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.

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.

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

The current rapid pace of technological progress necessitates the demand for more resilient and high-performance alloys. To achieve this, a thorough understanding of the relationships between material properties and its structure is indispensable. To establish this correlation and achieve desired properties from structural alloys, microstructural response to mechanical stimuli needs to be understood in three-dimensions (3D). To that effect, in situ tests were conducted at the synchrotron (Advanced Photon Source) using Transmission X-Ray Microscopy as well as in a scanning electron microscope (SEM) to study real-time damage evolution in such alloys. Findings of precipitate size-dependent transition in deformation behavior from these tests have inspired a novel resilient aluminum alloy design.

This dissertation investigates the potential for enzyme induced carbonate cementation as an alternative to Portland cement for creating building material from sand aggregate. We create a solution of urease enzyme, calcium chloride (CaCl2), and urea in water and added sand. The urease catalyzes the synthesis of carbonate from urea, and the carbonate then bonds with a dissociated calcium ion and precipitates from the solution as calcium carbonate (CaCO3). This precipitate can form small crystal bridges at contacts between sand grains that lock the sand grains in place. Using enzyme induced carbonate precipitation we created a cemented sand sample with a maximum compressive strength of 319 kPa and an elastic modulus of approximately 10 MPa. Images from the SEM showed that a major failure mechanism in the cemented samples was the delamination of the CaCO3 from the sand grains. We observed that CaCO3 cementation did not when solutions with high concentrations of CaCl2 and urea were used.

Nanocrystalline (NC) and Ultrafine-grained (UFG) metal films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. These properties, such as very high strength, primarily arise from the change in the underlying deformation mechanisms. Experimental and simulation studies have shown that because of the small grain size, conventional dislocation plasticity is curtailed in these materials and grain boundary mediated mechanisms become more important. Although the deformation behavior and the underlying mechanisms in these materials have been investigated in depth, relatively little attention has been focused on the inhomogeneous nature of their microstructure (particularly originating from the texture of the film) and its influence on their macroscopic response. Furthermore, the rate dependency of mechanical response in NC/UFG metal films with different textures has not been systematically investigated. The objectives of this dissertation are two-fold.

The first objective is to carry out a systematic investigation of the mechanical behavior of NC/UFG thin films with different textures under different loading rates. This includes a novel approach to study the effect of texture-induced plastic anisotropy on mechanical behavior of the films. Efforts are made to correlate the behavior of UFG metal films and the underlying deformation mechanisms. The second objective is to understand the deformation mechanisms of UFG aluminum films using in-situ transmission electron microscopy (TEM) experiments with Automated Crystal Orientation Mapping. This technique enables us to investigate grain rotations in UFG Al films and to monitor the microstructural changes in these films during deformation, thereby revealing detailed information about the deformation mechanisms prevalent in UFG metal films.

Sn and Al alloys are widely used in various industries. Environmental-induced damage resulting in whiskering in Sn and corrosion in Al account for numerous failures globally every year. Therefore, for designing materials that can better withstand these failures, a comprehensive study on the characterization of the damage is necessary. This research implements advanced characterization techniques to study the above-mentioned environmental-induced damage in Sn and Al alloys.

Tin based films are known to be susceptible to whisker growth resulting in numerous failures. While the mechanisms and factors affecting whisker growth have been studied extensively, not much has been reported on the mechanical properties of tin whiskers themselves. This study focuses on the tensile behavior of tin whiskers. Tensile tests of whiskers were conducted in situ a dual beam focused ion beam (FIB) with a scanning electron microscope (SEM) using a micro electro-mechanical system (MEMS) tensile testing stage. The deformation mechanisms of whiskers were analyzed using transmission electron microscopy (TEM).

