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Description
Stress corrosion cracking (SCC) is a materials degradation phenomena resulting from a combination of stress and a corrosive environment. Among the alphabet soup of proposed mechanism of SCC the most important are film-rupture, film-induced cleavage and hydrogen embrittlement.

This work examines various aspects of film-induced cleavage in gold alloys for which

Stress corrosion cracking (SCC) is a materials degradation phenomena resulting from a combination of stress and a corrosive environment. Among the alphabet soup of proposed mechanism of SCC the most important are film-rupture, film-induced cleavage and hydrogen embrittlement.

This work examines various aspects of film-induced cleavage in gold alloys for which the operation of hydrogen embrittlement processes can be strictly ruled out on thermodynamic grounds. This is so because in such alloys SCC occurs under electrochemical conditions within which water is stable to hydrogen gas evolution. The alloy system examined in this work is AgAu since the corrosion processes in this system occur by a dealloying mechanism that results in the formation of nanoporous gold. The physics behind the dealloying process as well as the resulting formation of nanoporous gold is today well understood.

Two important aspects of the film-induced cleavage mechanism are examined in this work: dynamic fracture in monolithic nanoporous gold and crack injection. In crack injection there is a finite thickness dealloyed layer formed on a AgAu alloy sample and the question of whether or not a crack that nucleates within this layer can travel for some finite distance into the un-corroded parent phase alloy is addressed. Dynamic fracture tests were performed on single edge-notched monolithic nanoporous gold samples as well as “infinite strip” sample configurations for which the stress intensity remains constant over a significant portion of the crack length. High-speed photography was used to measure the crack velocity. In the dynamic fracture experiments cracks were observed to travel at speeds as large as 270 m/s corresponding to about 68% of the Raleigh wave velocity. Crack injection experiments were performed on single crystal Ag77Au23, polycrystalline Ag72Au28 and pure gold, all of which had thin nanoporous gold layers on the surface of samples. Through-thickness fracture was seen in both the single crystal and polycrystalline samples and there was an indication of ~ 1 μm injected cracks into pure gold. These results have important implications for the operation of the film-induced cleavage mechanism and represent a first step in the development of a fundamental model of SCC.
ContributorsChen, Xiying (Author) / Sieradzki, Karl (Thesis advisor) / Jiao, Yang (Committee member) / Oswald, Jay (Committee member) / Crozier, Peter (Committee member) / Peralta, Pedro (Committee member) / Arizona State University (Publisher)
Created2016
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Description
Structural stability and performance of structural materials is important for energy production, whether renewable or non renewable, to have uninterrupted energy supply, that is economically feasible and safe. High temperature metallic materials used in the turbines of AORA, an Israel-based clean energy producer, often experience high temperature, high stress and

Structural stability and performance of structural materials is important for energy production, whether renewable or non renewable, to have uninterrupted energy supply, that is economically feasible and safe. High temperature metallic materials used in the turbines of AORA, an Israel-based clean energy producer, often experience high temperature, high stress and foreign object damage (FOD). In this study, efforts were made to study the effects of FOD on the fatigue life of these materials and to understand their failure mechanisms. The foreign objects/debris recovered by AORA were characterized using Powder X-ray Diffraction (XRD) and Energy Dispersive Spectroscopy (EDS) to identify composition and phases. To perform foreign object damage experiment a gas gun was built and results of XRD and EDS were used to select particles to mimic FOD in lab experiments for two materials of interest to AORA: Hastelloy X and SS 347. Electron Backscattering Diffraction, hardness and tensile tests were also performed to characterize microstructure and mechanical properties. Fatigue tests using at high temperature were performed on dog bone samples with and without FOD and the fracture surfaces and well as the regions affected by FOD were analyzed using Scanning Electron Microscopy (SEM) to understand the failure mechanism. The findings of these study indicate that FOD is causing multiple secondary cracks at and around the impact sites, which can potentially grow to coalesce and remove pieces of material, and the multisite damage could also lead to lower fatigue lives, despite the fact that the FOD site was not always the most favorable for initiation of the fatal fatigue crack. It was also seen by the effect of FOD on fatigue life that SS 347 is more susceptible to FOD than Hastelloy X.
ContributorsDobaria, Nirmal (Author) / Peralta, Pedro (Thesis advisor) / Sieradzki, Karl (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2016
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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 use of solar energy to produce power has increased substantially in the past few decades. In an attempt to provide uninterrupted solar power, production plants may find themselves having to operate the systems at temperatures higher than the operational capacity of the materials used in many of their components,

The use of solar energy to produce power has increased substantially in the past few decades. In an attempt to provide uninterrupted solar power, production plants may find themselves having to operate the systems at temperatures higher than the operational capacity of the materials used in many of their components, which affects the microstructural and mechanical properties of those materials. Failures in components that have been exposed to these excessive temperatures have been observed during operations in the turbine used by AORA Solar Ltd. A particular component of interest was made of a material similar to the Ni-based superalloy Inconel 718 (IN 718), which was observed to have damage that is believed to have been initiated by Foreign Object Damage (FOD) and worsened by the high temperatures in the turbine. The potential links among the observed failure, FOD and the high temperatures of operation are investigated in this study.

