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Description
Nanocrystalline (NC) and Ultrafine-grained (UFG) metal films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. These properties, such as very high strength, primarily arise from the change in the underlying deformation mechanisms. Experimental and simulation studies have shown that because of the small grain size,

Nanocrystalline (NC) and Ultrafine-grained (UFG) metal films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. These properties, such as very high strength, primarily arise from the change in the underlying deformation mechanisms. Experimental and simulation studies have shown that because of the small grain size, conventional dislocation plasticity is curtailed in these materials and grain boundary mediated mechanisms become more important. Although the deformation behavior and the underlying mechanisms in these materials have been investigated in depth, relatively little attention has been focused on the inhomogeneous nature of their microstructure (particularly originating from the texture of the film) and its influence on their macroscopic response. Furthermore, the rate dependency of mechanical response in NC/UFG metal films with different textures has not been systematically investigated. The objectives of this dissertation are two-fold.

The first objective is to carry out a systematic investigation of the mechanical behavior of NC/UFG thin films with different textures under different loading rates. This includes a novel approach to study the effect of texture-induced plastic anisotropy on mechanical behavior of the films. Efforts are made to correlate the behavior of UFG metal films and the underlying deformation mechanisms. The second objective is to understand the deformation mechanisms of UFG aluminum films using in-situ transmission electron microscopy (TEM) experiments with Automated Crystal Orientation Mapping. This technique enables us to investigate grain rotations in UFG Al films and to monitor the microstructural changes in these films during deformation, thereby revealing detailed information about the deformation mechanisms prevalent in UFG metal films.
ContributorsIzadi, Ehsan (Author) / Rajagopalan, Jagannathan (Thesis advisor) / Peralta, Pedro (Committee member) / Chawla, Nikhilesh (Committee member) / Solanki, Kiran (Committee member) / Oswald, Jay (Committee member) / Arizona State University (Publisher)
Created2017
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Description
The Very High Temperature Reactor (VHTR) is one of six conceptual designs proposed for Generation IV nuclear reactors. Alloy 617, a solid solution strengthened Ni-base superalloy, is currently the primary candidate material for the tubing of the Intermediate Heat Exchanger (IHX) in the VHTR design. Steady-state operation of the nuclear

The Very High Temperature Reactor (VHTR) is one of six conceptual designs proposed for Generation IV nuclear reactors. Alloy 617, a solid solution strengthened Ni-base superalloy, is currently the primary candidate material for the tubing of the Intermediate Heat Exchanger (IHX) in the VHTR design. Steady-state operation of the nuclear power plant at elevated temperatures leads to creep deformation, whereas loading transients including startup and shutdown generate fatigue. A detailed understanding of the creep-fatigue interaction in Alloy 617 is necessary before it can be considered as a material for nuclear construction in ASME Boiler and Pressure Vessel Code. Current design codes for components undergoing creep-fatigue interaction at elevated temperatures require creep-fatigue testing data covering the entire range from fatigue-dominant to creep-dominant loading. Classical strain-controlled tests, which produce stress relaxation during the hold period, show a saturation in cycle life with increasing hold periods due to the rapid stress-relaxation of Alloy 617 at high temperatures. Therefore, applying longer hold time in these tests cannot generate creep-dominated failure. In this study, uniaxial isothermal creep-fatigue tests with non-traditional loading waveforms were designed and performed at 850 and 950°C, with an objective of generating test data in the creep-dominant regime. The new loading waveforms are hybrid strain-controlled and force-controlled testing which avoid stress relaxation during the creep hold. The experimental data showed varying proportions of creep and fatigue damage, and provided evidence for the inadequacy of the widely-used time fraction rule for estimating creep damage under creep-fatigue conditions. Micro-scale damage features in failed test specimens, such as fatigue cracks and creep voids, were quantified using a Scanning Electron Microscope (SEM) to find a correlation between creep and fatigue damage. Quantitative statistical imaging analysis showed that the microstructural damage features (cracks and voids) are correlated with a new mechanical driving force parameter. The results from this image-based damage analysis were used to develop a phenomenological life-prediction methodology called the effective time fraction approach. Finally, the constitutive creep-fatigue response of the material at 950°C was modeled using a unified viscoplastic model coupled with a damage accumulation model. The simulation results were used to validate an energy-based constitutive life-prediction model, as a mechanistic model for potential component and structure level creep-fatigue analysis.
ContributorsTahir, Fraaz (Author) / Liu, Yongming (Thesis advisor) / Jiang, Hanqing (Committee member) / Rajagopalan, Jagannathan (Committee member) / Oswald, Jay (Committee member) / Jiao, Yang (Committee member) / Arizona State University (Publisher)
Created2017
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Description
Interstitial impurity atoms can significantly alter the chemical and physical properties of the host material. Oxygen impurity in HCP titanium is known to have a considerable strengthening effect mainly through interactions with dislocations. To better understand such an effect, first the role of oxygen on various slip planes in titanium

