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- Creators: Chawla, Nikhilesh
- Creators: Sieradzki, Karl
- Creators: Barrett, The Honors College
- Creators: Rajagopalan, Jagannathan
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 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
Description
The work presented in this thesis covers the synthesis and characterization of an ionomer that is applicable to zinc-air batteries. Polysulfone polymer is first chloromethylated and then quaternized to create an ion-conducting polymer. Nuclear magnetic resonance (NMR) spectra indicates that the degree of chloromethylation was 114%. The chemical and physical properties that were investigated include: the ionic conductivity, ion exchange capacity, water retention capacity, diameter and thickness swelling ratios, porosity, glass transition temperature, ionic conductivity enhanced by free salt addition, and the concentration and diffusivity of oxygen within the ionomer. It was found that the fully hydrated hydroxide form of the ionomer had a room temperature ionic conductivity of 39.92mS/cm while the chloride form had a room temperature ionic conductivity of 11.80mS/cm. The ion exchange capacity of the ionomer was found to be 1.022mmol/g. The water retention capacity (WRC) of the hydroxide form was found to be 172.6% while the chloride form had a WRC of 67.9%. The hydroxide form of the ionomer had a diameter swelling ratio of 34% and a thickness swelling ratio of 55%. The chloride form had a diameter swelling ratio of 32% and a thickness swelling ratio of 28%. The largest pore size in the ionomer was found to be 32.6nm in diameter. The glass transition temperature of the ionomer is speculated to be 344°C. A definite measurement could not be made. The room temperature ionic conductivity at 50% relative humidity was improved to 12.90mS/cm with the addition of 80% free salt. The concentration and diffusivity of oxygen in the ionomer was found to be 1.3 ±0.2mMol and (0.49 ±0.15)x10-5 cm2/s respectively. The ionomer synthesized in this research had material properties and performance that is comparable to other ionomers reported in the literature. This is an indication that this ionomer is suitable for further study and integration into a zinc-air battery. This thesis is concluded with suggestions for future research that is focused on improving the performance of the ionomer as well as improving the methodology.
ContributorsPadilla, Manuel (Author) / Friesen, Cody A (Thesis advisor) / Buttry, Daniel (Committee member) / Sieradzki, Karl (Committee member) / Arizona State University (Publisher)
Created2012
Description
Dealloying, the selective dissolution of an elemental component from an alloy, is an important corrosion mechanism and a technological significant means to fabricate nanoporous structures for a variety of applications. In noble metal alloys, dealloying proceeds above a composition dependent critical potential, and bi-continuous structure evolves "simultaneously" as a result of the interplay between percolation dissolution and surface diffusion. In contrast, dealloying in alloys that show considerable solid-state mass transport at ambient temperature is largely unexplored despite its relevance to nanoparticle catalysts and Li-ion anodes. In my dissertation, I discuss the behaviors of two alloy systems in order to elucidate the role of bulk lattice diffusion in dealloying. First, Mg-Cd alloys are chosen to show that when the dealloying is controlled by bulk diffusion, a new type of porosity - negative void dendrites will form, and the process mirrors electrodeposition. Then, Li-Sn alloys are studied with respect to the composition, particle size and dealloying rate effects on the morphology evolution. Under the right condition, dealloying of Li-Sn supported by percolation dissolution results in the same bi-continuous structure as nanoporous noble metals; whereas lattice diffusion through the otherwise "passivated" surface allows for dealloying with no porosity evolution. The interactions between bulk diffusion, surface diffusion and dissolution are revealed by chronopotentiometry and linear sweep voltammetry technics. The better understanding of dealloying from these experiments enables me to construct a brief review summarizing the electrochemistry and morphology aspects of dealloying as well as offering interpretations to new observations such as critical size effect and encased voids in nanoporous gold. At the end of the dissertation, I will describe a preliminary attempt to generalize the morphology evolution "rules of dealloying" to all solid-to-solid interfacial controlled phase transition process, demonstrating that bi-continuous morphologies can evolve regardless of the nature of parent phase.