IN718 is a precipitation hardened nickel superalloy with resistance to oxidation and ability to withstand high stresses over a wide range of temperatures. Several studies have been conducted to understand IN 718 tensile and fatigue properties at elevated temperatures (600- 950°C). However, this study focuses on understanding the behavior of IN718 with FOD induced by a stream of 50 μm Alumina particles at a velocity of 200 m/s. under high cycle fatigue at an elevated temperature of 1050 °C. Tensile tests were conducted for both as-received and heat treated (1050 °C in air for 8hrs) samples at room and high temperature. Fatigue tests were performed at heat treated samples at 1050 °C for samples with and without ablation. The test conditions were as similar as possible to the conditions in the AORA turbine. The results of the study provide an insight into tensile properties, fatigue properties and FOD. The results indicated a reduction in fatigue life for the samples with ablation damage, where crack nucleation occurred either at the edge or inside the ablation region and multisite cracking was observed under far field stresses that were the same than for pristine samples, which showed single cracks. Fracture surfaces indicate intergranular fracture, with the presence of secondary cracks and a lack of typical fatigue features, e.g., beach marks which was attributed to environmental effects and creep.
ContributorsShenoy, Sneha (Author) / Peralta, Pedro (Thesis advisor) / Solanki, Kiran (Committee member) / Sieradzki, Karl (Committee member) / Arizona State University (Publisher)
Created2017
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Description
The increasing demand for structural materials with superior mechanical properties has provided a strong impetus to the discovery of novel materials, and innovations in processing techniques to improve the properties of existing materials. Methods like severe plastic deformation (SPD) and surface mechanical attrition treatment (SMAT) have led to significant enhancement

The increasing demand for structural materials with superior mechanical properties has provided a strong impetus to the discovery of novel materials, and innovations in processing techniques to improve the properties of existing materials. Methods like severe plastic deformation (SPD) and surface mechanical attrition treatment (SMAT) have led to significant enhancement in the strength of traditional structural materials like Al and Fe based alloys via microstructural refinement. However, the nanocrystalline materials produced using these techniques exhibit poor ductility due to the lack of effective strain hardening mechanisms, and as a result the well-known strength-ductility trade-off persists. To overcome this trade-off, researchers have proposed the concept of heterostructured materials, which are composed of domains ranging in size from a few nanometers to several micrometers. Over the last two decades, there has been intense research on the development of new methods to synthesize heterostructured materials. However, none of these methods is capable of providing precise control over key microstructural parameters such as average grain size, grain morphology, and volume fraction and connectivity of coarse and fine grains. Due to the lack of microstructural control, the relationship between these parameters and the deformation behavior of heterostructured materials cannot be investigated systematically, and hence designing heterostructured materials with optimized properties is currently infeasible. This work aims to address this scientific and technological challenge and is composed of two distinct but interrelated parts. The first part concerns the development of a broadly applicable synthesis method to produce heterostructured metallic films with precisely defined architectures. This method exploits two forms of film growth (epitaxial and Volmer-Weber) to generate heterostructured metallic films. The second part investigates the effect of different microstructural parameters on the deformation behavior of heterostructured metallic films with the aim of elucidating their structure-property relationships. Towards this end, freestanding heterostructured Fe films with different architectures were fabricated and uniaxially deformed using MEMS stages. The results from these experiments are presented and their implications for the mechanical properties of heterostructured materials is discussed.
ContributorsBerlia, Rohit (Author) / Rajagopalan, Jagannathan (Thesis advisor) / Sieradzki, Karl (Committee member) / Peralta, Pedro (Committee member) / Crozier, Peter (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2021
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Description
Solid-state and non-equilibrium processings are of great interest to researchers due to their ability to control and refine bulk and/or surface microstructure of metallic alloys and push them to surpass their conventional properties limit. In this dissertation, solid-state processing i.e., Shear Assisted Processing and Extrusion (ShAPE), and non-equilibrium processes i.e.,

