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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

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
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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

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.
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
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Description
As one of the most promising materials for high capacity electrode in next generation of lithium ion batteries, silicon has attracted a great deal of attention in recent years. Advanced characterization techniques and atomic simulations helped to depict that the lithiation/delithiation of silicon electrode involves processes including large volume change

As one of the most promising materials for high capacity electrode in next generation of lithium ion batteries, silicon has attracted a great deal of attention in recent years. Advanced characterization techniques and atomic simulations helped to depict that the lithiation/delithiation of silicon electrode involves processes including large volume change (anisotropic for the initial lithiation of crystal silicon), plastic flow or softening of material dependent on composition, electrochemically driven phase transformation between solid states, anisotropic or isotropic migration of atomic sharp interface, and mass diffusion of lithium atoms. Motivated by the promising prospect of the application and underlying interesting physics, mechanics coupled with multi-physics of silicon electrodes in lithium ion batteries is studied in this dissertation. For silicon electrodes with large size, diffusion controlled kinetics is assumed, and the coupled large deformation and mass transportation is studied. For crystal silicon with small size, interface controlled kinetics is assumed, and anisotropic interface reaction is studied, with a geometry design principle proposed. As a preliminary experimental validation, enhanced lithiation and fracture behavior of silicon pillars via atomic layer coatings and geometry design is studied, with results supporting the geometry design principle we proposed based on our simulations. Through the work documented here, a consistent description and understanding of the behavior of silicon electrode is given at continuum level and some insights for the future development of the silicon electrode are provided.
ContributorsAn, Yonghao (Author) / Jiang, Hanqing (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Phelan, Patrick (Committee member) / Wang, Yinming (Committee member) / Yu, Hongyu (Committee member) / Arizona State University (Publisher)
Created2014
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Description
This report will review the mechanical and microstructural properties of the refractory element rhenium (Re) deposited using Laser Additive Manufacturing (LAM). With useable structural strength over 2200 °C, existing applications up to 2760 °C, very high strength, ductility and chemical resistance, interest in Re is understandable. This study includes data

This report will review the mechanical and microstructural properties of the refractory element rhenium (Re) deposited using Laser Additive Manufacturing (LAM). With useable structural strength over 2200 °C, existing applications up to 2760 °C, very high strength, ductility and chemical resistance, interest in Re is understandable. This study includes data about tensile properties including tensile data up to 1925 °C, fracture modes, fatigue and microstructure including deformation systems and potential applications of that information. The bulk mechanical test data will be correlated with nanoindentation and crystallographic examination. LAM properties are compared to the existing properties found in the literature for other manufacturing processes. The literature indicates that Re has three significant slip systems but also twins as part of its deformation mechanisms. While it follows the hcp metal characteristics for deformation, it has interesting and valuable extremes such as high work hardening, potentially high strength, excellent wear resistance and superior elevated temperature strength. These characteristics are discussed in detail.
ContributorsAdams, Robbie (Author) / Chawla, Nikhilesh (Thesis advisor) / Adams, James (Committee member) / Krause, Stephen (Committee member) / Arizona State University (Publisher)
Created2012
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Description
Pb-free solder joints are commonly used as interconnects in semiconductor packaging. One of the major defects affecting the mechanical performance of solder joints are reflow pores that form during processing. These pores exhibit significant variability in size and distribution, and understanding the effects of pore geometry on failure is an

Pb-free solder joints are commonly used as interconnects in semiconductor packaging. One of the major defects affecting the mechanical performance of solder joints are reflow pores that form during processing. These pores exhibit significant variability in size and distribution, and understanding the effects of pore geometry on failure is an important reliability concern. In this thesis, the pore microstructures of solder joint samples and the localized plastic deformation around individual pores was characterized in 3D using lab scale X-ray Microtomography. To observe the deformation of a solder joint in 3D, a solder joint was imaged with Microtomography after reflow and then deformed in shear in several loading steps with additional tomography data taken between each. The 3D tomography datasets were then segmented using the 3D Livewire technique into regions corresponding to solder and pores, and used to generate 3D models of the joint at each strain value using Mimics software. The extent of deformation of individual pores in the joint as a function of strain was quantified using sphericity measurements, and correlated with the observed cracking in the joint. In addition, the error inherent in the data acquisition and 3D modeling process was also quantified. The progression of damage observed with X-ray Microtomography was then used to validate the deformation and failure predicted by a Finite Element (FE) simulation. The FE model was based on the as-reflowed tomography data, and incorporated a ductile damage failure model to simulate fracture. Using the measured sphericity change and cracking information obtained from the tomography data, the FE model is shown to correctly capture the broad plastic deformation and strain localization seen in the actual joint, as well as the crack propagation. Lastly, Digital Image Correlation was investigated as a method of obtaining improved local strain measurements in 3D. This technique measures the displacement of the inherent microstructural features of the joint, and can give localized strain measurements that can be directly comparable to that predicted by modeling. The technique is demonstrated in 2D on Pb-Sn solder, and example 3D data is presented for future analysis.
ContributorsPadilla, Erick (Author) / Chawla, Nikhilesh (Thesis advisor) / Alford, Terry (Committee member) / Krause, Stephen (Committee member) / Arizona State University (Publisher)
Created2012
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Description
The objective of this research is to develop robust, accurate, and adaptive algorithms in the framework of the extended finite element method (XFEM) for fracture analysis of highly heterogeneous materials with complex internal geometries. A key contribution of this work is the creation of novel methods designed to automate the