ContributorsChen, Qing (Author) / Sieradzki, Karl (Thesis advisor) / Friesen, Cody (Committee member) / Buttry, Daniel (Committee member) / Chan, Candace (Committee member) / Arizona State University (Publisher)
Created2013
Description
Aluminum alloys and their composites are attractive materials for applications requiring high strength-to-weight ratios and reasonable cost. Many of these applications, such as those in the aerospace industry, undergo fatigue loading. An understanding of the microstructural damage that occurs in these materials is critical in assessing their fatigue resistance. Two distinct experimental studies were performed to further the understanding of fatigue damage mechanisms in aluminum alloys and their composites, specifically fracture and plasticity. Fatigue resistance of metal matrix composites (MMCs) depends on many aspects of composite microstructure. Fatigue crack growth behavior is particularly dependent on the reinforcement characteristics and matrix microstructure. The goal of this work was to obtain a fundamental understanding of fatigue crack growth behavior in SiC particle-reinforced 2080 Al alloy composites. In situ X-ray synchrotron tomography was performed on two samples at low (R=0.1) and at high (R=0.6) R-ratios. The resulting reconstructed images were used to obtain three-dimensional (3D) rendering of the particles and fatigue crack. Behaviors of the particles and crack, as well as their interaction, were analyzed and quantified. Four-dimensional (4D) visual representations were constructed to aid in the overall understanding of damage evolution. During fatigue crack growth in ductile materials, a plastic zone is created in the region surrounding the crack tip. Knowledge of the plastic zone is important for the understanding of fatigue crack formation as well as subsequent growth behavior. The goal of this work was to quantify the 3D size and shape of the plastic zone in 7075 Al alloys. X-ray synchrotron tomography and Laue microdiffraction were used to non-destructively characterize the volume surrounding a fatigue crack tip. The precise 3D crack profile was segmented from the reconstructed tomography data. Depth-resolved Laue patterns were obtained using differential-aperture X-ray structural microscopy (DAXM), from which peak-broadening characteristics were quantified. Plasticity, as determined by the broadening of diffracted peaks, was mapped in 3D. Two-dimensional (2D) maps of plasticity were directly compared to the corresponding tomography slices. A 3D representation of the plastic zone surrounding the fatigue crack was generated by superimposing the mapped plasticity on the 3D crack profile.
ContributorsHruby, Peter (Author) / Chawla, Nikhilesh (Thesis advisor) / Solanki, Kiran (Committee member) / Liu, Yongming (Committee member) / Arizona State University (Publisher)
Created2014
Description
In engineering, buckling is mechanical instability of walls or columns under compression and usually is a problem that engineers try to prevent. In everyday life buckles (wrinkles) on different substrates are ubiquitous -- from human skin to a rotten apple they are a commonly observed phenomenon. It seems that buckles with macroscopic wavelengths are not technologically useful; over the past decade or so, however, thanks to the widespread availability of soft polymers and silicone materials micro-buckles with wavelengths in submicron to micron scale have received increasing attention because it is useful for generating well-ordered periodic microstructures spontaneously without conventional lithographic techniques. This thesis investigates the buckling behavior of thin stiff films on soft polymeric substrates and explores a variety of applications, ranging from optical gratings, optical masks, energy harvest to energy storage. A laser scanning technique is proposed to detect micro-strain induced by thermomechanical loads and a periodic buckling microstructure is employed as a diffraction grating with broad wavelength tunability, which is spontaneously generated from a metallic thin film on polymer substrates. A mechanical strategy is also presented for quantitatively buckling nanoribbons of piezoelectric material on polymer substrates involving the combined use of lithographically patterning surface adhesion sites and transfer printing technique. The precisely engineered buckling configurations provide a route to energy harvesters with extremely high levels of stretchability. This stiff-thin-film/polymer hybrid structure is further employed into electrochemical field to circumvent the electrochemically-driven stress issue in silicon-anode-based lithium ion batteries. It shows that the initial flat silicon-nanoribbon-anode on a polymer substrate tends to buckle to mitigate the lithiation-induced stress so as to avoid the pulverization of silicon anode. Spontaneously generated submicron buckles of film/polymer are also used as an optical mask to produce submicron periodic patterns with large filling ratio in contrast to generating only ~100 nm edge submicron patterns in conventional near-field soft contact photolithography. This thesis aims to deepen understanding of buckling behavior of thin films on compliant substrates and, in turn, to harness the fundamental properties of such instability for diverse applications.