Interstitial impurity atoms can significantly alter the chemical and physical properties of the host material. Oxygen impurity in HCP titanium is known to have a considerable strengthening effect mainly through interactions with dislocations. To better understand such an effect, first the role of oxygen on various slip planes in titanium is examined using generalized stacking fault energies (GSFE) computed by the first principles calculations. It is shown that oxygen can significantly increase the energy barrier to dislocation motion on most of the studied slip planes. Then the Peierls-Nabbaro model is utilized in conjunction with the GSFE to estimate the Peierls stress ratios for different slip systems. Using such information along with a set of tension and compression experiments, the parameters of a continuum scale crystal plasticity model, namely CRSS values, are calibrated. Effect of oxygen content on the macroscopic stress-strain response is further investigated through experiments on oxygen-boosted samples at room temperature. It is demonstrated that the crystal plasticity model can very well capture the effect of oxygen content on the global response of the samples. It is also revealed that oxygen promotes the slip activity on the pyramidal planes.

The effect of oxygen impurity on titanium is further investigated under high cycle fatigue loading. For that purpose, a two-step hierarchical crystal plasticity for fatigue predictions is presented. Fatigue indicator parameter is used as the main driving force in an energy-based crack nucleation model. To calculate the FIPs, high-resolution full-field crystal plasticity simulations are carried out using a spectral solver. A nucleation model is proposed and calibrated by the fatigue experimental data for notched titanium samples with different oxygen contents and under two load ratios. Overall, it is shown that the presented approach is capable of predicting the high cycle fatigue nucleation time. Moreover, qualitative predictions of microstructurally small crack growth rates are provided. The multi-scale methodology presented here can be extended to other material systems to facilitate a better understanding of the fundamental deformation mechanisms, and to effectively implement such knowledge in mesoscale-macroscale investigations.
ContributorsGholami Bazehhour, Benyamin (Author) / Solanki, Kiran N (Thesis advisor) / Liu, Yongming (Committee member) / Oswald, Jay J (Committee member) / Rajagopalan, Jagannathan (Committee member) / Jiao, Yang (Committee member) / Arizona State University (Publisher)
Created2018
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Description
Increasing density of microelectronic packages, results in an increase in thermal and mechanical stresses within the various layers of the package. To accommodate the high-performance demands, the materials used in the electronic package would also require improvement. Specifically, the damage that often occurs in solders that function as die-attachment and

Increasing density of microelectronic packages, results in an increase in thermal and mechanical stresses within the various layers of the package. To accommodate the high-performance demands, the materials used in the electronic package would also require improvement. Specifically, the damage that often occurs in solders that function as die-attachment and thermal interfaces need to be addressed. This work evaluates and characterizes thermo-mechanical damage in two material systems – Electroplated Tin and Sintered Nano-Silver solder.