Solid-state and non-equilibrium processings are of great interest to researchers due to their ability to control and refine bulk and/or surface microstructure of metallic alloys and push them to surpass their conventional properties limit. In this dissertation, solid-state processing i.e., Shear Assisted Processing and Extrusion (ShAPE), and non-equilibrium processes i.e., surface mechanical attrition (SMAT) and additive manufacturing (AM) techniques were used to process the magnesium and aluminum alloys respectively. A synergistic investigation of processing-induced microstructural modification and its effect on corrosion resistance was performed using various ex-situ, quasi in-situ, and in-situ electrochemical, microscopy, and spectroscopy characterization techniques. To evaluate the effect of the same processing condition on a range of microstructures, a variety of magnesium alloys such as AZ31B, Mg-3Si, ZK60, and Pure Mg were processed using a novel solid-state processing method, namely ShAPE. It induced a significant grain refinement, homogenized distribution of second phases, and low residual strain in AZ31B alloy, which contributed toward a noble breakdown potential, stable protective film, and hence better corrosion resistance compared to the parent extruded counterpart. However, with variations in composition, volume fraction, and distribution of second phases with Mg-3Si and ZK60 magnesium alloy an opposite response was inferred indicating a strong dependence of corrosion on underlying microstructure compared to a processing condition. Non-equilibrium processes, i.e. SMAT and AM were utilized to process high-strength 7xxx series aluminum alloys. Continuous high energy impacts of hard balls in room temperature (RT SMAT) and liquid nitrogen (LN2 SMAT) flow environment generated a gradient nanocrystalline surface layer with the dissolution of inherent second phase and precipitation of new phases in aluminum 7075 alloys. RT SMAT showed a reduced anodic dissolution rate and improved film resistance, which was attributed to the thicker and composite oxide layer along with new nanoscale precipitates. Lastly, reactive AM was used to process aluminum 7075 and 7050 alloys which resulted in a refined and textureless microstructure. A reduction in corrosion resistance was observed with precipitation of excessive reactive particles (Ti and B4C) in AM alloys compared to wrought counterparts.
ContributorsBeura, Vikrant Kumar (Author) / Solanki, Kiran N (Thesis advisor) / Peralta, Pedro (Committee member) / Alford, Terry (Committee member) / Ankit, Kumar (Committee member) / Joshi, Vineet V (Committee member) / Arizona State University (Publisher)
Created2022
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Description
Microstructure refinement and alloy additions are considered potential routes to increase high temperature performance of existing metallic superalloys used under extreme conditions. Nanocrystalline (NC) Cu-10at%Ta exhibits such improvements over microstructurally unstable NC metals, leading to enhanced creep behavior compared to its coarse-grained (CG) counterparts. However, the low melting point of

Microstructure refinement and alloy additions are considered potential routes to increase high temperature performance of existing metallic superalloys used under extreme conditions. Nanocrystalline (NC) Cu-10at%Ta exhibits such improvements over microstructurally unstable NC metals, leading to enhanced creep behavior compared to its coarse-grained (CG) counterparts. However, the low melting point of Cu compared to other FCC metals, e.g., Ni, might lead to an early onset of diffusional creep mechanisms. Thus, this research seeks to study the thermo-mechanical behavior and stability of hierarchical (prepared using arc-melting) and NC (prepared by collaborators through powder pressing and annealing) Ni-Y-Zr alloys where Zr is expected to provide solid solution and grain boundary strengthening in hierarchical and NC alloys, respectively, while Ni-Y and Ni-Zr intermetallic precipitates (IMCs) would provide kinetic stability. Hierarchical alloys had microstructures stable up to 1100 °C with ultrafine eutectic of ~300 nm, dendritic arm spacing of ~10 μm, and grain size ~1-2 mm. Room temperature hardness tests along with uniaxial compression performed at 25 and 600 °C revealed that microhardness and yield strength of hierarchical alloys with small amounts of Y (0.5-1wt%) and Zr (1.5-3 wt%) were comparable to Ni-superalloys, due to the hierarchical microstructure and potential presence of nanoscale IMCs. In contrast, NC alloys of the same composition were found to be twice as hard as the hierarchical alloys. Creep tests at 0.5 homologous temperature showed active Coble creep mechanisms in hierarchical alloys at low stresses with creep rates slower than Fe-based superalloys and dislocation creep mechanisms at higher stresses. Creep in NC alloys at lower stresses was only 20 times faster than hierarchical alloys, with the difference in grain size ranging from 10^3 to 10^6 times at the same temperature. These NC alloys showed enhanced creep properties over other NC metals and are expected to have rates equal to or improved over the CG hierarchical alloys with ECAP processing techniques. Lastly, the in-situ wide-angle x-ray scattering (WAXS) measurements during quasi-static and creep tests implied stresses being carried mostly by the matrix before yielding and in the primary creep stage, respectively, while relaxation was observed in Ni5Zr for both hierarchical and NC alloys. Beyond yielding and in the secondary creep stage, lattice strains reached a steady state, thereby, an equilibrium between plastic strain rates was achieved across different phases, so that deformation reaches a saturation state where strain hardening effects are compensated by recovery mechanisms.
ContributorsSharma, Shruti (Author) / Peralta, Pedro (Thesis advisor) / Alford, Terry (Committee member) / Jiao, Yang (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2022
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Description
Aromatic polymers, with benzene-like rings in their main chains, include materials such as polyurea, an amorphous elastomer capable of dissipating large amounts of energy under dynamic loading, which makes it a promising coating for defensive systems. Although computational research exists that investigates the atomic-level response of polyurea and other amorphous