ContributorsMa, Teng (Author) / Jiang, Hanqing (Thesis advisor) / Yu, Hongyu (Committee member) / Yu, Hongbin (Committee member) / Poon, Poh Chieh Benny (Committee member) / Rajagopalan, Jagannathan (Committee member) / Arizona State University (Publisher)
Created2014
Description
Concrete is the most widely used infrastructure material worldwide. Production of portland cement, the main binding component in concrete, has been shown to require significant energy and account for approximately 5-7% of global carbon dioxide production. The expected continued increased use of concrete over the coming decades indicates this is an ideal time to implement sustainable binder technologies. The current work aims to explore enhanced sustainability concretes, primarily in the context of limestone and flow. Aspects such as hydration kinetics, hydration product formation and pore structure add to the understanding of the strength development and potential durability characteristics of these binder systems. Two main strategies for enhancing this sustainability are explored in this work: (i) the use of high volume limestone in combination with other alternative cementitious materials to decrease the portland cement quantity in concrete and (ii) the use of geopolymers as the binder phase in concrete. The first phase of the work investigates the use of fine limestone as cement replacement from the perspective of hydration, strength development, and pore structure. The nature of the potential synergistic benefit of limestone and alumina will be explored. The second phase will focus on the rheological characterization of these materials in the fresh state, as well as a more general investigation of the rheological characterization of suspensions. The results of this work indicate several key ideas. (i) There is a potential synergistic benefit for strength, hydration, and pore structure by using alumina and in portland limestone cements, (ii) the limestone in these systems is shown to react to some extent, and fine limestone is shown to accelerate hydration, (iii) rheological characteristics of cementitious suspensions are complex, and strongly dependent on several key parameters including: the solid loading, interparticle forces, surface area of the particles present, particle size distribution of the particles, and rheological nature of the media in which the particles are suspended, and (iv) stress plateau method is proposed for the determination of rheological properties of concentrated suspensions, as it more accurately predicts apparent yield stress and is shown to correlate well with other viscoelastic properties of the suspensions.
ContributorsVance, Kirk (Author) / Neithalath, Narayanan (Thesis advisor) / Rajan, Subramaniam D. (Committee member) / Mobasher, Barzin (Committee member) / Chawla, Nikhilesh (Committee member) / Marzke, Robert (Committee member) / Arizona State University (Publisher)
Created2014
Description
For decades, microelectronics manufacturing has been concerned with failures related to electromigration phenomena in conductors experiencing high current densities. The influence of interconnect microstructure on device failures related to electromigration in BGA and flip chip solder interconnects has become a significant interest with reduced individual solder interconnect volumes. A survey indicates that x-ray computed micro-tomography (µXCT) is an emerging, novel means for characterizing the microstructures' role in governing electromigration failures. This work details the design and construction of a lab-scale µXCT system to characterize electromigration in the Sn-0.7Cu lead-free solder system by leveraging in situ imaging.
In order to enhance the attenuation contrast observed in multi-phase material systems, a modeling approach has been developed to predict settings for the controllable imaging parameters which yield relatively high detection rates over the range of x-ray energies for which maximum attenuation contrast is expected in the polychromatic x-ray imaging system. In order to develop this predictive tool, a model has been constructed for the Bremsstrahlung spectrum of an x-ray tube, and calculations for the detector's efficiency over the relevant range of x-ray energies have been made, and the product of emitted and detected spectra has been used to calculate the effective x-ray imaging spectrum. An approach has also been established for filtering `zinger' noise in x-ray radiographs, which has proven problematic at high x-ray energies used for solder imaging. The performance of this filter has been compared with a known existing method and the results indicate a significant increase in the accuracy of zinger filtered radiographs.
The obtained results indicate the conception of a powerful means for the study of failure causing processes in solder systems used as interconnects in microelectronic packaging devices. These results include the volumetric quantification of parameters which are indicative of both electromigration tolerance of solders and the dominant mechanisms for atomic migration in response to current stressing. This work is aimed to further the community's understanding of failure-causing electromigration processes in industrially relevant material systems for microelectronic interconnect applications and to advance the capability of available characterization techniques for their interrogation.
In order to enhance the attenuation contrast observed in multi-phase material systems, a modeling approach has been developed to predict settings for the controllable imaging parameters which yield relatively high detection rates over the range of x-ray energies for which maximum attenuation contrast is expected in the polychromatic x-ray imaging system. In order to develop this predictive tool, a model has been constructed for the Bremsstrahlung spectrum of an x-ray tube, and calculations for the detector's efficiency over the relevant range of x-ray energies have been made, and the product of emitted and detected spectra has been used to calculate the effective x-ray imaging spectrum. An approach has also been established for filtering `zinger' noise in x-ray radiographs, which has proven problematic at high x-ray energies used for solder imaging. The performance of this filter has been compared with a known existing method and the results indicate a significant increase in the accuracy of zinger filtered radiographs.
The obtained results indicate the conception of a powerful means for the study of failure causing processes in solder systems used as interconnects in microelectronic packaging devices. These results include the volumetric quantification of parameters which are indicative of both electromigration tolerance of solders and the dominant mechanisms for atomic migration in response to current stressing. This work is aimed to further the community's understanding of failure-causing electromigration processes in industrially relevant material systems for microelectronic interconnect applications and to advance the capability of available characterization techniques for their interrogation.
ContributorsMertens, James Charles Edwin (Author) / Chawla, Nikhilesh (Thesis advisor) / Alford, Terry (Committee member) / Jiao, Yang (Committee member) / Neithalath, Narayanan (Committee member) / Arizona State University (Publisher)
Created2015
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 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.
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
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, 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
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 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.
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