Inconel alloys are commonly used as structural materials in nuclear reactors. One of these alloys, the Inconel X-750, is a γ’ Ni3(Al, Ti) strengthened superalloy extensively used in the cores of reactors, such as spacers in CANada Deuterium Uranium (CANDU) fuel channels. Prior to their application in commercial reactors, accelerated irradiation tests had been conducted in liquid metal fast reactors. Results did not indicate any problem stemming from significant fast neutron irradiation. However, recently it has been found that the ex-service CANDU Inconel X-750 spacers became severely brittle after a lengthy exposure to reactor environment. The underlying mechanism remains unclear and thus forms the focus of this current investigation, predominantly through transmission electron microscopy (TEM). This dissertation unfolds with the literature review in Chapter 2, followed by presentation of novel techniques in Chapter 3 on the preparation of TEM samples from small reactor components, namely the spacers. Chapter 4 presents TEM characterizations of ex-service spacers removed from the reactors. To simulate neutron irradiation over wide temperature range in an effort to understand the damage mechanisms, heavy ion irradiations were conducted and reported in Chapter 5 and 6. Irradiations are found to significantly alter the stability of the primary strengthening phase γ’, a systematic experimental study of which is presented in Chapter 7. To fully understand the effects of transmutation produced helium on irradiation induced cavity and dislocation microstructures, TEM in-situ heavy ion irradiations with hot/cold pre-injected helium were conducted and reported in Chapter 8 and 9. Helium was found to play an important role in the irradiation-induced instability of γ’ in nickel-based superalloys, the discussion of which is presented in Chapter 10. As one of the most important defect structures induced from irradiation, the stacking-fault-tetrahedra, were dynamically observed and are described in a journal manuscript in Appendix A. In addition to broadening current understanding of material degradation mechanism for in-service CANDU spacer, this study also provides comprehensive information on irradiation damage in nickel based superalloys, irradiation induced lattice defects and phase instability in face centered cubic alloys, as well as helium’s effects on cavity formation, dislocation evolution, and phase transformation. / Thesis (Ph.D, Mechanical and Materials Engineering) -- Queen's University, 2013-09-06 15:21:02.334

The aim of this master thesis project was to statistically correlate various powder characteristics to the quality of additively manufactured parts. An additional goal of this project was to find a potential second source supplier of powder for GKN Aerospace Sweden in Trollhättan. Five Inconel® alloy 718 powders from four individual powder suppliers have been analyzed in this project regarding powder characteristics such as: morphology, porosity, size distribution, flowability and bulk properties. One powder out of the five, Powder C, is currently used in production at GKN and functions as a reference. The five powders were additively manufactured by the process of laser metal deposition according to a pre-programmed model utilized at GKN Aerospace Sweden in Trollhättan. Five plates were produced per powder and each cut to obtain three area sections to analyze, giving a total of fifteen area sections per powder. The quality of deposited parts was assessed by means of their porosity content, powder efficiency, geometry and microstructure. The final step was to statistically evaluate the results through the analysis methods of Analysis of Variance (ANOVA) and simple linear regression with the software Minitab. The method of ANOVA found a statistical significant difference between the five powders regarding their experimental results. This made it possible to compare the five powders against each other. Statistical correlations by simple linear regression analysis were found between various powder characteristics and quality of deposited part. This led to the conclusion that GKN should consider additions to current powder material specification by powder characteristics such as: particle morphology, powder porosity and flowability measurements by a rheometer. One powder was found to have the potential of becoming a second source supplier to GKN, namely Powder A. Powder A had overall good powder properties such as smooth and spherical particles, high particle density at 99,94% and good flowability. The deposited parts with Powder A also showed the lowest amount of pores compared to Powder C, a total of 78 in all five plates, and sufficient powder efficiency at 81,6%.

Microstructure controls many physical properties of a material such as strength, ductility, 1density, conductivity, which, in turn, determine the application of these materials. This thesis work focuses on studying microstructural features (such as grain size, shape, defects, orientation gradients) and mechanical properties (such as hardness and yield strength) of multilayered materials that have undergone different loading and/or operating conditions. Two materials that are studied in detail are 18 nm Cu-Nb nanolaminates and 3D printed Inconel 718. Copper-Niobium (Cu-Nb) nanolaminate is a highly stable, high strength, nuclear irradiation resistant composite, which is destabilized with application of high pressure torsion (HPT). This work focuses on understanding the deformation and failure behavior of Cu-Nb using a novel orientation mapping technique in transmission electron microscopy in (TEM) called Automated Crystal Orientation Mapping (ACOM) and Digistar (ASTARTM) or Precession Electron Diffraction (PED). A new theory is postulated to explain strengthening mechanisms at the nanoscale using a data analytics approach. In-situ TEM compression and tensile testing is performed to image dislocation movement with the application of strain. This experiment was performed by Dr. Lakshmi Narayan Ramasubramanian at Xi’an Jiaotong University in China. Another major aspect of this research focuses on the design, fabrication, and microstructural characterization of 3D printed Inconel 718 heat exchangers. Various heat exchanger designs, machine resolution, printing techniques such as build orientation, power, and velocity of the laser beam are explored. Microstructural and mechanical properties of printed parts (before and after heat treatment) are then analyzed to check consistency in grain size, shape, porosity, hardness in relation to build height, scan parameters, and design. Various tools have been utilized such as scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), x-ray computed microtomography (at Advanced Photon Source at Argonne National Lab), hardness and micro-pillar compression testing for this study.