Tin plated electrical contacts are prone to formation of single crystalline tin whiskers which can cause short circuiting. A mechanistic model of their formation, evolution and microstructural influence is still not fully understood. In this work, growth of mechanically induced tin whiskers/hillocks is studied using in situ Nano-indentation and Electron Backscatter Diffraction (EBSD). Electroplated tin was indented and monitored in vacuum to study growth of hillocks without the influence of atmosphere. Thermal aging was done to study the effect of intermetallic compounds. Grain orientation of the hillocks and the plastically deformed region surrounding the indent was studied using Focused Ion Beam (FIB) lift-out technique. In addition, micropillars were milled on the surface of electroplated Sn using FIB to evaluate the yield strength and its relation to Sn grain size.

High operating temperature power electronics use wide band-gap semiconductor devices (Silicon Carbide/Gallium Nitride). The operating temperature of these devices can exceed 250oC, preventing use of traditional Sn-solders as Thermal Interface materials (TIM). At high temperature, the thermomechanical stresses can severely degrade the reliability and life of the device. In this light, new non-destructive approach is needed to understand the damage mechanism when subjected to reliability tests such as thermal cycling. In this work, sintered nano-Silver was identified as a promising high temperature TIM. Sintered nano-Silver samples were fabricated and their shear strength was evaluated. Thermal cycling tests were conducted and damage evolution was characterized using a lab scale 3D X-ray system to periodically assess changes in the microstructure such as cracks, voids, and porosity in the TIM layer. The evolution of microstructure and the effect of cycling temperature during thermal cycling are discussed.
ContributorsLujan Regalado, Irene (Author) / Chawla, Nikhilesh (Thesis advisor) / Frear, Darrel (Committee member) / Rajagopalan, Jagannathan (Committee member) / Jiao, Yang (Committee member) / Arizona State University (Publisher)
Created2018
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Description
The stability of nanocrystalline microstructural features allows structural materials to be synthesized and tested in ways that have heretofore been pursued only on a limited basis, especially under dynamic loading combined with temperature effects. Thus, a recently developed, stable nanocrystalline alloy is analyzed here for quasi-static (<100 s-1) and dynamic

The stability of nanocrystalline microstructural features allows structural materials to be synthesized and tested in ways that have heretofore been pursued only on a limited basis, especially under dynamic loading combined with temperature effects. Thus, a recently developed, stable nanocrystalline alloy is analyzed here for quasi-static (<100 s-1) and dynamic loading (103 to 104 s-1) under uniaxial compression and tension at multiple temperatures ranging from 298-1073 K. After mechanical tests, microstructures are analyzed and possible deformation mechanisms are proposed. Following this, strain and strain rate history effects on mechanical behavior are analyzed using a combination of quasi-static and dynamic strain rate Bauschinger testing. The stable nanocrystalline material is found to exhibit limited flow stress increase with increasing strain rate as compared to that of both pure, coarse grained and nanocrystalline Cu. Further, the material microstructural features, which includes Ta nano-dispersions, is seen to pin dislocation at quasi-static strain rates, but the deformation becomes dominated by twin nucleation at high strain rates. These twins are pinned from further growth past nucleation by the Ta nano-dispersions. Testing of thermal and load history effects on the mechanical behavior reveals that when thermal energy is increased beyond 200 °C, an upturn in flow stress is present at strain rates below 104 s-1. However, in this study, this simple assumption, established 50-years ago, is shown to break-down when the average grain size and microstructural length-scale is decreased and stabilized below 100nm. This divergent strain-rate behavior is attributed to a unique microstructure that alters slip-processes and their interactions with phonons; thus enabling materials response with a constant flow-stress even at extreme conditions. Hence, the present study provides a pathway for designing and synthesizing a new-level of tough and high-energy absorbing materials.
ContributorsTurnage, Scott Andrew (Author) / Solanki, Kiran N (Thesis advisor) / Rajagopalan, Jagannathan (Committee member) / Peralta, Pedro (Committee member) / Darling, Kristopher A (Committee member) / Mignolet, Marc (Committee member) / Arizona State University (Publisher)
Created2017
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Description
Sn and Al alloys are widely used in various industries. Environmental-induced damage resulting in whiskering in Sn and corrosion in Al account for numerous failures globally every year. Therefore, for designing materials that can better withstand these failures, a comprehensive study on the characterization of the damage is necessary. This

Sn and Al alloys are widely used in various industries. Environmental-induced damage resulting in whiskering in Sn and corrosion in Al account for numerous failures globally every year. Therefore, for designing materials that can better withstand these failures, a comprehensive study on the characterization of the damage is necessary. This research implements advanced characterization techniques to study the above-mentioned environmental-induced damage in Sn and Al alloys.

