hardness and grain size measurements. Measurements were carried out in samples subjected to different heat treatment cycles between 620-1035°C. Results show that different microstructures of Inconel 718 have a distinguishable effect on electrical conductivity when this is measured through an appropriately sensitive technique (i.e. eddy current testing). The influence of microstructure on conductivity could be shown to be due to the competition between two effects on the scattering of electrons: matrix purification and precipitate size, distribution and morphology. A combination of hardness values and electrical properties proved to be a fast and practical way of determining the stage of aging of the alloy; 2) An optimization method of eddy current sensor design was developed through finite element modeling (FEM). Through a methodology of optimization, the construction and operation parameters of the sensor were optimized for inspection of superficial and subsuperficial defect, commonly found in weld overlay Inconel 625 claddings. A prototype of this sensor with the optimum geometry was built and tested on blocks identical to those considered in the models in order to verify the efficiency of the optimization process. A very good agreement between numerical and experimental results was found. Moreover, the optimal sensor was efficient to detect small surface and subsurface defects in Inconel 625 when operated at appropriate frequencies.

In this licentiate thesis the work done in the TURBO POWER project Influence of high temperature hold times on the fatigue life of nickel-based superalloys will be presented. The overall objective of this project is to develop and evaluate tools for designing against fatigue in gas turbine applications, with special focus on the nickel-based superalloy Inconel 718. Firstly, the constitutive behaviour of the material has been been studied, where focus has been placed on trying to describe the mean stress relaxation and initial softening of the material under intermediate temperatures. Secondly, the fatigue crack propagation behaviour under high temperature hold times has been studied. Focus has here been placed on investigating the main fatigue crack propagation phenomena with the aim of setting up a basis for fatigue crack propagation modelling. This thesis is divided into two parts. The first part describes the general framework, including basic constitutive and fatigue crack propagation behaviour as well as a theoretical background for the constitutive modelling of mean stress relaxation. This framework is then used in the second part, which consists of the four included papers.

This thesis deals with the heat evolution duringsolidification and its relation to the formation of porosity.It intends to improve the current understanding of theformation of porosity in cast materials with special interestin nodular cast iron and the spray forming process. Twodifferent systems, a Fe-based alloy, Cast iron, and a Ni-basedalloy, Inconel 625, are examined. The effect on the heatevolution of the morphology and the processing parameters inspray forming are treated. An evaluation of the microstructural features, segregationbehavior and physical properties such as latent heat of fusionis performed byusing thermal analysis under cooling ratesranging from 0.1 to 104 K/s. In order to achieve this amodified differential thermal analysis (DTA) equipment, amirror furnace and levitation casting are used. Results arepresented in terms of the fraction of solidified, the coolingrate and the microstructure observed. The measured latent heatof fusion is not constant throughout the solidificationprocess. Variations in morphology and cooling rate affect therelease of the latent heat. A thermodynamic model is used to describe the experimentalobservations and to explain the formation of pores in nodularcast iron by taking into consideration the formation of latticedefects during the liquid/solid transformation. In this casethe formation of porosity is regarded as a consequence ofchanges in the volume fraction ratio graphite/ during thesolidification process. A numerical model of the spray forming process is developedby means of CFD modelling and compared with experimentalmeasurements performed in an industrial facility. Stagnationpressure measurements provided information about the gas flowvelocity and an analysis of the overspray powder providedinformation about the particle thermal history. Evaluation ofthe deposit was also performed. It is observed that the processconditions in spray forming promote non-equilibriumsolidification even though solidification at the deposit occursat a lower rate. In this case the porosity formed near theinterface substrate/deposit depends largely on the substratetemperature. The presence of certain reactive elements, such astitanium, affects the porosity levels in the rest of thedeposit. <b>Keywords:</b>Thermal Analysis, Nodular Cast Iron, Inconel625, CFD, Flow Assesment, Multiphase Flow, Spray Deposition,Microporosity, Superalloys

In this master thesis, work done in the TURBO POWER project High temperature fatigue crack propagation in nickel-based superalloys during spring 2012 will be presented. The overall objective of this project is to develop and evaluate tools for designing against fatigue in gas turbine applications, with special focus on the crack propagation in the nickel-based superalloy Inconel 718. Experiments have been performed to study the effect of initial overloads, and it has been shown that even for small initial overloads a significant reduction of the crack growth rate is received. Furthermore, FE simulations have been carried out in order to describe the local stress state in front of the crack tip since it is believed to control, at least partly the diffusion of oxygen into the crack tip and thus also the hold time crack growth behaviour of the material. Finally, an evaluation method for the stresses is presented, where the results are averaged over an identifiable process/damaged zone in front of the crack tip.