Orientador: Vicente Afonso Ventrella / Resumo: O presente trabalho consistiu em uma análise da influência da adição de elementos gamagênicos, estabilizadores da austenita, no processo de união autógena do aço superduplex UNS S32750, soldados com Laser Pulsado Nd:YAG. Os corpos de prova foram soldados utilizando duas técnicas: introdução de nitrogênio gasoso na atmosfera protetora, e adição de uma liga de níquel (Inconel 625 e Hastelloy C-276) na junta a ser soldada, tendo-se como objetivo a avaliação das propriedades mecânicas e microestruturais da junta soldada, como microdureza e tração. Todos os dados foram obtidos nos laboratórios da área de Materiais e Processos de Fabricação e no Laboratório de Soldagem da UNESP – Universidade Estadual Paulista Júlio de Mesquita Filho, Campus de Ilha Solteira, SP. O processo de soldagem foi realizado com a máquina de solda a laser UW 150A. Para a revelação dos detalhes dos cordões de solda foi utilizado o reagente Behara modificado. As medidas geométricas dos cordões de solda, como largura e profundidade, foram realizadas no microscópio Estéreo Zeiss Discovery V8. O MEV (Microscópio Eletrônico de Varredura) foi utilizado para a obtenção dos detalhes microscópicos dos cordões de solda. Os ensaios de tração foram realizados na Máquina Universal de Ensaios, e os valores de microdureza Vickers foram obtidos com o apoio do ultramicrodurômetro digital Shimadzu, modelo DUH 211S. Os resultados da microdureza Vickers, e dos ensaios de tração, nos corpos de prova obtidos com o uso dos gases d... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The present work consisted in an analysis of the influence of the addition of gamma - genic elements, stabilizers of austenite, in the process of autogenous union of the superduplex steel UNS S32750, welded with Nd: YAG Pulsed Laser. The specimens were welded using two techniques: introduction of gaseous nitrogen into the protective atmosphere and addition of a nickel alloy (Inconel 625 and Hastelloy C-276) in the joint to be welded, with the objective of evaluating the mechanical properties and microstructural weld joints, such as microhardness and tensile strength. All data were obtained from laboratories in the area of Materials and Processes of Manufacture and at the Welding Laboratory of UNESP - Paulista State University Júlio de Mesquita Filho, Campus de Ilha Solteira, SP. The welding process was performed with the UW 150A laser welding machine. For the development of details of the weld beads, the modified Behara reagent was used. The geometric measurements of the weld beads, such as width and depth, were performed on the Zeiss Discovery V8 Stereo Microscope. SEM (Scanning Electron Microscope) was used to obtain the microscopic details of the weld beads. The tensile tests were performed in the Universal Testing Machine, and the Vickers microhardness values were obtained with the support of the Shimadzu digital ultramicrodurometer, model DUH 211S. The results of the Vickers microhardness and the tensile tests on the specimens obtained with the protection gases Argon and... (Complete abstract click electronic access below) / Mestre

