The goal of this work is to establish a life prediction methodology for thermomechanical loading of the Ni-base superalloy Mar-M247 over a larger temperature range than previous work. The work presented in this thesis extends the predictive capability of the Sehitoglu-Boismier unified thermo-viscoplasticity constitutive model and thermomechanical life model from a maximum temperature of 871C to a maximum temperature of 1038C. The constitutive model, which is suitable for predicting stress-strain history under thermomechanical loading, is adapted and calibrated using the response from isothermal cyclic experiments conducted at temperatures from 500C to 1038C at different strain rates with and without dwells. In the constitutive model, the flow rule function and parameters as well as the temperature dependence of the evolution equation for kinematic hardening are established. In the elevated temperature regime, creep and stress relaxation are critical behaviors captured by the constitutive model. The life model accounts for fatigue, creep, and environmental-fatigue damage under both isothermal and thermomechanical fatigue. At elevated temperatures, the damage terms must be calibrated to account for thermally activated damage mechanisms which change with increasing temperature. At lower temperatures and higher strain rates, fatigue damage dominates life prediction, while at higher temperatures and slower strain rates, environmental-fatigue and creep damage dominate life prediction. Under thermomechanical loading, both environmental-fatigue and creep damage depend strongly on the relative phasing of the thermal and mechanical strain rates, with environmental-fatigue damage dominating during out-of-phase thermomechanical loading and creep damage dominating in-phase thermomechanical loading. The coarse-grained polycrystalline microstructure of the alloy studied causes a significant variation in the elastic response, which can be linked to the crystallographic orientation of the large grains. This variation in the elastic response presents difficulties for both the constitutive and life models, which depend upon the assumption of an isotropic material. The extreme effects of a large grained microstructure on the life predictions is demonstrated, and a suitable modeling framework is proposed to account for these effects in future work.

In this research, controlled Waspaloy microstructures were produced with the objective of studying microstructural evolution in this alloy via electrically-based ac/dc non-destructive techniques. Correlations were developed between electrical measurements and alternate characterization techniques such as Ultra Small Angle X-ray Scattering (USAXS), Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) to gain a complete understanding of the microstructural transformations and the associated mechanisms. Three different sets of controlled microstructures were produced in this research. In Set I microstructures, matrix (gamma) grain sizes of 13, 52 and 89 micrometers were obtained after solution-treatments at 1045 and 176;C, 1090 and 176;C and 1145 and 176;C respectively. A vacancy stabilization treatment at 1045 and 176;C followed after which, the specimens were aged at 800 and 176;C for times ranging from 0.1 hrs to 100 hrs to vary the gamma prime precipitate size distribution. In Sets II and III, the solution-treatment was only conducted at 1145 and 176;C, with the stabilization treatment conducted only in Set II. Subsequently, aging experiments were conducted at 725 and 176;C (or 700 and 176;C in Set II), 800 and 176;C and 875 and 176;C for times up to 100 hrs. DC four-point probe resistivity of specimens increased to a maximum upon initial aging from the solution-treated condition and showed a decreasing trend thereafter with successive aging. This, in addition to complementary evidence from SEM and USAXS, led to the conclusion that gamma prime nucleation-growth was complete by the time the resistivity maximum was observed. Resistivity variations that ensued upon successive aging after the maximum were attributed to microstructural/compositional changes due to gamma prime coarsening. The height of the maximum decreased drastically with increase in aging temperature from 725 and 176;C to 800 and 176;C, while the resistivity did not increase from the solution-treated condition upon aging at 875 and 176; C. Coarsening studies based on USAXS analysis indicated an LSW type volume diffusion mechanism of coarsening in Waspaloy, with an average coarsening rate constant of 3.25x10-29 [m3/sec] for Set I specimens aged at 800 and 176;C. Analytical and Finite Element (FE) models of two-probe impedance and dc four-point probe resistivity methods were developed to gain insight into the measured response and the accurate determination of material properties. AFM-based localized electrical examination of sub-grain Waspaloy microstructures was successfully conducted using electrostatic force microscopy (EFM), scanning Kelvin probe microscopy (SKPM) and current-AFM (I-AFM) electrical modes. I-AFM experiments revealed that the conductivity of the gamma prime phase was lower than that of the gamma phase.