Engineers constantly seek advancements in the performance of aircraft and power generation engines, including, lower costs and emissions, and improved fuel efficiency. Nickel-base superalloys are the material of choice for turbine discs, which experience some of the highest temperatures and stresses in the engine. Engine performance is proportional to operating temperatures. Consequently, the high-temperature capabilities of disc materials limit the performance of gas-turbine engines. Therefore, any improvements to engine performance necessitate improved alloy performance. In order to take advantage of improvements in high-temperature capabilities through tailoring of alloy microstructure, the overall objectives of this work were to establish relationships between alloy processing and microstructure, and between microstructure and mechanical properties. In addition, the project aimed to demonstrate the applicability of neural network modeling to the field of Ni-base disc alloy development and behavior. A full program of heat-treatment, microstructural quantification, mechanical testing, and neural network modeling was successfully applied to next generation Ni-base disc alloys. Mechanical testing included hot tensile, hot hardness, creep deformation, creep crack growth, and fatigue crack growth. From this work the mechanisms of processing-structure and structure-property relationships were studied. Further, testing results were used to demonstrate the applicability of machine-learning techniques to the development and optimization of this family of superalloys.

Nickel-base superalloys obtain high temperature mechanical properties through formation of precipitate phases formed via heat treatment. The precipitate microstructure evolves with heat treatment or thermal exposure, which can lead to degrading mechanical properties. This project focuses on the use of electrical resistivity as a non-destructive testing method to monitor the precipitate phase in Waspaloy (a polycrystalline nickel-base superalloy). The evolution of the precipitate microstructure is characterized throughout the volume of the specimens using both small angle neutron scattering (SANS) and ultra small angle X-ray scattering (USAXS) measurements. These measurements are also aided by microscopy and X-ray diffraction measurements.

<p>This thesis deals with the heat evolution duringsolidification and its relation to the formation of porosity.It intends to improve the current understanding of theformation of porosity in cast materials with special interestin nodular cast iron and the spray forming process. Twodifferent systems, a Fe-based alloy, Cast iron, and a Ni-basedalloy, Inconel 625, are examined. The effect on the heatevolution of the morphology and the processing parameters inspray forming are treated.</p><p>An evaluation of the microstructural features, segregationbehavior and physical properties such as latent heat of fusionis performed byusing thermal analysis under cooling ratesranging from 0.1 to 104 K/s. In order to achieve this amodified differential thermal analysis (DTA) equipment, amirror furnace and levitation casting are used. Results arepresented in terms of the fraction of solidified, the coolingrate and the microstructure observed. The measured latent heatof fusion is not constant throughout the solidificationprocess. Variations in morphology and cooling rate affect therelease of the latent heat.</p><p>A thermodynamic model is used to describe the experimentalobservations and to explain the formation of pores in nodularcast iron by taking into consideration the formation of latticedefects during the liquid/solid transformation. In this casethe formation of porosity is regarded as a consequence ofchanges in the volume fraction ratio graphite/ during thesolidification process.</p><p>A numerical model of the spray forming process is developedby means of CFD modelling and compared with experimentalmeasurements performed in an industrial facility. Stagnationpressure measurements provided information about the gas flowvelocity and an analysis of the overspray powder providedinformation about the particle thermal history. Evaluation ofthe deposit was also performed. It is observed that the processconditions in spray forming promote non-equilibriumsolidification even though solidification at the deposit occursat a lower rate. In this case the porosity formed near theinterface substrate/deposit depends largely on the substratetemperature. The presence of certain reactive elements, such astitanium, affects the porosity levels in the rest of thedeposit.</p><p><b>Keywords:</b>Thermal Analysis, Nodular Cast Iron, Inconel625, CFD, Flow Assesment, Multiphase Flow, Spray Deposition,Microporosity, Superalloys</p>