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Description
With the increasing focus on developing environmentally benign electronic packages, lead-free solder alloys have received a great deal of attention. Mishandling of packages, during manufacture, assembly, or by the user may cause failure of solder joint. A fundamental understanding of the behavior of lead-free solders under mechanical shock conditions is

With the increasing focus on developing environmentally benign electronic packages, lead-free solder alloys have received a great deal of attention. Mishandling of packages, during manufacture, assembly, or by the user may cause failure of solder joint. A fundamental understanding of the behavior of lead-free solders under mechanical shock conditions is lacking. Reliable experimental and numerical analysis of lead-free solder joints in the intermediate strain rate regime need to be investigated. This dissertation mainly focuses on exploring the mechanical shock behavior of lead-free tin-rich solder alloys via multiscale modeling and numerical simulations. First, the macroscopic stress/strain behaviors of three bulk lead-free tin-rich solders were tested over a range of strain rates from 0.001/s to 30/s. Finite element analysis was conducted to determine appropriate specimen geometry that could reach a homogeneous stress/strain field and a relatively high strain rate. A novel self-consistent true stress correction method is developed to compensate the inaccuracy caused by the triaxial stress state at the post-necking stage. Then the material property of micron-scale intermetallic was examined by micro-compression test. The accuracy of this measure is systematically validated by finite element analysis, and empirical adjustments are provided. Moreover, the interfacial property of the solder/intermetallic interface is investigated, and a continuum traction-separation law of this interface is developed from an atomistic-based cohesive element method. The macroscopic stress/strain relation and microstructural properties are combined together to form a multiscale material behavior via a stochastic approach for both solder and intermetallic. As a result, solder is modeled by porous plasticity with random voids, and intermetallic is characterized as brittle material with random vulnerable region. Thereafter, the porous plasticity fracture of the solders and the brittle fracture of the intermetallics are coupled together in one finite element model. Finally, this study yields a multiscale model to understand and predict the mechanical shock behavior of lead-free tin-rich solder joints. Different fracture patterns are observed for various strain rates and/or intermetallic thicknesses. The predictions have a good agreement with the theory and experiments.
ContributorsFei, Huiyang (Author) / Jiang, Hanqing (Thesis advisor) / Chawla, Nikhilesh (Thesis advisor) / Tasooji, Amaneh (Committee member) / Mobasher, Barzin (Committee member) / Rajan, Subramaniam D. (Committee member) / Arizona State University (Publisher)
Created2011
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Description
Ordered mesoporous materials have tunable pore sizes between 2 and 50 nm and are characterized by ordered pore structures and high surface areas (~1000 m2/g). This makes them particularly favorable for a number of membrane applications such as protein separation, polymer extrusion, nanowire fabrication and membrane reactors. These membranes can

Ordered mesoporous materials have tunable pore sizes between 2 and 50 nm and are characterized by ordered pore structures and high surface areas (~1000 m2/g). This makes them particularly favorable for a number of membrane applications such as protein separation, polymer extrusion, nanowire fabrication and membrane reactors. These membranes can be fabricated as top-layers on macroporous supports or as embedded membranes in a dense matrix. The first part of the work deals with the hydrothermal synthesis and water-vapor/oxygen separation properties of supported MCM-48 and a new Al-MCM-48 type membrane for potential use in air conditioning systems. Knudsen-type permeation is observed in these membranes. The combined effect of capillary condensation and the aluminosilicate matrix resulted in the highest separation factor (142) in Al-MCM-48 membranes, with a water vapor permeance of 6×10-8mol/m2Pas. The second part focuses on synthesis of embedded mesoporous silica membranes with helically ordered pores by a novel Counter Diffusion Self-Assembly (CDSA) method. This method is an extension of the interfacial synthesis method for fiber synthesis using tetrabutylorthosilicate (TBOS) and cetyltrimethylammonium bromide (CTAB) as the silica source and surfactant respectively. The initial part of this study determined the effect of TBOS height and humidity on fiber formation. From this study, the range of TBOS heights for best microscopic and macroscopic ordering were established. Next, the CDSA method was used to successfully synthesize membranes, which were characterized to have good support plugging and an ordered pore structure. Factors that influence membrane synthesis and plug microstructure were determined. SEM studies revealed the presence of gaps between the plugs and support pores, which occur due to shrinking of the plug on drying. Development of a novel liquid deposition method to seal these defects constituted the last part of this work. Post sealing, excess silica was removed by etching with hydrofluoric acid. Membrane quality was evaluated at each step using SEM and gas permeation measurements. After surfactant removal by liquid extraction, the membranes exhibited an O2 permeance of 1.65x10-6mol/m2.Pa.s and He/O2 selectivity of 3.30. The successful synthesis of this membrane is an exciting new development in the area of ordered mesoporous membrane technology.
ContributorsSeshadri, Shriya (Author) / Lin, Jerry Y. S. (Thesis advisor) / Dai, Lenore (Committee member) / Rege, Kaushal (Committee member) / Smith, David J. (Committee member) / Vogt, Bryan (Committee member) / Arizona State University (Publisher)
Created2011
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Description
Mesoporous materials that possess large surface area, tunable pore size, and ordered structures are attractive features for many applications such as adsorption, protein separation, enzyme encapsulation and drug delivery as these materials can be tailored to host different guest molecules. Films provide a model system to understand how the pore

