AA 7XXX alloys are used extensively in aircraft and naval structures due to their excellent strength to weight ratio. These alloys are often exposed to harsh corrosive environments and mechanical stresses that can compromise their reliability in service. They are also coupled with fasteners that are composed of different materials such as Titanium alloys. Such dissimilar metal contact facilitates galvanic and crevice corrosion, which can further reduce their lifetimes. Despite decades of research in the area, the confluence of mechanical, microstructural, and electrochemical aspects of damage is still unclear. Traditionally, 2D and destructive methods have often been employed to study the corrosion and cracking behavior in these systems which can be severely limiting and lead to inaccurate conclusions. This dissertation is aimed at comprehensively studying the corrosion and cracking behavior of these systems using time-dependent 3D microstructural characterization, as well as correlative microscopy. The microstructural evolution of corrosion in AA 7075 was studied using a combination of potentiodynamic polarization, X-ray Computed Tomography (XCT) and Transmission X-ray Microscopy (TXM). In both experiments, a strong emphasis was placed on studying localized corrosion attack at constituent particles and intergranular corrosion. With an understanding of the alloy’s corrosion behavior, a dissimilar alloy couple comprising AA 7075 / Ti-6Al-4V was then investigated. Ex situ and in situ x-ray microtomography was used extensively to investigate the evolution of pitting corrosion and corrosion fatigue in AA 7075 plates fastened separately with Ti-6Al-4V screws and rivets. The 4D tomography combined with the extensive fractography yielded valuable information pertaining the preferred sites of pit initiation, crack initiation and growth in these complex geometries. The use of correlative microscopy-based methodologies yielded multimodal characterization results that provided a unique and seminal insight on corrosion mechanisms in these materials.

Single drop impact of liquid on a static powder bed was studied to investigate the granule formation mechanism, droplet penetration time, the characterization of granules (morphology, surface structure and internal structure), as well as the formation regime map. Water was used as the liquid and two pharmaceutical powders, microcrystalline cellulose (MCC) and acetaminophen (APAP), were mixed to make heterogeneous powder beds. The complete drop impact and penetration was recorded by a high-speed camera. Two granule formation mechanisms identified previously occurred: Spreading and Tunneling. Spreading occurred for mixtures of large particle sizes, while Tunneling started to occur when the particle sizes of the mixtures decreased. With an increase of APAP concentration, the overall drop penetration time increased, which was in good agreement with previous literature. The granule morphology, surface structure, and internal structure were characterized by a prism method with image analysis, scanning electron microscope, and X-ray microtomography, respectively. The Spreading mechanism produced flat disks with porous internal structures, while the Tunneling mechanism produced round granules with dense internal structures. Granules that were formed via a hybrid of the mechanisms, Spreading/Tunneling, were hybrid granules, with some dense areas and some porous areas. The results of the granule content uniformity from UV-vis spectrometry revealed that with the increase of APAP proportion, the overall uniformity was compromised for mixtures with fine ingredients, while the content was much more uniform for coarse mixtures. It is believed that the mean particle size of the powder bed is the predominant factor in influencing the formation mechanism, drop penetration time, and granule properties, while the content uniformity is affected by both the particle sizes and the mixture hydrophobicity.

There has been a renewed interest to understand the degradation mechanism of concrete under radiation as many nuclear reactors are reaching their expiration date. Much of the information on the degradation mechanism of concrete under radiation comes from the experiments, which are carried out on very small specimens. With the advent of finite element analysis, a numerical predictive tool is desired that can predict the extent of damage in the nuclear concrete structure.

A mesoscale micro-structural framework is proposed in Multiphysics Object-Oriented Simulation Environment (MOOSE) finite element framework which represents the first step in this direction. As part of the framework, a coupled creep damage algorithm was developed and implemented in MOOSE. The algorithm considers creep through rheological models, while damage evolves exponentially as a function of elastic strain and creep strain. A characteristic length is introduced in the formulation such that the energy release rate associated with each element remains the same to avoid vanishing energy dissipation with mesh refinement. A creep damage parameter quantifies the effect of creep strain on the damage that was calibrated using three-point bending experiments with varying rates of loading.

