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Fission products in nuclear fuel pellets can affect fuel performance as they change the fuel chemistry and structure. The behavior of the fission products and their release mechanisms are important to the operation of a power reactor. Research has shown that fission product release can occur through grain boundary (GB)

Fission products in nuclear fuel pellets can affect fuel performance as they change the fuel chemistry and structure. The behavior of the fission products and their release mechanisms are important to the operation of a power reactor. Research has shown that fission product release can occur through grain boundary (GB) at low burnups. Early fission gas release models, which assumed spherical grains with no effect of GB diffusion, did not capture the early stage of the release behavior well. In order to understand the phenomenon at low burnup and how it leads to the later release mechanism, a microstructurally explicit model is needed. This dissertation conducted finite element simulations of the transport behavior using 3-D microstructurally explicit models. It looks into the effects of GB character, with emphases on conditions that can lead to enhanced effective diffusion. Moreover, the relationship between temperature and fission product transport is coupled to reflect the high temperature environment.

The modeling work began with 3-D microstructure reconstruction for three uranium oxide samples with different oxygen stoichiometry: UO2.00 UO2.06 and UO2.14. The 3-D models were created based on the real microstructure of depleted UO2 samples characterized by Electron Backscattering Diffraction (EBSD) combined with serial sectioning. Mathematical equations on fission gas diffusion and heat conduction were studied and derived to simulate the fission gas transport under GB effect. Verification models showed that 2-D elements can be used to model GBs to reduce the number of elements. The effect of each variable, including fuel stoichiometry, temperature, GB diffusion, triple junction diffusion and GB thermal resistance, is verified, and they are coupled in multi-physics simulations to study the transport of fission gas at different radial location of a fuel pellet. It was demonstrated that the microstructural model can be used to incorporate the effect of different physics to study fission gas transport. The results suggested that the GB effect is the most significant at the edge of fuel pellet where the temperature is the lowest. In the high temperature region, the increase in bulk diffusivity due to excess oxygen diminished the effect of GB diffusion.
ContributorsLim, Harn Chyi (Author) / Peralta, Pedro (Thesis advisor) / Jiang, Hanqing (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2014
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Description
With increasing concerns of the intrinsic toxicity of lead (Pb) in electronics, a series of tin (Sn) based alloys involving silver (Ag) and copper (Cu) have been proposed as replacements for Pb-Sn solder and widely accepted by industry. However, they have a higher melting point and often exhibit poorer damage

With increasing concerns of the intrinsic toxicity of lead (Pb) in electronics, a series of tin (Sn) based alloys involving silver (Ag) and copper (Cu) have been proposed as replacements for Pb-Sn solder and widely accepted by industry. However, they have a higher melting point and often exhibit poorer damage tolerance than Pb-Sn alloys. Recently, a new class of alloys with trace amount of rare-earth (RE) elements has been discovered and investigated. In previous work from Prof. Chawla's group, it has been shown that cerium (Ce)-based Pb-free solder are less prone to oxidation and Sn whiskering, and exhibit desirable attributes of microstructural refinement and enhanced ductility relative to lanthanum (La)-based Sn-3.9Ag-0.7Cu (SAC) alloy. Although the formation of RESn3 was believed to be directly responsible for the enhanced ductility in RE-containing SAC solder by allowing microscopic voids to nucleate throughout the solder volume, this cavitation-based mechanism needs to be validated experimentally and numerically. Additionally, since the previous study has exhibited the realistic feasibility of Ce-based SAC lead-free solder alloy as a replacement to conventional SAC alloys, in this study, the proposed objective focuses on the in in-depth understanding of mechanism of enhanced ductility in Ce-based SAC alloy and possible issues associated with integration of this new class of solder into electronic industry, including: (a) study of long-term thermal and mechanical stability on industrial metallization, (b) examine the role of solder volume and wetting behavior of the new solder, relative to Sn-3.9Ag-0.7Cu alloys, (c) conduct experiments of new solder alloys in the form of mechanical shock and electromigration. The research of this new class alloys will be conducted in industrially relevant conditions, and the results would serve as the first step toward integration of these new, next generation solders into the industry.
ContributorsXie, Huxiao (Author) / Chawla, Nikhilesh (Thesis advisor) / Krause, Stephen (Committee member) / Solanki, Kiran (Committee member) / Mirpuri, Kabir (Committee member) / Arizona State University (Publisher)
Created2012
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Description
Al 7075 alloys are used in a variety of structural applications, such as aircraft wings, automotive components, fuselage, spacecraft, missiles, etc. The mechanical and corrosion behavior of these alloys are dependent on their microstructure and the environment. Therefore, a comprehensive study on microstructural characterization and stress-environment interaction is necessary. Traditionally,