Mesoporous materials that possess large surface area, tunable pore size, and ordered structures are attractive features for many applications such as adsorption, protein separation, enzyme encapsulation and drug delivery as these materials can be tailored to host different guest molecules. Films provide a model system to understand how the pore orientation impacts the potential for loading and release of selectively sized molecules. This research work aims to develop structure-property relationships to understand how pore size, geometry, and surface hydrophobicity influence the loading and release of drug molecules. In this study, the pore size is systematically varied by incorporating pore-swelling agent of polystyrene oligomers (hPS) to soft templated mesoporous carbon films fabricated by cooperative assembly of poly(styrene-block-ethylene oxide) (SEO) with phenolic resin. To examine the impact of morphology, different compositions of amphiphilic triblock copolymer templates, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) (PEO-PPO-PEO), are used to form two-dimensional hexagonal and cubic mesostructures. Lastly, the carbonization temperature provides a handle to tune the hydrophobicity of the film. These mesoporous films are then utilized to understand the uptake and release of a model drug Mitoxantrone dihydrochloride from nanostructured materials. The largest pore size (6nm) mesoporous carbon based on SEO exhibits the largest uptake (3.5μg/cm2); this is attributed to presence of larger internal volume compared to the other two films. In terms of release, a controlled response is observed for all films with the highest release for the 2nm cubic film (1.45 μg/cm2) after 15 days, but this is only 56 % of the drug loaded. Additionally, the surface hydrophobicity impacts the fraction of drug release with a decrease from 78% to 43%, as the films become more hydrophobic when carbonized at higher temperatures. This work provides a model system to understand how pore morphology, size and chemistry influence the drug loading and release for potential implant applications.
ContributorsLabiano, Alpha (Author) / Vogt, Bryan (Thesis advisor) / Rege, Kaushal (Committee member) / Dai, Lenore (Committee member) / Potta, Thrimoorthy (Committee member) / Arizona State University (Publisher)
Created2011
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Description
Biological membranes are critical to cell sustainability by selectively permeating polar molecules into the intracellular space and providing protection to the interior organelles. Biomimetic membranes (model cell membranes) are often used to fundamentally study the lipid bilayer backbone structure of the biological membrane. Lipid bilayer membranes are often supported using