Tin based films are known to be susceptible to whisker growth resulting in numerous failures. While the mechanisms and factors affecting whisker growth have been studied extensively, not much has been reported on the mechanical properties of tin whiskers themselves. This study focuses on the tensile behavior of tin whiskers. Tensile tests of whiskers were conducted in situ a dual beam focused ion beam (FIB) with a scanning electron microscope (SEM) using a micro electro-mechanical system (MEMS) tensile testing stage. The deformation mechanisms of whiskers were analyzed using transmission electron microscopy (TEM).

Due to the heterogenous nature of the microstructure of Al 7075, it is susceptible to corrosion forming corrosion products and pits. These can be sites for cracks nucleation and propagation resulting in stress corrosion cracking (SCC). Therefore, complete understanding of the corrosion damaged region and its effect on the strength of the alloy is necessary. Several studies have been performed to visualize pits and understand their effect on the mechanical performance of Al alloys using two-dimensional (2D) approaches which are often inadequate. To get a thorough understanding of the pits, it is necessary for three-dimensional (3D) studies. In this study, Al 7075 alloys were corroded in 3.5 wt.% NaCl solution and X-ray tomography was used to obtain the 3D microstructure of pits enabling the quantification of their dimensions accurately. Furthermore, microstructure and mechanical property correlations helped in a better understanding of the effect of corrosion. Apart from the pits, a surface corrosion layer also forms on Al. A subsurface damage layer has also been identified that forms due to the aggressive nature of NaCl. Energy dispersive X-ray spectroscopy (EDX) and nanoindentation helped in identifying this region and understanding the variation in properties.
ContributorsVallabhaneni, Venkata Sathya Sai Renuka (Author) / Chawla, Nikhilesh (Thesis advisor) / Rajagopalan, Jagannathan (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2017
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Description
Traditionally nanoporous gold is created by selective dissolution of silver or copper from a binary silver-gold or copper-gold alloy. These alloys serve as prototypical model systems for a phenomenon referred to as stress-corrosion cracking. Stress-corrosion cracking is the brittle failure of a normally ductile material occurring in a

Traditionally nanoporous gold is created by selective dissolution of silver or copper from a binary silver-gold or copper-gold alloy. These alloys serve as prototypical model systems for a phenomenon referred to as stress-corrosion cracking. Stress-corrosion cracking is the brittle failure of a normally ductile material occurring in a corrosive environment under a tensile stress. Silver-gold can experience this type of brittle fracture for a range of compositions. The corrosion process in this alloy results in a bicontinuous nanoscale morphology composed of gold-rich ligaments and voids often referred to as nanoporous gold. Experiments have shown that monolithic nanoporous gold can sustain high speed cracks which can then be injected into parent-phase alloy. This work compares nanoporous gold created from ordered and disordered copper-gold using digital image analysis and electron backscatter diffraction. Nanoporous gold from both disordered copper-gold and silver-gold, and ordered copper-gold show that grain orientation and shape remain largely unchanged by the dealloying process. Comparing the morphology of the nanoporous gold from ordered and disordered copper-gold with digital image analysis, minimal differences are found between the two and it is concluded that they are not statistically significant. This reveals the robust nature of nanoporous gold morphology against small variations in surface diffusion and parent-phase crystal structure.
Then the corrosion penetration down the grain boundary is compared to the depth of crack injections in polycrystal silver-gold. Based on statistical comparison, the crack-injections penetrate into the parent-phase grain boundary beyond the corrosion-induced porosity. To compare crack injections to stress-corrosion cracking, single crystal silver-gold samples are employed. Due to the cleavage-like nature of the fracture surfaces, electron backscatter diffraction is possible and employed to compare the crystallography of stress-corrosion crack surfaces and crack-injection surfaces. From the crystallographic similarities of these fracture surfaces, it is concluded that stress-corrosion can occur via a series of crack-injection events. This relationship between crack injections and stress corrosion cracking is further examined using electrochemical data from polycrystal silver-gold samples during stress-corrosion cracking. The results support the idea that crack injection is a mechanism for stress-corrosion cracking.
ContributorsKarasz, Erin (Author) / Sieradzki, Karl (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Peralta, Pedro (Committee member) / Rajagopalan, Jagannathan (Committee member) / Arizona State University (Publisher)
Created2020
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Description
Thin films are widely used for a variety of applications such as electrical interconnects, sensors, as well as optical, mechanical, and decorative coatings. Thin films made of NiTi, commonly referred to as nitinol, have generated recent interest as they are highly suitable for high frequency thermal actuation in microelectromechanical devices

