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Description
Dealloying induced stress corrosion cracking is particularly relevant in energy conversion systems (both nuclear and fossil fuel) as many failures in alloys such as austenitic stainless steel and nickel-based systems result directly from dealloying. This study provides evidence of the role of unstable dynamic fracture processes in dealloying induced stress-corrosion

Dealloying induced stress corrosion cracking is particularly relevant in energy conversion systems (both nuclear and fossil fuel) as many failures in alloys such as austenitic stainless steel and nickel-based systems result directly from dealloying. This study provides evidence of the role of unstable dynamic fracture processes in dealloying induced stress-corrosion cracking of face-centered cubic alloys. Corrosion of such alloys often results in the formation of a brittle nanoporous layer which we hypothesize serves to nucleate a crack that owing to dynamic effects penetrates into the un-dealloyed parent phase alloy. Thus, since there is essentially a purely mechanical component of cracking, stress corrosion crack propagation rates can be significantly larger than that predicted from electrochemical parameters. The main objective of this work is to examine and test this hypothesis under conditions relevant to stress corrosion cracking. Silver-gold alloys serve as a model system for this study since hydrogen effects can be neglected on a thermodynamic basis, which allows us to focus on a single cracking mechanism. In order to study various aspects of this problem, the dynamic fracture properties of monolithic nanoporous gold (NPG) were examined in air and under electrochemical conditions relevant to stress corrosion cracking. The detailed processes associated with the crack injection phenomenon were also examined by forming dealloyed nanoporous layers of prescribed properties on un-dealloyed parent phase structures and measuring crack penetration distances. Dynamic fracture in monolithic NPG and in crack injection experiments was examined using high-speed (106 frames s-1) digital photography. The tunable set of experimental parameters included the NPG length scale (20-40 nm), thickness of the dealloyed layer (10-3000 nm) and the electrochemical potential (0.5-1.5 V). The results of crack injection experiments were characterized using the dual-beam focused ion beam/scanning electron microscopy. Together these tools allow us to very accurately examine the detailed structure and composition of dealloyed grain boundaries and compare crack injection distances to the depth of dealloying. The results of this work should provide a basis for new mathematical modeling of dealloying induced stress corrosion cracking while providing a sound physical basis for the design of new alloys that may not be susceptible to this form of cracking. Additionally, the obtained results should be of broad interest to researchers interested in the fracture properties of nano-structured materials. The findings will open up new avenues of research apart from any implications the study may have for stress corrosion cracking.
ContributorsSun, Shaofeng (Author) / Sieradzki, Karl (Thesis advisor) / Jiang, Hanqing (Committee member) / Peralta, Pedro (Committee member) / Arizona State University (Publisher)
Created2012
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Description
The initial microstructure of oxide fuel pellets can play a key role in their performance. At low burnups, the transport of fission products has a strong dependence on oxygen content, grain size distribution, porosity and grain boundary (GB) characteristics (crystallography, geometry and topology), all of which, in turn depend on