Al 7075 alloys are used in a variety of structural applications, such as aircraft wings, automotive components, fuselage, spacecraft, missiles, etc. The mechanical and corrosion behavior of these alloys are dependent on their microstructure and the environment. Therefore, a comprehensive study on microstructural characterization and stress-environment interaction is necessary. Traditionally, 2D techniques have been used to characterize microstructure, which are inaccurate and inadequate since the research has shown that the results obtained in the bulk are different from those obtained on the surface. There now exist several techniques in 3D, which can be used to characterize the microstructure. Al 7075 alloys contain second phase particles which can be classified as Fe-bearing inclusions, Si-bearing inclusions and precipitates. The variation in mechanical and corrosion properties of aluminum alloys has been attributed to the size, shape, distribution, corrosion properties and mechanical behavior of these precipitates and constituent particles. Therefore, in order to understand the performance of Al 7075 alloys, it is critical to investigate the size and distribution of inclusions and precipitates in the alloys along with their mechanical properties, such as Young's modulus, hardness and stress-strain behavior. X-ray tomography and FIB tomography were used to visualize and quantify the microstructure of constituent particles (inclusions) and precipitates, respectively. Microscale mechanical characterization techniques, such as nanoindentation and micropillar compression, were used to obtain mechanical properties of inclusions. Over the years, studies have used surface measurements to understand corrosion behavior of materials. More recently, in situ mechanical testing has become more attractive and advantageous, as it enables visualization and quantification of microstructural changes as a function of time (4D). In this study, in situ X-ray synchrotron tomography was used to study the SCC behavior of Al 7075 alloys in moisture and deionized water. Furthermore, experiments were performed in EXCO solution to study the effect of applied stress on exfoliation behavior in 3D. Contrary to 2D measurements made at the surface which suggest non-uniform crack growth rates, three dimensional measurements of the crack length led to a much more accurate measurement of crack growth rates.
ContributorsSingh, Sudhanshu Shekhar (Author) / Chawla, Nikhilesh (Thesis advisor) / Alford, Terry (Committee member) / Solanki, Kiran (Committee member) / Oswald, Jay (Committee member) / Arizona State University (Publisher)
Created2015
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Description
Hydrogen embrittlement (HE) is a phenomenon that affects both the physical and chemical properties of several intrinsically ductile metals. Consequently, understanding the mechanisms behind HE has been of particular interest in both experimental and modeling research. Discrepancies between experimental observations and modeling results have led to various proposals for HE

Hydrogen embrittlement (HE) is a phenomenon that affects both the physical and chemical properties of several intrinsically ductile metals. Consequently, understanding the mechanisms behind HE has been of particular interest in both experimental and modeling research. Discrepancies between experimental observations and modeling results have led to various proposals for HE mechanisms. Therefore, to gain insights into HE mechanisms in iron, this dissertation aims to investigate several key issues involving HE such as: a) the incipient crack tip events; b) the cohesive strength of grain boundaries (GBs); c) the dislocation-GB interactions and d) the dislocation mobility.

The crack tip, which presents a preferential trap site for hydrogen segregation, was examined using atomistic methods and the continuum based Rice-Thompson criterion as sufficient concentration of hydrogen can alter the crack tip deformation mechanism. Results suggest that there is a plausible co-existence of the adsorption induced dislocation emission and hydrogen enhanced decohesion mechanisms. In the case of GB-hydrogen interaction, we observed that the segregation of hydrogen along the interface leads to a reduction in cohesive strength resulting in intergranular failure. A methodology was further developed to quantify the role of the GB structure on this behavior.

GBs play a fundamental role in determining the strengthening mechanisms acting as an impediment to the dislocation motion; however, the presence of an unsurmountable barrier for a dislocation can generate slip localization that could further lead to intergranular crack initiation. It was found that the presence of hydrogen increases the strain energy stored within the GB which could lead to a transition in failure mode. Finally, in the case of body centered cubic metals, understanding the complex screw dislocation motion is critical to the development of an accurate continuum description of the plastic behavior. Further, the presence of hydrogen has been shown to drastically alter the plastic deformation, but the precise role of hydrogen is still unclear. Thus, the role of hydrogen on the dislocation mobility was examined using density functional theory and atomistic simulations. Overall, this dissertation provides a novel atomic-scale understanding of the HE mechanism and development of multiscale tools for future endeavors.
ContributorsAdlakha, Ilaksh (Author) / Solanki, Kiran (Thesis advisor) / Mignolet, Marc (Committee member) / Chawla, Nikhilesh (Committee member) / Jiang, Hanqing (Committee member) / Liu, Yongming (Committee member) / Arizona State University (Publisher)
Created2015
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Description
Aluminum alloys are ubiquitously used in almost all structural applications due to their high strength-to-weight ratio. Their superior mechanical performance can be attributed to complex dispersions of nanoscale intermetallic particles that precipitate out from the alloy’s solid solution and offer resistance to deformation. Although they have been extensively investigated in