Thin films are widely used for a variety of applications such as electrical interconnects, sensors, as well as optical, mechanical, and decorative coatings. Thin films made of NiTi, commonly referred to as nitinol, have generated recent interest as they are highly suitable for high frequency thermal actuation in microelectromechanical devices because of their small thermal mass and large surface-to-volume ratio. The functional properties of NiTi arise from a diffusionless phase transformation between two of its primary phases: austenite and martensite. This transformation leads to either the shape memory or pseudoelastic effect, where inelastic deformation is recovered with and without the application of heat, respectively. It is well known that the mechanical properties of NiTi are highly dependent on the microstructure, but few studies have been performed to examine the mechanical behavior of thin NiTi films (thickness below 200 nm), which are expected to have grain sizes in a similar range. The primary intent of this work is the synthesis of NiTi thin films with controlled microstructures, followed by characterization of their microstructure and its relationship to the mechanical properties. Microstructural control was achieved by utilizing a novel synthesis technique in which amorphous precursor films are seeded with nanocrystals, which serve as nucleation sites during subsequent crystallization via thermal annealing. This technique enables control of grain size, dispersion, and phase composition of thin films by varying the parameters of seed deposition as well as annealing conditions. The microstructures and composition of the NiTi thin films were characterized using X-ray Diffraction, Electron Microprobe Analysis, High-resolution Transmission Electron Microscopy, Secondary Ion Mass Spectroscopy, Differential Scanning Calorimetry, as well as other complementary techniques. Mechanical properties of the films were investigated using uniaxial tensile testing performed using a custom microfabricated tensile testing stage. The NiTi thin films exhibit mechanical behavior that is distinct from bulk NiTi, which is also highly sensitive to small changes in microstructure and phase composition. These findings are rationalized in terms of the changes in deformation mechanisms that occur at small grain sizes and sample dimensions.
ContributorsRASMUSSEN, Paul (Author) / Rajagopalan, Jagannathan (Thesis advisor) / Solanki, Kiran (Committee member) / Sieradzki, Karl (Committee member) / Arizona State University (Publisher)
Created2021
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Description
Physical vapor deposition (PVD) of phase-separating multicomponent alloy films generates a rich variety of unique self-organized nanoscale morphologies. However, an understanding of how the different material and process parameters influence the formation of these nanostructures is limited. My dissertation aims to bridge this gap by developing phase-field models that can