The initial microstructure of oxide fuel pellets can play a key role in their performance. At low burnups, the transport of fission products has a strong dependence on oxygen content, grain size distribution, porosity and grain boundary (GB) characteristics (crystallography, geometry and topology), all of which, in turn depend on processing conditions. These microstructural features can also affect the fuel densification, thermal conductivity and microstructure evolution inside the reactor. Understanding these effects can provide insight into microstructure evolution of fuels in-pile. In this work, mechanical and ion beam serial sectioning techniques were developed to obtain Electron Backscatter Diffraction (EBSD) data, both in 2-D and 3-D, for depleted UO2+X pellets manufactured under different conditions. The EBSD maps were used to relate processing conditions to microstructural features, with emphasis on special GBs according to the Coincident Site Lattice (CSL) model, as well as correlations between pore size and location in the microstructure. Furthermore, larger grains (at least 2.5 times the average grain size) were observed in all the samples and studied. Results indicate that larger grains, in samples manufactured under different conditions, dominate the overall crystallographic texture and have a fairly strong GB texture. Moreover, it seems that the preferential misorientation axis for these GBs, regardless of the O/M, is {001}. These results might be related to GB energy and structure and, suggest that the mechanism that controls grain growth seems to be independent of both processing conditions and stoichiometry. Additionally, a sample was heat treated to relate grain growth and crystallography. The results indicate that at least two mechanisms were involved. Lengthening of GBs was observed for larger grains. Another mechanism of grain growth was observed, in this case, grains rotate to match a neighboring grain forming a larger grain. In the new grain, the misorientation between the two neighboring grains decreases to less than 5 degrees, forming a new larger grain. The results presented in this work indicate that detailed studies of the initial microstructure of the fuel, with emphasis on the crystallography of grains and GBs could help to give insights on the in-pile microstructural evolution of the fuel.
ContributorsRudman Prieto, Karin (Author) / Peralta, Pedro (Thesis advisor) / Ponce, Fernando (Committee member) / Sieradski, Karl (Committee member) / Arizona State University (Publisher)
Created2014
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Description
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
This research examines several critical aspects of the so-called "film induced cleavage" model of stress corrosion cracking using silver-gold alloys as the parent-phase material. The model hypothesizes that the corrosion generates a brittle nanoporous film, which subsequently fractures forming a high-speed crack that is injected into the uncorroded parent-phase alloy.

This research examines several critical aspects of the so-called "film induced cleavage" model of stress corrosion cracking using silver-gold alloys as the parent-phase material. The model hypothesizes that the corrosion generates a brittle nanoporous film, which subsequently fractures forming a high-speed crack that is injected into the uncorroded parent-phase alloy. This high speed crack owing to its kinetic energy can penetrate beyond the corroded layer into the parent phase and thus effectively reducing strength of the parent phase. Silver-gold alloys provide an ideal system to study this effect, as hydrogen effect can be ruled out on thermodynamic basis. During corrosion of the silver-gold alloy, the less noble metal i.e. silver is removed from the system leaving behind a nanoporous gold (NPG) layer. In the case of polycrystalline material, this corrosion process proceeds deeper along the grain boundary than the matrix grain. All of the cracks with apparent penetration beyond the corroded (dealloyed) layer are intergranular. Our aim was to study the crack penetration depth along the grain boundary to ascertain whether the penetration occurs past the grain-boundary dealloyed depth. EDS and imaging in high-resolution aberration corrected scanning transmission electron microscope (STEM) and atom probe tomography (APT) have been used to evaluate the grain boundary corrosion depth.

The mechanical properties of monolithic NPG are also studied. The motivation behind this is two-fold. The crack injection depth depends on the speed of the crack formed in the nanoporous layer, which in turn depends on the mechanical properties of the NPG. Also NPG has potential applications in actuation, sensing and catalysis. The measured value of the Young's modulus of NPG with 40 nm ligament size and 28% density was ~ 2.5 GPa and the Poisson's ratio was ~ 0.20. The fracture stress was observed to be ~ 11-13 MPa. There was no significant change observed between these mechanical properties on oxidation of NPG at 1.4 V. The fracture toughness value for the NPG was ~ 10 J/m2. Also dynamic fracture tests showed that the NPG is capable of supporting crack velocities ~ 100 - 180 m/s.
ContributorsBadwe, Nilesh (Author) / Sieradzki, Karl (Thesis advisor) / Peralta, Pedro (Committee member) / Oswald, Jay (Committee member) / Mahajan, Ravi (Committee member) / Arizona State University (Publisher)
Created2014
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Description
Commercially pure (CP) and extra low interstitial (ELI) grade Ti-alloys present excellent corrosion resistance, lightweight, and formability making them attractive materials for expanded use in transportation and medical applications. However, the strength and toughness of CP titanium are affected by relatively small variations in their impurity/solute content (IC), e.g., O,