This thesis involves the development of digital algorithms for the microstructural analysis of metallic deposits produced through the use of Scanning Laser Epitaxy (SLE). SLE is a new direct digital manufacturing (DDM) technique which allows for the creation of three dimensional nickel-based superalloy components using an incremental layering system. Using a bed of powder placed on an underlying substrate and a laser propagating a melt-pool across the sample, a layer of material can be added and through the careful control of SLE settings various microstructures can be created or extended from the substrate. To create parts that are within specified microstructure tolerances the ideal SLE settings must be located through experimental runs, with each material needing different operating parameters. This thesis focuses on improving the microstructural analysis by use of a program that tracks various features found in samples produced through the SLE technique and a data analysis program that provides greater insights into how the SLE settings influence the microstructure. Using this program the isolation of optimal SLE settings is faster while also providing greater insights into the process than is currently possible. The microstructure recognition program features three key aspects. The first evaluates major characteristics that typically arise during the SLE process; such as sample deformation, the aspects of a single crystal deposit, and the total deposit height. The second saves the data and all relevant test settings in a format that will allow for future analysis and comparison to other samples. Finally, it features a robust yet rapid execution so it may be used for entire runs of SLE samples, which can number up to 25, within a week. The program is designed for the types of microstructure found in CMSX-4 and Rene-80, specifically single crystal and equiaxed regions. The data fitting program uses optimally piecewise-fitted equations to find relationships between the SLE settings and the microstructure traits. The data is optimally piecewise fitted as the SLE process is a two-stage procedure, establishing then propagating the melt-pool across a sample, which creates distinct microstructure transitions. Using the information gathered, graphs provide a visual aid to better allow the experimenter to understand the process and a DOE is performed using sequential analysis; allowing the previously run samples to influence the future trials, reducing the amount of materials used while still providing great insight into the parameter field. Having access to the microstructure data across the entire sample and an advanced data fitting program that can accurately relate them to the SLE settings allows the program to track and optimize features that were never before possible.

Thesis (M.S.)--Rutgers University, 2007. / "Graduate Program in Civil and Environmental Engineering." Includes bibliographical references (p. 74-76).

Aluminum (Al) and its alloys are widely used in various technological applications, mainly due to the excellent thermal conductivity, non-magnetic, ecofriendly, easy formability and good recyclability. However due to the inferior corrosion resistance its applications are hampered in various engineering sectors. Besides, the corrosion related failures such as leakage of gas from pipeline, catastrophic breakdown of bridges and fire accidents in processing plants further puts the human life in jeopardy. Within the United States over $ 400 billion dollars per year are spent over research to understand and prevent the corrosion related failures. Recently, the development of transition metal(TM) aluminides (AlxTMy, where, TM = Mo, W, Ta, Nb, Cr, Zr and V) has received the global attention mainly due to high strength at elevated temperatures, light-weight, excellent corrosion and wear resistance. In light of this, surface modification via laser surface alloying (LSA) is a promising engineering approach to mitigate the corrosion and wear problems. In the present study the attempts are made to study the Al-Mo, Al-W, Al-Nb, and Al-Ta systems as a potential corrosion resistant coatings on aluminum. The refractory metal (Mo, W, Nb, Ta) precursor deposit was spray coated separately on aluminum substrate and was subsequently surface alloyed using a continuous wave diode-pumped ytterbium laser at varying laser energy densities. Microstructural analysis was conducted using scanning electron microscopy and further X-ray diffractometry was carried out to evaluate the various phases evolved during laser surface alloying. Corrosion resistance of laser alloyed coatings were evaluated using open circuit potential, cyclic potentiodynamic polarization, electrochemical impedance spectroscopy measurements were performed in 0.6 M NaCl solution (pH:6.9±0.2, 23˚C). Open circuit potential measurements indicate the more stable (steady state) potential values over long periods after laser surface alloying. Cyclic polarization results indicated reduction in the corrosion current density, enhancement in the polarization resistance, and increase in coating/protective efficiency with increase in laser energy density compared to untreated aluminum. Electrochemical impedance spectroscopy measurements also indicated an increase in charge transfer resistance after laser surface alloying of refractory metals on aluminum. Additionally, first principle calculations of thermodynamic, electronic and elastic properties of intermetallics evolved during LSA were also thoroughly investigated to correlate the corrosion performance of intermetallic coatings with these properties. The present study indicates that novel Al-Mo, Al-W, Al-Nb, and Al-Ta intermetallics has a great potential for light weight structural applications with enhanced corrosion resistance.

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.