Biological membranes are critical to cell sustainability by selectively permeating polar molecules into the intracellular space and providing protection to the interior organelles. Biomimetic membranes (model cell membranes) are often used to fundamentally study the lipid bilayer backbone structure of the biological membrane. Lipid bilayer membranes are often supported using inorganic materials in an effort to improve membrane stability and for application to novel biosensing platforms. Published literature has shown that a variety of dense inorganic materials with various surface properties have been investigated for the study of biomimetic membranes. However, literature does not adequately address the effect of porous materials or supports with varying macroscopic geometries on lipid bilayer membrane behavior. The objective of this dissertation is to present a fundamental study on the synthesis of lipid bilayer membranes supported by novel inorganic supports in an effort to expand the number of available supports for biosensing technology. There are two fundamental areas covered including: (1) synthesis of lipid bilayer membranes on porous inorganic materials and (2) synthesis and characterization of cylindrically supported lipid bilayer membranes. The lipid bilayer membrane formation behavior on various porous supports was studied via direct mass adsorption using a quartz crystal microbalance. Experimental results demonstrate significantly different membrane formation behaviors on the porous inorganic supports. A lipid bilayer membrane structure was formed only on SiO2 based surfaces (dense SiO2 and silicalite, basic conditions) and gamma-alumina (acidic conditions). Vesicle monolayer adsorption was observed on gamma-alumina (basic conditions), and yttria stabilized zirconia (YSZ) of varying roughness. Parameters such as buffer pH, surface chemistry and surface roughness were found to have a significant impact on the vesicle adsorption kinetics. Experimental and modeling work was conducted to study formation and characterization of cylindrically supported lipid bilayer membranes. A novel sensing technique (long-period fiber grating refractometry) was utilized to measure the formation mechanism of lipid bilayer membranes on an optical fiber. It was found that the membrane formation kinetics on the fiber was similar to its planar SiO2 counterpart. Fluorescence measurements verified membrane transport behavior and found that characterization artifacts affected the measured transport behavior.
ContributorsEggen, Carrie (Author) / Lin, Jerry Y.S. (Thesis advisor) / Dai, Lenore (Committee member) / Rege, Kaushal (Committee member) / Thornton, Trevor (Committee member) / Vogt, Bryan (Committee member) / Arizona State University (Publisher)
Created2011
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Description
Increasing demand for high strength powder metallurgy (PM) steels has resulted in the development of dual phase PM steels. In this work, the effects of thermal aging on the microstructure and mechanical behavior of dual phase precipitation hardened powder metallurgy (PM) stainless steels of varying ferrite-martensite content were examined. Quantitative

Increasing demand for high strength powder metallurgy (PM) steels has resulted in the development of dual phase PM steels. In this work, the effects of thermal aging on the microstructure and mechanical behavior of dual phase precipitation hardened powder metallurgy (PM) stainless steels of varying ferrite-martensite content were examined. Quantitative analyses of the inherent porosity and phase fractions were conducted on the steels and no significant differences were noted with respect to aging temperature. Tensile strength, yield strength, and elongation to fracture all increased with increasing aging temperature reaching maxima at 538oC in most cases. Increased strength and decreased ductility were observed in steels of higher martensite content. Nanoindentation of the individual microconstituents was employed to obtain a fundamental understanding of the strengthening contributions. Both the ferrite and martensite hardness values increased with aging temperature and exhibited similar maxima to the bulk tensile properties. Due to the complex non-uniform stresses and strains associated with conventional nanoindentation, micropillar compression has become an attractive method to probe local mechanical behavior while limiting strain gradients and contributions from surrounding features. In this study, micropillars of ferrite and martensite were fabricated by focused ion beam (FIB) milling of dual phase precipitation hardened powder metallurgy (PM) stainless steels. Compression testing was conducted using a nanoindenter equipped with a flat punch indenter. The stress-strain curves of the individual microconstituents were calculated from the load-displacement curves less the extraneous displacements of the system. Using a rule of mixtures approach in conjunction with porosity corrections, the mechanical properties of ferrite and martensite were combined for comparison to tensile tests of the bulk material, and reasonable agreement was found for the ultimate tensile strength. Micropillar compression experiments of both as sintered and thermally aged material allowed for investigation of the effect of thermal aging.
ContributorsStewart, Jennifer (Author) / Chawla, Nikhilesh (Thesis advisor) / Jiang, Hanqing (Committee member) / Krause, Stephen (Committee member) / Arizona State University (Publisher)
Created2011
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Description
The mechanical behavior of Pb-free solder alloys is important, since they must maintain mechanical integrity under thermomechanical fatigue, creep, and mechanical shock conditions. Mechanical shock, in particular, has become an increasing concern in the electronics industry, since electronic packages can be subjected to mechanical shock by mishandling during manufacture or