Aluminum alloys are ubiquitously used in almost all structural applications due to their high strength-to-weight ratio. Their superior mechanical performance can be attributed to complex dispersions of nanoscale intermetallic particles that precipitate out from the alloy’s solid solution and offer resistance to deformation. Although they have been extensively investigated in the last century, the traditional approaches employed in the past haven’t rendered an authoritative microstructural understanding in such materials. The effect of the precipitates’ inherent complex morphology and their three-dimensional (3D) spatial distribution on evolution and deformation behavior have often been precluded. In this study, for the first time, synchrotron-based hard X-ray nano-tomography has been implemented in Al-Cu alloys to measure growth kinetics of different nanoscale phases in 3D and reveal mechanistic insights behind some of the observed novel phase transformation reactions occurring at high temperatures. The experimental results were reconciled with coarsening models from the LSW theory to an unprecedented extent, thereby establishing a new paradigm for thermodynamic analysis of precipitate assemblies. By using a unique correlative approach, a non-destructive means of estimating precipitation-strengthening in such alloys has been introduced. Limitations of using existing mechanical strengthening models in such alloys have been discussed and a means to quantify individual contributions from different strengthening mechanisms has been established.

The current rapid pace of technological progress necessitates the demand for more resilient and high-performance alloys. To achieve this, a thorough understanding of the relationships between material properties and its structure is indispensable. To establish this correlation and achieve desired properties from structural alloys, microstructural response to mechanical stimuli needs to be understood in three-dimensions (3D). To that effect, in situ tests were conducted at the synchrotron (Advanced Photon Source) using Transmission X-Ray Microscopy as well as in a scanning electron microscope (SEM) to study real-time damage evolution in such alloys. Findings of precipitate size-dependent transition in deformation behavior from these tests have inspired a novel resilient aluminum alloy design.
ContributorsKaira, Chandrashekara Shashank (Author) / Chawla, Nikhilesh (Thesis advisor) / Solanki, Kiran (Committee member) / Jiao, Yang (Committee member) / De Andrade, Vincent (Committee member) / Arizona State University (Publisher)
Created2017
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Description
Shock loading is a complex phenomenon that can lead to failure mechanisms such as strain localization, void nucleation and growth, and eventually spall fracture. The length scale of damage with respect to that of the surrounding microstructure has proven to be a key aspect in determining sites of failure initiation.

Shock loading is a complex phenomenon that can lead to failure mechanisms such as strain localization, void nucleation and growth, and eventually spall fracture. The length scale of damage with respect to that of the surrounding microstructure has proven to be a key aspect in determining sites of failure initiation. Studying incipient stages of spall damage is of paramount importance to accurately determine initiation sites in the material microstructure where damage will nucleate and grow and to formulate continuum models that account for the variability of the damage process due to microstructural heterogeneity, which is the focus of this research. Shock loading experiments were conducted via flyer-plate impact tests for pressures of 2-6 GPa and strain rates of 105/s on copper polycrystals of varying thermomechanical processing conditions. Serial cross sectioning of recovered target disks was performed along with electron microscopy, electron backscattering diffraction (EBSD), focused ion beam (FIB) milling, and 3-D X-ray tomogrpahy (XRT) to gain 2-D and 3-D information on the spall plane and surrounding microstructure. Statistics on grain boundaries (GB) containing damage were obtained from 2-D data and GBs of misorientations 25° and 50° were found to have the highest probability to contain damage in as-received (AR), heat treated (HT), and fully recrystallized (FR) microstructures, while {111} Σ3 GBs were globally strong. The AR microstructure’s probability peak was the most pronounced indicating GB strength is the dominant factor for damage nucleation. 3-D XRT data was used to digitally render the spall planes of the AR, HT, and FR microstructures. From shape fitting the voids to ellipsoids, it was found that the AR microstructure contained greater than 55% intergranular damage, whereas the HT and FR microstructures contained predominantly transgranular and coalesced damage modes, respectively. 3-D reconstructions of large volume damage sites in shocked Cu multicrystals showed preference for damage nucleation at GBs between adjacent grains of a high Taylor factor mismatches as well as an angle between the shock direction and the GB physical normal of ~30°-45°. 3-D FIB sectioning of individual voids led to the discovery of uniform plastic zones ~25-50% the size of the void diameter and plastic deformation directions were characterized via local average misorientation maps. Incipient transgranular voids revealed from the sectioning process were present in grains of high Taylor factors along the shock direction, which is expected as materials with a low Taylor factor along the shock direction are susceptible to growth due their accomodation of plastic deformation. Fabrication of square waves using photolithography and chemical etching was developed to study the nature of plasticity at GBs away from the spall plane. Grains oriented close to <0 1 1> had half the residual amplitudes than grains oriented close to <0 0 1>.
ContributorsBrown, Andrew (Author) / Peralta, Pedro (Committee member) / Mignolet, Marc (Committee member) / Sieradzki, Karl (Committee member) / Solanki, Kiran (Committee member) / Jiang, Hanqing (Committee member) / Arizona State University (Publisher)
Created2015
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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
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
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
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