Due to the heterogenous nature of the microstructure of Al 7075, it is susceptible to corrosion forming corrosion products and pits. These can be sites for cracks nucleation and propagation resulting in stress corrosion cracking (SCC). Therefore, complete understanding of the corrosion damaged region and its effect on the strength of the alloy is necessary. Several studies have been performed to visualize pits and understand their effect on the mechanical performance of Al alloys using two-dimensional (2D) approaches which are often inadequate. To get a thorough understanding of the pits, it is necessary for three-dimensional (3D) studies. In this study, Al 7075 alloys were corroded in 3.5 wt.% NaCl solution and X-ray tomography was used to obtain the 3D microstructure of pits enabling the quantification of their dimensions accurately. Furthermore, microstructure and mechanical property correlations helped in a better understanding of the effect of corrosion. Apart from the pits, a surface corrosion layer also forms on Al. A subsurface damage layer has also been identified that forms due to the aggressive nature of NaCl. Energy dispersive X-ray spectroscopy (EDX) and nanoindentation helped in identifying this region and understanding the variation in properties.

An accurate knowledge of the complex microstructure of a heterogeneous material is crucial for quantitative structure-property relations establishment and its performance prediction and optimization. X-ray tomography has provided a non-destructive means for microstructure characterization in both 3D and 4D (i.e., structural evolution over time). Traditional reconstruction algorithms like filtered-back-projection (FBP) method or algebraic reconstruction techniques (ART) require huge number of tomographic projections and segmentation process before conducting microstructural quantification. This can be quite time consuming and computationally intensive.

In this thesis, a novel procedure is first presented that allows one to directly extract key structural information in forms of spatial correlation functions from limited x-ray tomography data. The key component of the procedure is the computation of a “probability map”, which provides the probability of an arbitrary point in the material system belonging to specific phase. The correlation functions of interest are then readily computed from the probability map. Using effective medium theory, accurate predictions of physical properties (e.g., elastic moduli) can be obtained.

Secondly, a stochastic optimization procedure that enables one to accurately reconstruct material microstructure from a small number of x-ray tomographic projections (e.g., 20 - 40) is presented. Moreover, a stochastic procedure for multi-modal data fusion is proposed, where both X-ray projections and correlation functions computed from limited 2D optical images are fused to accurately reconstruct complex heterogeneous materials in 3D. This multi-modal reconstruction algorithm is proved to be able to integrate the complementary data to perform an excellent optimization procedure, which indicates its high efficiency in using limited structural information.

Finally, the accuracy of the stochastic reconstruction procedure using limited X-ray projection data is ascertained by analyzing the microstructural degeneracy and the roughness of energy landscape associated with different number of projections. Ground-state degeneracy of a microstructure is found to decrease with increasing number of projections, which indicates a higher probability that the reconstructed configurations match the actual microstructure. The roughness of energy landscape can also provide information about the complexity and convergence behavior of the reconstruction for given microstructures and projection number.

Over the past several years, the density of integrated circuits has been increasing at a very fast rate, following Moore’s law. The advent of three dimensional (3D) packaging technologies enable the increase in density of integrated circuits without necessarily shrinking the dimensions of the device. Under such constraints, the solder volume necessary to join the various layers of the package is also extremely small. At smaller length scales, the local cooling rates are higher, so the microstructures are much finer than that obtained in larger joints (BGA, C4). The fraction of intermetallic compounds (IMCs) present in solder joints in these volumes will be larger. The Cu6Sn5 precipitate size and spacing, and Sn grain structure and crystallography will be different at very small volumes. These factors will most certainly affect the performance of the solder. Examining the mechanical behavior and reliability of Pb-free solders is difficult, primarily because a methodology to characterize the microstructure and the mechanics of deformation at these extremely small length scales has yet to be developed.

In this study, Sn grain orientation and Cu6Sn5 IMC fraction, size, and morphology are characterized in 3D, in pure Sn based solder joints. The obtained results show differences in morphology of Sn grains and IMC precipitates as a function of location within the solder joint indicating influence of local cooling rate differences. Ex situ and in situ electromigration tests done on 250 um and 500 um pure Sn solder joints elucidate the evolution of microstructure, specifically Sn grain growth, IMC segregation and surface degradation. This research implements 3D quantification of microstructural features over micro and nano-scales, thereby enabling a multi-scale / multi-characterization approach.