As ligas a base de Níquel são frequentemente utilizadas na indústria do petróleo devido à elevada resistência mecânica e excelente resistência à corrosão. Neste cenário, a utilização da soldagem como etapa na fabricação de dutos rígidos de grande comprimento é inevitável. Assim, chapas da liga Inconel 625® foram unidas através do processo Friction Stir Welding (FSW). A soldagem foi executada com uma ferramenta de nitreto cúbico de boro policristalino e o inerente desta ferramenta foi analisado. Em um primeiro momento, na seleção de parâmetros de processo, diversas condições de processo foram analisadas para escolha da melhor solda. Após esta etapa, novas juntas soldadas foram produzidas com o parâmetro de processo adequado (velocidade de rotação da ferramenta de 200 rpm e velocidade de avanço de 1 mm/s). A caracterização da superfície de topo da solda foi realizada através da microscopia ótica, microscopia eletrônica de varredura, microdureza e ensaios de dobramento. Defeitos superficiais foram inspecionados com líquidos penetrantes. Além disso, os estados de tensões residuais foram obtidos com a difração de raios-X. Ainda, a resistência à corrosão localizada foi estudada com o ensaio de imersão em cloreto férrico e a determinação da temperatura crítica de pite (conhecida como CPT) Por fim, a susceptibilidade à corrosão intergranular foi avaliada com o ensaio Streicher Test. O processo de soldagem promoveu o refino de grão e o aumento de dureza na solda. As micrografias do metal de base (MB) mostraram carbonetos do tipo MC, M6C, M23C6. Por outro lado, a melhor junta soldada apresentou uma microestrutura livre de defeitos, homogênea, onde não foram percebidos carbonetos do tipo M6C, M23C6 nos contornos de grão, foi aprovada nos ensaios de dobramento, líquidos penetrantes e imersão em FeCl3. Entretanto, ocorreu o um desgaste da ferramenta, mas reduzido e aceitável para esta solda. Tensões residuais longitudinais trativas da ordem de 50 MPa foram observadas na zona de mistura. Considerando o valor médio, o MB alcançou uma CPT de 77 °C, enquanto no centro da solda a CPT foi de 86°C. A taxa de corrosão média alcançada após o ensaio de corrosão intergranular foi de 0,4406 mm/ano, valor que sugere uma boa qualidade da solda. / Nickel based alloys are often used in the oil and gas industry due to their great mechanical strenght as well as excelent corrosion resistance. In this scenario, welding as manufacturing step for long lenght rigid tubes is inevitable. Therefore, Inconel 625® sheets were joined by Friction Stir Welding (FSW). The welding was performed with a Polycrystalline Cubic Boron Nitride (pcBN) tool and the unavoidable tool wear was verified. At first, in the process parameter development step, different process conditions were analyzed for choosing the best welded joint. Afterwards, new welded joints were produced with the suitable process parameter (tool rotational speed of 200 rpm and welding speed of 1 mm/s). Top surface characterization of friction-stir-welded Inconel 625 was carried out by optical microscopy, scanning electron microscopy, microhardness and bending tests. Surface defects were verified by dye penetrant inspection (DPI). In addition, residual stress states were obtained by X-ray diffraction. Furthermore, localized corrosion resistance was studied by the immersion test in FeCl3 and the critical pitting temperature (CPT) determination. Finally, the susceptibility to intergranular corrosion was evaluated by Streicher Test. FSW process promoted grain refining as well as increased microhardness in the joint Base material micrographs showed different carbides as MC, M6C, M23C6. On the other hand, the best joint presented a sounds weld without defetcs, homogeneous microstructure, grain boundaries free of M6C, M23C6 carbides, approved in bending tests, DPI and the immersion test. However, a tool wear was also noted, but reduced and acceptable for this weld. Tensile longitudinal residual stresses of 50 MPa were observed in the stir zone. As an avarage, the base material CPT was 77 °C, while the CPT was 86 °C at the weld center. The mean corrosion rate after intergranular corrosion test was 0.4406 mm/year, a value which suggests a good weld quality.