Commercially pure (CP) and extra low interstitial (ELI) grade Ti-alloys present excellent corrosion resistance, lightweight, and formability making them attractive materials for expanded use in transportation and medical applications. However, the strength and toughness of CP titanium are affected by relatively small variations in their impurity/solute content (IC), e.g., O, Al, and V. This increase in strength is due to the fact that the solute either increases the critical stress required for the prismatic slip systems ({10-10}<1-210>) or activates another slip system ((0001)<11-20>, {10-11}<11-20>). In particular, solute additions such as O can effectively strengthen the alloy but with an attendant loss in ductility by changing the behavior from wavy (cross slip) to planar nature. In order to understand the underlying behavior of strengthening by solutes, it is important to understand the atomic scale mechanism. This dissertation aims to address this knowledge gap through a synergistic combination of density functional theory (DFT) and molecular dynamics. Further, due to the long-range strain fields of the dislocations and the periodicity of the DFT simulation cells, it is difficult to apply ab initio simulations to study the dislocation core structure. To alleviate this issue we developed a multiscale quantum mechanics/molecular mechanics approach (QM/MM) to study the dislocation core. We use the developed QM/MM method to study the pipe diffusion along a prismatic edge dislocation core. Complementary to the atomistic simulations, the Semi-discrete Variational Peierls-Nabarro model (SVPN) was also used to analyze the dislocation core structure and mobility. The chemical interaction between the solute/impurity and the dislocation core is captured by the so-called generalized stacking fault energy (GSFE) surface which was determined from DFT-VASP calculations. By taking the chemical interaction into consideration the SVPN model can predict the dislocation core structure and mobility in the presence and absence of the solute/impurity and thus reveal the effect of impurity/solute on the softening/hardening behavior in alpha-Ti. Finally, to study the interaction of the dislocation core with other planar defects such as grain boundaries (GB), we develop an automated method to theoretically generate GBs in HCP type materials.
ContributorsBhatia, Mehul Anoopkumar (Author) / Solanki, Kiran N (Thesis advisor) / Peralta, Pedro (Committee member) / Jiang, Hanqing (Committee member) / Neithalath, Narayanan (Committee member) / Rajagopalan, Jagannathan (Committee member) / Arizona State University (Publisher)
Created2014
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Description
The United States Department of Energy (DOE) has always held the safety and reliability of the nation's nuclear reactor fleet as a top priority. Continual improvements and advancements in nuclear fuels have been instrumental in maximizing energy generation from nuclear power plants and minimizing waste. One aspect of the DOE

The United States Department of Energy (DOE) has always held the safety and reliability of the nation's nuclear reactor fleet as a top priority. Continual improvements and advancements in nuclear fuels have been instrumental in maximizing energy generation from nuclear power plants and minimizing waste. One aspect of the DOE Fuel Cycle Research and Development Advanced Fuels Campaign is to improve the mechanical properties of uranium dioxide (UO2) for nuclear fuel applications.

In an effort to improve the performance of UO2, by increasing the fracture toughness and ductility, small quantities of oxide materials have been added to samples to act as dopants. The different dopants used in this study are: titanium dioxide, yttrium oxide, aluminum oxide, silicon dioxide, and chromium oxide. The effects of the individual dopants and some dopant combinations on the microstructure and mechanical properties are determined using indentation fracture experiments in tandem with scanning electron microscopy. Indentation fracture experiments are carried out at room temperature and at temperatures between 450 °C and 1160 °C.

The results of this work find that doping with aluminosilicate produces the largest favorable change in the mechanical properties of UO2. This sample exhibits an increase in fracture toughness at room temperature without showing a change in yield strength at elevated temperatures. The results also show that doping with Al2O3 and TiO2 produce stronger samples and it is hypothesized that this is a result of the sample containing dopant-rich secondary phase particles.
ContributorsMcDonald, Robert (Author) / Peralta, Pedro (Thesis advisor) / Rajagopalan, Jagannathan (Committee member) / Solanki, Kiran (Committee member) / Arizona State University (Publisher)
Created2014
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Description
ABSTRACT The behavior of the fission products, as they are released from fission events during nuclear reaction, plays an important role in nuclear fuel performance. Fission product release can occur through grain boundary (GB) at low burnups; therefore, this study simulates the mass transport of fission gases in a 2-D