The objective of this research is to develop robust, accurate, and adaptive algorithms in the framework of the extended finite element method (XFEM) for fracture analysis of highly heterogeneous materials with complex internal geometries. A key contribution of this work is the creation of novel methods designed to automate the incorporation of high-resolution data, e.g. from X-ray tomography, that can be used to better interpret the enormous volume of data generated in modern in-situ experimental testing. Thus new algorithms were developed for automating analysis of complex microstructures characterized by segmented tomographic images.

A centrality-based geometry segmentation algorithm was developed to accurately identify discrete inclusions and particles in composite materials where limitations in imaging resolution leads to spurious connections between particles in close contact.To allow for this algorithm to successfully segment geometry independently of particle size and shape, a relative centrality metric was defined to allow for a threshold centrality criterion for removal of voxels that spuriously connect distinct geometries.

To automate incorporation of microstructural information from high-resolution images, two methods were developed that initialize signed distance fields on adaptively-refined finite element meshes. The first method utilizes a level set evolution equation that is directly solved on the finite element mesh through Galerkins method. The evolution equation is formulated to produce a signed distance field that matches geometry defined by a set of voxels segmented from tomographic images. The method achieves optimal convergence for the order of elements used. In a second approach, the fast marching method is employed to initialize a distance field on a uniform grid which is then projected by least squares onto a finite element mesh. This latter approach is shown to be superior in speed and accuracy.

Lastly, extended finite element method simulations are performed for the analysis of particle fracture in metal matrix composites with realistic particle geometries initialized from X-ray tomographic data. In the simulations, particles fracture probabilistically through a Weibull strength distribution. The model is verified through comparisons with the experimentally-measured stress-strain response of the material as well as analysis of the fracture. Further, simulations are then performed to analyze the effect of mesh sensitivity, the effect of fracture of particles on their neighbors, and the role of a particles shape on its fracture probability.
ContributorsYuan, Rui (Author) / Oswald, Jay (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Liu, Yongming (Committee member) / Solanki, Kiran (Committee member) / Chen, Kangping (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
7XXX Aluminum alloys have high strength to weight ratio and low cost. They are used in many critical structural applications including automotive and aerospace components. These applications frequently subject the alloys to static and cyclic loading in service. Additionally, the alloys are often subjected to aggressive corrosive environments such as

7XXX Aluminum alloys have high strength to weight ratio and low cost. They are used in many critical structural applications including automotive and aerospace components. These applications frequently subject the alloys to static and cyclic loading in service. Additionally, the alloys are often subjected to aggressive corrosive environments such as saltwater spray. These chemical and mechanical exposures have been known to cause premature failure in critical applications. Hence, the microstructural behavior of the alloys under combined chemical attack and mechanical loading must be characterized further. Most studies to date have analyzed the microstructure of the 7XXX alloys using two dimensional (2D) techniques. While 2D studies yield valuable insights about the properties of the alloys, they do not provide sufficiently accurate results because the microstructure is three dimensional and hence its response to external stimuli is also three dimensional (3D). Relevant features of the alloys include the grains, subgrains, intermetallic inclusion particles, and intermetallic precipitate particles. The effects of microstructural features on corrosion pitting and corrosion fatigue of aluminum alloys has primarily been studied using 2D techniques such as scanning electron microscopy (SEM) surface analysis along with post-mortem SEM fracture surface analysis to estimate the corrosion pit size and fatigue crack initiation site. These studies often limited the corrosion-fatigue testing to samples in air or specialized solutions, because samples tested in NaCl solution typically have fracture surfaces covered in corrosion product. Recent technological advancements allow observation of the microstructure, corrosion and crack behavior of aluminum alloys in solution in three dimensions over time (4D). In situ synchrotron X-Ray microtomography was used to analyze the corrosion and cracking behavior of the alloy in four dimensions to elucidate crack initiation at corrosion pits for samples of multiple aging conditions and impurity concentrations. Additionally, chemical reactions between the 3.5 wt% NaCl solution and the crack surfaces were quantified by observing the evolution of hydrogen bubbles from the crack. The effects of the impurity particles and age-hardening particles on the corrosion and fatigue properties were examined in 4D.
ContributorsStannard, Tyler (Author) / Chawla, Nikhilesh (Thesis advisor) / Solanki, Kiran N (Committee member) / Goswami, Ramasis (Committee member) / Liu, Yongming (Committee member) / Arizona State University (Publisher)
Created2017
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Description
Increasing density of microelectronic packages, results in an increase in thermal and mechanical stresses within the various layers of the package. To accommodate the high-performance demands, the materials used in the electronic package would also require improvement. Specifically, the damage that often occurs in solders that function as die-attachment and