Physical vapor deposition (PVD) of phase-separating multicomponent alloy films generates a rich variety of unique self-organized nanoscale morphologies. However, an understanding of how the different material and process parameters influence the formation of these nanostructures is limited. My dissertation aims to bridge this gap by developing phase-field models that can predict an entire spectrum of nanostructures as a function of processing conditions and composition in multicomponent alloys under a set of material-specific constraints. Firstly, I developed a numerical model to simulate nanoscale phase separation in codeposited immiscible binary alloy films. An investigation on the influence of deposition rates, phase-fraction, and temperature, on the evolution of self-assembled nanostructures yielded many characteristic patterns, including well-known morphologies such as the lateral and vertical concentration modulations, as well as some previously undocumented variants. I also simulated phase-separation in ternary alloyed PVD films, and studied the influence of deposition rate and composition on the evolution of self-assembled nanostructures, and recorded many novel nanoscale morphologies. I then sought to understand the role of material properties such as elastic misfit due to lattice mismatch between phases, grain boundaries formed in polycrystalline films, and the interplay of interphase and surface boundaries at the film surface. To this end, I developed phase-field models of binary PVD film deposition that incorporated these constraints and studied their role in altering the temporal and spatial characteristics of the evolving morphologies. I also investigated the formation of surface hillocks and the role of surface and interfacial energies in their evolution. By studying the change in total free energy across the different deposition models, I established that, in addition to influencing the temporal and spatial characteristics of nanoscale structures in the films, this quantity is also responsible for driving morphological transitions as the rate of deposition is increased. Insights gained from this computational study will demonstrate the viability of these models in predicting experimentally observed morphologies and form a basis for understanding the various factors involved in driving phase-separation and morphological transitions. In addition, morphology maps will serve as templates for developing new pathways for morphology control in the manufacturing of PVD alloy films.
ContributorsRaghavan, Rahul (Author) / Ankit, Kumar (Thesis advisor) / Rajagopalan, Jagannathan (Committee member) / Mushongera, Leslie T (Committee member) / Arizona State University (Publisher)
Created2021
Description
Layer-wise extrusion of soft-solid like cement pastes and mortars is commonly used in 3D printing of concrete. Rheological and mechanical characterization of the printable binder for on-demand flow and subsequent structuration is a critical challenge. This research is an effort to understand the mechanics of cementitious binders as soft solids

Layer-wise extrusion of soft-solid like cement pastes and mortars is commonly used in 3D printing of concrete. Rheological and mechanical characterization of the printable binder for on-demand flow and subsequent structuration is a critical challenge. This research is an effort to understand the mechanics of cementitious binders as soft solids in the fresh state, towards establishing material-process relationships to enhance print quality. This study introduces 3D printable binders developed based on rotational and capillary rheology test parameters, and establish the direct influence of packing coefficients, geometric ratio, slip velocities, and critical print velocities on the extrudate quality. The ratio of packing fraction to the square of average particle diameter (0.01-0.02), and equivalent microstructural index (5-20) were suitable for printing, and were directly related to the cohesion and extrusional yield stress of the material. In fact, steady state pressure for printing (30-40 kPa) is proportional to the extrusional yield stress, and increases with the geometric ratio (0-60) and print velocity (5-50 mm/s). Higher print velocities results in higher wall shear stresses and was exponentially related to the slip layer thickness (estimated between 1-5μ), while the addition of superplasticizers improve the slip layer thickness and the extrudate flow. However, the steady state pressure and printer capacity limits the maximum print velocity while the deadzone length limits the minimum velocity allowable (critical velocity regime) for printing. The evolution of buildability with time for the fresh state mortars was characterized with digital image correlation using compressive strain and strain rate in printed layers. The fresh state characteristics (interlayer and interfilamentous) and process parameters (layer height and fiber dimensions) influence the hardened mechanical properties. A lower layer height generally improves the mechanical properties and slight addition of fiber (up to 0.3% by volume) results in a 15-30% increase in the mechanical properties. 3D scanning and point-cloud analysis was also used to assess the geometric tolerance of a print based on mean error distances, print accuracy index, and layer-wise percent overlap. The research output will contribute to a synergistic material-process design and development of test methods for printability in the context of 3D printing of concrete.
ContributorsAmbadi Omanakuttan Nair, Sooraj Kumar (Author) / Neithalath, Narayanan (Thesis advisor) / Rajan, Subramaniam (Committee member) / Mobasher, Barzin (Committee member) / Hoover, Christian (Committee member) / Chawla, Nikhilesh (Committee member) / Arizona State University (Publisher)
Created2021