A study was done to determine the temperature and load interaction effects on the fatigue crack growth rate of polycrystalline superalloy IN100. Temperature interaction testing was performed by cycling between 316°C and 649°C in blocks of 1, 10 and 100 cycles. Load interaction testing in the form of single overloads was performed at 316°C and 649°C. After compiling a database of constant temperature, constant amplitude FCGR data for IN100, fatigue crack growth predictions assuming no load or temperature interactions were made. Experimental fatigue crack propagation data was then compared and contrasted with these predictions. Through the aid of scanning electron microscopy the fracture mechanisms observed during interaction testing were compared with the mechanisms present during constant temperature, constant amplitude testing. One block alternating temperature interaction testing grew significantly faster than the non-interaction prediction, while ten block alternating temperature interaction testing also grew faster but not to the same extent. One hundred block alternating testing grew slower than non-interaction predictions. It was found that as the number of alternating temperature cycles increased, changes in the gamma prime morphology (and hence deformation mode) caused changes in the environmental interactions thus demonstrating the sensitivity of the environmental interaction on the details of the deformation mode. SEM fractography was used to show that at low alternating cycles, 316°C crack growth was accelerated due to crack tip embrittlement caused by 649°C cycling. At higher alternating cycles the 316°C cycling quickly grew through the embrittled crack tip but then grew slower than expected due to the possible formation of Kear-Wilsdorf locks at 649°C. Overload interaction testing led to full crack retardation at 2.0x overloads for both 316°C and 649°C testing. 1.6x overloading at both temperatures led to retarded crack growth whereas 1.3x overloads at 649°C created accelerated crack growth and at 316°C the crack growth was retarded.

A model was created to predict the thermo-mechanical fatigue crack growth rates under typical engine spectrum loading conditions. This model serves as both a crack growth analysis tool to determine residual lifetime of ageing turbine components and as a design tool to assess the effects of temperature and loading variables on crack propagation. The material used in the development of this model was a polycrystalline superalloy, Inconel 100 (IN-100). The first step in creating a reliable model was to define the first order effects that influence TMF crack growth in a typical engine spectrum. Load interaction effects were determined to be major contributors to lifetime estimates by influencing crack growth rates based upon previous load histories. A yield zone model was modified to include temperature dependent properties that controlled the effects of crack growth retardation and acceleration based upon overloads and underloads, respectively. Multiple overload effects were included in the model to create enhanced retardation compared to single overload tests. Temperature interaction effects were also considered very important due to the wide temperature ranges of turbine engine components. Oxidation and changing temperature effects were accounted for by accelerating crack growth in regions that had been affected by higher temperatures. Constant amplitude crack growth rates were used as a baseline, upon which load and temperature interaction effects were applied. Experimental data of isolated first order effects was used to calibrate and verify the model. Experimental data provided the means to verify that the model was a good fit to experimental results. The load interaction effects were described by a yield zone model, which included temperature dependent properties. These properties were determined experimentally and were essential in the model's development to include load and temperature contributions. Other interesting factors became apparent through testing. It was seen that specific combinations of strain rate and temperature would lead to serrated yielding, discovered to be the Portevin-Le Chatelier effect. This effect manifested itself as enhanced hardening, leading to unstable strain bursts in specimens that cyclically yielded while changing temperature.

Inconel 718 is a high nickel content superalloy possessing high strength at elevated temperatures and resistance to oxidation and corrosion. The non-traditional manufacturing process of wire-electrical discharge machining (EDM) possesses many advantages over traditional machining during the manufacture of Inconel 718 parts. However, certain detrimental effects are also present. The top layer of the machined surface is melted and resolidified to form what is known as the recast layer. This layer demonstrates microstructural differences from the bulk workpiece, resulting in altered material properties. An experimental investigation was conducted to determine the main machining parameters which contribute to recast layer formation in wire-EDM of Inconel 718. It was found that average recast layer thickness increased with energy per spark, peak discharge current, current pulse duration, and open-voltage time and decreased with sparking frequency and table feed rate. Over the range of parameters tested, the recast layer was observed to be between 5 and 10 μm in average thickness, although highly variable in nature. Surface roughness of the cut parts showed an increase with energy per spark. Electron Probe Microanalysis (EPMA) revealed the recast layer to be alloyed with elements from the wire electrode. X-ray diffraction testing showed the residual tensile stresses evident near the cut surface to decrease with energy per spark. Additionally, nano-indentation hardness testing indicated that the recast layer is reduced in hardness and elastic modulus compared to the bulk material. Vibratory tumbling was found to be a moderately effective post-processing tool for recast layer removal when using pre-formed ceramic abrasive media or fine grained aluminum oxide.

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