The mechanical behavior of Pb-free solder alloys is important, since they must maintain mechanical integrity under thermomechanical fatigue, creep, and mechanical shock conditions. Mechanical shock, in particular, has become an increasing concern in the electronics industry, since electronic packages can be subjected to mechanical shock by mishandling during manufacture or by accidental dropping. In this study, the mechanical shock behavior of Sn and Sn-Ag-Cu alloys was systematically analyzed over the strain rate range 10-3 - 30 s-1 in bulk samples, and over 10-3 - 12 s-1 on the single solder joint level. More importantly, the influences of solder microstructure and intermetallic compounds (IMC) on mechanical shock resistance were quantified. A thorough microstructural characterization of Sn-rich alloys was conducted using synchrotron x-ray computed tomography. The three-dimensional morphology and distribution of contiguous phases and precipitates was analyzed. A multiscale approach was utilized to characterize Sn-rich phases on the microscale with x-ray tomography and focused ion beam tomography to characterize nanoscale precipitates. A high strain rate servohydraulic test system was developed in conjunction with a modified tensile specimen geometry and a high speed camera for quantifying deformation. The effect of microstructure and applied strain rate on the local strain and strain rate distributions were quantified using digital image correlation. Necking behavior was analyzed using a novel mirror fixture, and the triaxial stresses associated with necking were corrected using a self-consistent method to obtain the true stress-true strain constitutive behavior. Fracture mechanisms were quantified as a function of strain rate. Finally, the relationship between solder microstructure and intermetallic compound layer thickness with the mechanical shock resistance of Sn-3.8Ag-0.7Cu solder joints was characterized. It was found that at low strain rates the dynamic solder joint strength was controlled by the solder microstructure, while at high strain rates it was controlled by the IMC layer. The influences of solder microstructure and IMC layer thickness were then isolated using extended reflow or isothermal aging treatments. It was found that at large IMC layer thicknesses the trend described above does not hold true. The fracture mechanisms associated with the dynamic solder joint strength regimes were analyzed.
ContributorsYazzie, Kyle (Author) / Chawla, Nikhilesh (Thesis advisor) / Sane, Sandeep (Committee member) / Jiang, Hanqing (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
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
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
Electromigration, the net atomic diffusion associated with the momentum transfer from electrons moving through a material, is a major cause of device and component failure in microelectronics. The deleterious effects from electromigration rise with increased current density, a parameter that will only continue to increase as our electronic devices get

Electromigration, the net atomic diffusion associated with the momentum transfer from electrons moving through a material, is a major cause of device and component failure in microelectronics. The deleterious effects from electromigration rise with increased current density, a parameter that will only continue to increase as our electronic devices get smaller and more compact. Understanding the dynamic diffusional pathways and mechanisms of these electromigration-induced and propagated defects can further our attempts at mitigating these failure modes. This dissertation provides insight into the relationships between these defects and parameters of electric field strength, grain boundary misorientation, grain size, void size, eigenstrain, varied atomic mobilities, and microstructure.First, an existing phase-field model was modified to investigate the various defect modes associated with electromigration in an equiaxed non-columnar microstructure. Of specific interest was the effect of grain boundary misalignment with respect to current flow and the mechanisms responsible for the changes in defect kinetics. Grain size, magnitude of externally applied electric field, and the utilization of locally distinct atomic mobilities were other parameters investigated. Networks of randomly distributed grains, a common microstructure of interconnects, were simulated in both 2- and 3-dimensions displaying the effects of 3-D capillarity on diffusional dynamics. Also, a numerical model was developed to study the effect of electromigration on void migration and coalescence. Void migration rates were found to be slowed from compressive forces and the nature of the deformation concurrent with migration was examined through the lens of chemical potential. Void migration was also validated with previously reported theoretical explanations. Void coalescence and void budding were investigated and found to be dependent on the magnitude of interfacial energy and electric field strength. A grasp on the mechanistic pathways of electromigration-induced defect evolution is imperative to the development of reliable electronics, especially as electronic devices continue to miniaturize. This dissertation displays a working understanding of the mechanistic pathways interconnects can fail due to electromigration, as well as provide direction for future research and understanding.
ContributorsFarmer, William McHann (Author) / Ankit, Kumar (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Jiao, Yang (Committee member) / McCue, Ian (Committee member) / Arizona State University (Publisher)
Created2022