As superligas de níquel apresentam boa combinação de resistência à corrosão e à oxidação, resistência mecânica, resistência à fadiga e resistência à fluência. Além disso, apresentam bom desempenho operacional em temperaturas próximas à temperatura de fusão da liga. Estudos apontam à possibilidade de se obter aço carbono revestido com a superliga de níquel Inconel 625 pelo processo de cladeamento e pelo processo de aspersão térmica. A presença de molibdênio na composição química do Inconel625 garante excelente resistência à corrosão por pites e por fresta, enquanto o nióbio confere alta soldabilidade e resistência à corrosão intergranular a essas ligas. O processo de soldagem é amplamente usado em processos industriais e pode ser aplicado em uma junta Inconel-Inconel, podendo modificar alguma propriedade dessa liga. O objetivo do presente trabalho é estudar uma junta soldada de Inconel 625, obtida pelo processo de soldagem por fusão a arco elétrico com o uso de eletrodo revestido ENiCrMo-3, quanto à morfologia estrutural, à dureza e à resistência à corrosão. A morfologia foi avaliada por microscopia óptica, por microscopia eletrônica de varredura e por espectroscopia de energia dispersiva. A propriedade mecânica de dureza foi avaliada a partir do perfil de microdureza Vickers ao longo da junta soldada Para avaliar a resistência à corrosão da junta soldada foram realizados os ensaios de polarização potenciodinâmica, reativação potenciodinâmica de varredura cíclica (norma ASTM G108-94), polarização potenciodinâmica cíclica e ensaio de imersão (norma ASTM G48-03). Também avaliou-se a susceptibilidade à corrosão por pites pela norma ASTM G61-86 a temperatura ambiente e a 90 ºC. Para a polarização potenciodinâmica, três diferentes eletrólitos foram empregados: 3,5% NaCl, 3,5% NaCl + 0,01 mol/L Na2S2O3 e 3,5% NaCl + 1M H2SO4. Os resultados obtidos mostraram que o metal de solda apresenta uma microestrutura dendrítica com precipitados de Nb e de Mo nas regiões interdendríticas. O desempenho quanto à resistência à corrosão foi satisfatório nos meios estudados, considerando as características dessas ligas. No entanto, a junta soldada apresentou maior suscetibilidade à corrosão por pites e à corrosão localizada comparativamente ao metal base. O filme passivo formado no metal base é melhor constituído do que o filme passivo formado no metal de solda. / Nickel superalloys show a good combination of corrosion, oxidation and creep resistance as well as mechanical and fatigue strength. These alloys can operate at temperatures close to their melting temperature. The Inconel 625 has desired characteristics for application in environments that require high corrosion resistance, such as in oil and gas exploitation. Some studies show the possibility of obtaining a coating of Inconel 625 onto carbon steel by the cladding process and by the thermal spray process. The molybdenum content in Inconel 625 ensures excellent resistance to pitting and crevice, while the niobium content gives high weldability to these alloys. The welding process is practically present in all industrial plants, so an Inconel-Inconel joint is unavoidable. However, the welding can lead to changes in the properties of these superalloys. Therefore, the present work aims to study the structural morphology, hardness and corrosion resistance of a welded joint of Inconel 625 obtained by the electric arc fusion welding process with ENICrMo-3 covered electrode. The morphology was evaluated by optical microscopy, scanning electron microscopy and dispersive energy spectroscopy. Hardness was studied by Vickers microhardness profile along the welded joint. In order to evaluate the corrosion resistance of the welded joint, the Potentiodynamic polarization, potentiodynamic cyclic sweep reactivation (ASTM G108-94), cyclic potentiodynamic polarization and immersion test (ASTM G48-03) were performed Also susceptibility to pitting corrosion was assessed by ASTM G61-86 at room temperature and at 90 ° C. Potentiodynamic polarization curves were performed in three different solutions to evaluate the corrosion resistance: 3.5% NaCl, 3.5% NaCl + 0.01 mol / L Na2S2O3 and 3.5% NaCl + 1M H2SO4 The results show that the weld metal has a dendritic microstructure with precipitates of Nb and Mo in the interdendritic regions. The corrosion performance in environments close to the environments of possible applications was satisfactory considering the resistance of these alloys, but the specific welded joint was more susceptibility to corrosion by pits and localized corrosion. The passive film formed in the base metal was better formed than the passive film formed in the welded metal.

As technology advances, mechanical and electrical systems are subjugated to intense temperature fluctuations through their service life. Designing coatings that operate in extreme temperatures is, therefore, a continuing challenge within the tribology community. Silver tantalate was chosen for investigation at the atomic level, the physical and chemical properties that influence the thermal, mechanical, and tribological behavior for moving assemblies in high temperature tribological applications. By correlating behavior of internal physical processes to the macro tribological behavior, the tribological community will potentially gain improved predicative performance of solid lubricants in future investigations. Three different approaches were explored for the creation of such materials on Inconel substrates: (1) powders produced using a solid state which were burnished on the surface; (2) monolithic silver tantalate thin films deposited by magnetron sputtering; and, (3) an adaptive tantalum nitride/silver nanocomposite sputter-deposited coating that forms a lubricious silver tantalate oxide on its surface when operated at elevated temperatures. Dry sliding wear tests of the coatings against Si3N4 counterfaces revealed friction coefficients in the 0.06 - 0.15 range at T ~ 750 °C. Reduced friction coefficients were found in nanocomposite materials that contained primarily a AgTaO3 phase with a small amount of segregated Ag phase, as suggested by structural characterization using X-ray diffraction. The presence of nanoparticles of segregated Ag in the thin films further enhanced the performance of these materials by increasing their toughness. Additional characterization of the AgTaO3 films at 750 °C under normal loads of 1, 2, 5, or 10 N revealed that the friction monotonically increased as the load was increased. These results were complemented by molecular dynamics simulations, which confirmed the increase of friction with load. Further, the simulations support the hypothesis that this trend can be explained in terms of decreased presence of Ag clusters near the sliding surface and the associated decreased porosity. The results suggest that the relative amount of Ag in a TaN or Ta2O5 mastrix may be used to tune film performance for a given application.

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.

<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>