ABSTRACT The behavior of the fission products, as they are released from fission events during nuclear reaction, plays an important role in nuclear fuel performance. Fission product release can occur through grain boundary (GB) at low burnups; therefore, this study simulates the mass transport of fission gases in a 2-D GB network to look into the effects of GB characteristics on this phenomenon, with emphasis on conditions that can lead to percolation. A finite element model was created based on the microstructure of a depleted UO2 sample characterized by Electron Backscattering Diffraction (EBSD). The GBs were categorized into high (D2), low (D1) and bulk diffusivity (Dbulk) based on their misorientation angles and Coincident Site Lattice (CSL) types. The simulation was run using different diffusivity ratios (D2/Dbulk) ranging from 1 to 10^8. The model was set up in three ways: constant temperature case, temperature gradient effects and window methods that mimic the environments in a Light Water Reactor (LWR). In general, the formation of percolation paths was observed at a ratio higher than 10^4 in the measured GB network, which had a 68% fraction of high diffusivity GBs. The presence of temperature gradient created an uneven concentration distribution and decreased the overall mass flux. Finally, radial temperature and fission gas concentration profiles were obtained for a fuel pellet in operation using an approximate 1-D model. The 100 µm long microstructurally explicit model was used to simulate, to the scale of a real UO2 pellet, the mass transport at different radial positions, with boundary conditions obtained from the profiles. Stronger percolation effects were observed at the intermediate and periphery position of the pellet. The results also showed that highest mass flux happens at the edge of a pellet at steady state to accommodate for the sharp concentration drop.
ContributorsLim, Harn Chyi (Author) / Peralta, Pedro (Thesis advisor) / Dey, Sandwip (Committee member) / Sieradzki, Karl (Committee member) / Arizona State University (Publisher)
Created2011
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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
The following is a report that will evaluate the microstructure of the nickel-based superalloy Hastelloy X and its relationship to mechanical properties in different load conditions. Hastelloy X is of interest to the company AORA because its strength and oxidation resistance at high temperatures is directly applicable to their needs

The following is a report that will evaluate the microstructure of the nickel-based superalloy Hastelloy X and its relationship to mechanical properties in different load conditions. Hastelloy X is of interest to the company AORA because its strength and oxidation resistance at high temperatures is directly applicable to their needs in a hybrid concentrated solar module. The literature review shows that the microstructure will produce different carbides at various temperatures, which can be beneficial to the strength of the alloy. These precipitates are found along the grain boundaries and act as pins that limit dislocation flow, as well as grain boundary sliding, and improve the rupture strength of the material. Over time, harmful precipitates form which counteract the strengthening effect of the carbides and reduce rupture strength, leading to failure. A combination of indentation and microstructure mapping was used in an effort to link local mechanical behavior to microstructure variability. Electron backscatter diffraction (EBSD) and energy dispersive spectroscopy (EDS) were initially used as a means to characterize the microstructure prior to testing. Then, a series of room temperature Vickers hardness tests at 50 and 500 gram-force were used to evaluate the variation in the local response as a function of indentation size. The room temperature study concluded that both the hardness and standard deviation increased at lower loads, which is consistent with the grain size distribution seen in the microstructure scan. The material was then subjected to high temperature spherical indentation. Load-displacement curves were essential in evaluating the decrease in strength of the material with increasing temperature. Through linear regression of the unloading portion of the curve, the plastic deformation was determined and compared at different temperatures as a qualitative method to evaluate local strength.
ContributorsCelaya, Andrew Jose (Author) / Peralta, Pedro (Thesis director) / Solanki, Kiran (Committee member) / Barrett, The Honors College (Contributor) / Mechanical and Aerospace Engineering Program (Contributor)
Created2015-05
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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