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

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

High operating temperature power electronics use wide band-gap semiconductor devices (Silicon Carbide/Gallium Nitride). The operating temperature of these devices can exceed 250oC, preventing use of traditional Sn-solders as Thermal Interface materials (TIM). At high temperature, the thermomechanical stresses can severely degrade the reliability and life of the device. In this light, new non-destructive approach is needed to understand the damage mechanism when subjected to reliability tests such as thermal cycling. In this work, sintered nano-Silver was identified as a promising high temperature TIM. Sintered nano-Silver samples were fabricated and their shear strength was evaluated. Thermal cycling tests were conducted and damage evolution was characterized using a lab scale 3D X-ray system to periodically assess changes in the microstructure such as cracks, voids, and porosity in the TIM layer. The evolution of microstructure and the effect of cycling temperature during thermal cycling are discussed.
ContributorsLujan Regalado, Irene (Author) / Chawla, Nikhilesh (Thesis advisor) / Frear, Darrel (Committee member) / Rajagopalan, Jagannathan (Committee member) / Jiao, Yang (Committee member) / Arizona State University (Publisher)
Created2018
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Description
Nanolaminate materials are layered composites with layer thickness ≤ 100 nm. They exhibit unique properties due to their small length scale, the presence of a high number of interfaces and the effect of imposed constraint. This thesis focuses on the mechanical behavior of Al/SiC nanolaminates. The high strength of ceramics

Nanolaminate materials are layered composites with layer thickness ≤ 100 nm. They exhibit unique properties due to their small length scale, the presence of a high number of interfaces and the effect of imposed constraint. This thesis focuses on the mechanical behavior of Al/SiC nanolaminates. The high strength of ceramics combined with the ductility of Al makes this combination desirable. Al/SiC nanolaminates were synthesized through magnetron sputtering and have an overall thickness of ~ 20 μm which limits the characterization techniques to microscale testing methods. A large amount of work has already been done towards evaluating their mechanical properties under indentation loading and micropillar compression. The effects of temperature, orientation and layer thickness have been well established. Al/SiC nanolaminates exhibited a flaw dependent deformation, anisotropy with respect to loading direction and strengthening due to imposed constraint. However, the mechanical behavior of nanolaminates under tension and fatigue loading has not yet been studied which is critical for obtaining a complete understanding of their deformation behavior. This thesis fills this gap and presents experiments which were conducted to gain an insight into the behavior of nanolaminates under tensile and cyclic loading. The effect of layer thickness, tension-compression asymmetry and effect of a wavy microstructure on mechanical response have been presented. Further, results on in situ micropillar compression using lab-based X-ray microscope through novel experimental design are also presented. This was the first time when a resolution of 50 nms was achieved during in situ micropillar compression in a lab-based setup. Pores present in the microstructure were characterized in 3D and sites of damage initiation were correlated with the channel of pores present in the microstructure.

The understanding of these deformation mechanisms paved way for the development of co-sputtered Al/SiC composites. For these composites, Al and SiC were sputtered together in a layer. The effect of change in the atomic fraction of SiC on the microstructure and mechanical properties were evaluated. Extensive microstructural characterization was performed at the nanoscale level and Al nanocrystalline aggregates were observed dispersed in an amorphous matrix. The modulus and hardness of co- sputtered composites were much higher than their traditional counterparts owing to denser atomic packing and the absence of synthesis induced defects such as pores and columnar boundaries.
ContributorsSingh, Somya (Author) / Chawla, Nikhilesh (Thesis advisor) / Neithalath, Narayanan (Committee member) / Jiao, Yang (Committee member) / Mara, Nathan (Committee member) / Arizona State University (Publisher)
Created2018