Aromatic polymers, with benzene-like rings in their main chains, include materials such as polyurea, an amorphous elastomer capable of dissipating large amounts of energy under dynamic loading, which makes it a promising coating for defensive systems. Although computational research exists that investigates the atomic-level response of polyurea and other amorphous aromatic polymers to extreme conditions, there is little experimental work to validate these models 1) at the atomic-scale and 2) under high pressures characteristic of extreme dynamic loading. Understanding structure-property relationships at the atomic-level is important for polymers, considering many of them undergo pressure and temperature-induced structural transformations, which must be understood to formulate accurate predictive models. This work aims to gain a deeper understanding of the high-pressure structural response of aromatic polymers at the atomic-level, with emphasis into the mechanisms associated with high-pressure transformations. Hence, atomic-level structural data at high pressures was obtained in situ via multiangle energy dispersive X-ray diffraction (EDXD) experiments at the Advanced Photon Source (APS) for polyurea and another amorphous aromatic polymer, polysulfone, chosen as a reference due to its relatively simple structure. Pressures up to 6 GPa were applied using a Paris Edinburgh (PE) hydraulic press at room temperature. Select polyurea samples were also heated to 277 °C at 6 GPa. The resulting structure factors and pair distribution functions, along with molecular dynamics simulations of polyurea provided by collaborators, suggest that the structures of both polymers are stable up to 6 GPa, aside from reductions in free-volume between polymer backbones. As higher pressures (≲ 32 GPa) were applied using diamond anvils in combination with the PE press, indications of structural transformations were observed in both polymers that appear similar in nature to the sp2-sp3 hybridization in compressed carbon. The transformation occurs gradually up to at least ~ 26 GPa in PSF, while it does not progress past ~ 15 GPa in polyurea. The changes are largely reversible, especially in polysulfone, consistent with pressure-driven, reversible graphite-diamond transformations in the absence of applied temperature. These results constitute some of the first in situ observations of the mechanisms that drive pressure-induced structural transformations in aromatic polymers.
ContributorsEastmond, Tyler (Author) / Peralta, Pedro (Thesis advisor) / Hoover, Christian (Committee member) / Hrubiak, Rostislav (Committee member) / Mignolet, Marc (Committee member) / Oswald, Jay (Committee member) / Arizona State University (Publisher)
Created2022
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Description
Shock loading produces a compressive stress pulse with steep gradients in density, temperature, and pressure that are also often modeled as discontinuities. When a material is subject to these dynamic (shock) loading conditions, fracture and deformation patterns due to spall damage can arise. Spallation is a dynamic material failure that

Shock loading produces a compressive stress pulse with steep gradients in density, temperature, and pressure that are also often modeled as discontinuities. When a material is subject to these dynamic (shock) loading conditions, fracture and deformation patterns due to spall damage can arise. Spallation is a dynamic material failure that is caused by the nucleation, growth, and coalescence of voids, with possible ejection of the surface of the material. Intrinsic defects, such as grain boundaries are the preferred initiation sites of spall damage in high purity materials. The focus of this research is to study the phenomena that cause void nucleation and growth at a particular grain boundary (GB), chosen to maximize spall damage localization.

Bicrystal samples were shock loaded using flyer-plates via light gas gun and direct laser ablation. Stress, pulse duration, and crystal orientation along the shock direction were varied for a fixed boundary misorientation to determine thresholds for void nucleation and coalescence as functions of these parameters. Pressures for gas gun experiments ranged from 2 to 5 GPa, while pressures for laser ablation experiments varied from 17 to 25 GPa. Samples were soft recovered to perform damage characterization using electron backscattering diffraction (EBSD) and Scanning Electron Microscopy (SEM). Results showed a 14% difference in the thresholds for void nucleation and coalescence between samples with different orientations along the shock direction, which were affected by pulse duration and stress level. Fractography on boundaries with strong damage localization showed many small voids, indicating they experience rapid nucleation, causing early coalescence. Composition analysis was also performed to determine the effect of impurities on damage evolution. Results showed that higher levels of impurities led to more damage. ABAQUS/Explicit models were developed to simulate flyer-plate impact and void growth with the same crystal orientations and experimental conditions. Results are able to match the damage seen in each grain of the target experimentally. The Taylor Factor mismatch at the boundary can also be observed in the model with the higher Taylor Factor grain exhibiting more damage.
ContributorsFortin, Elizabeth Victoria (Author) / Peralta, Pedro (Thesis advisor) / Mignolet, Marc (Committee member) / Loomis, Eric (Committee member) / Oswald, Jay (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2020
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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