The creep damage model was also validated with restrained ring shrinkage tests on cementitious materials containing compliant/stiff inclusions subjected to variable drying conditions. The simulation approach explicitly considers: (i) moisture diffusion driven differential shrinkage along the depth of the specimen (ii) viscoelastic response of aging cementitious materials (iii) isotropic damage model with Rankine′s failure initiation criterion, and (iv) random distribution of tensile strengths of individual finite elements.

The model was finally validated with experimental results on neutron-irradiated concrete. The simulation approach considers: (i) coupled hygro-thermal model to predict the temperature and humidity profile inside the specimen (ii) radiation-induced volumetric expansion of aggregates (RIVE) (iii) thermal, shrinkage and creep effects based on the temperature and humidity profile and (iv) isotropic damage model with Rankine’s criterion to determine failure initiation.

Miniaturization of microdevices comes at the cost of increased circuit complexity and operating current densities. At high current densities, the resulting electron wind imparts a large momentum to metal ions triggering electromigration which leads to degradation of interconnects and solder, ultimately resulting in circuit failure. Although electromigration-induced defects in electronic materials can manifest in several forms, the formation of voids is a common occurrence. This research aims at understanding the morphological evolution of voids under electromigration by formulating a diffuse interface approach that accounts for anisotropic mobility in the metallic interconnect. Based on an extensive parametric study, this study reports the conditions under which pancaking of voids or the novel void ‘swimming’ regimes are observed. Finally, inferences are drawn to formulate strategies using which the reliability of interconnects can be improved.

Aluminum alloys are commonly used for engineering applications due to their high strength to weight ratio, low weight, and low cost. Pitting corrosion, accelerated by saltwater environments, leads to fatigue cracks and stress corrosion cracking during service. Two-dimensional (2D) characterization methods are typically used to identify and characterize corrosion; however, these methods are destructive and do not enable an efficient means of quantifying mechanisms of pit initiation and growth. In this study, lab-scale x-ray microtomography was used to non-destructively observe, quantify, and understand pit growth in three dimensions over a 20-day corrosion period in the AA7075-T651 alloy. The XRT process, capable of imaging sample volumes with a resolution near one micrometer, was found to be an ideal tool for large-volume pit examination. Pit depths were quantified over time using renderings of sample volumes, leading to an understanding of how inclusion particles, oxide breakdown, and corrosion mechanisms impact the growth and morphology of pits. This process, when carried out on samples produced with two different rolling directions and rolling extents, yielded novel insights into the long-term macroscopic corrosion behaviors impacted by alloy production and design. Key among these were the determinations that the alloy’s rolling direction produces a significant difference in the average growth rate of pits and that the corrosion product layer loses its passivating effect as a result of cyclic immersion. In addition, a new mechanism of pitting corrosion is proposed which is focused on the pseudo-random spatial distribution of iron-rich inclusion particles in the alloy matrix, which produces a random distribution of pit depths based on the occurrence of co-operative corrosion near inclusion clusters.

As the microelectronics industry continues to decrease the size of solder joints, each joint will have to carry a greater current density, making atom diffusion due to current flow, electromigration (EM), a problem of ever-increasing severity. The rate of EM damage depends on current density, operating temperature, and the original microstructure of the solder joint, including void volume, grain orientation, and grain size. While numerous studies have investigated the post-mortem effects of EM and have tested a range of current densities and temperatures, none have been able to analyze how the same joint evolves from its initial to final microstructure. This thesis focuses on the study of EM, thermal aging, and thermal cycling in Sn-rich solder joints. Solder joints were either of controlled microstructure and orientation or had trace alloying element additions. Sn grain orientation has been linked to a solder joints’ susceptibility to EM damage, but the precise relationship between orientation and intermetallic (IMC) and void growth has not been deduced. In this research x-ray microtomography was used to nondestructively scan samples and generate 3D reconstructions of both surface and internal features such as interfaces, IMC particles, and voids within a solder joint. Combined with controlled fabrication techniques to create comparable samples and electron backscatter diffraction (EBSD) and energy-dispersive spectroscopy (EDS) analysis for grain orientation and composition analysis, this work shows how grain structure plays a critical role in EM damage and how it differs from damage accrued from thermal effects that occur simultaneously. Unique IMC growth and voiding behaviors are characterized and explained in relation to the solder microstructures that cause their formation and the possible IMC-suppression effects of trace alloying element addition are discussed.

Weevils are among the most diverse and evolutionarily successful animal lineages on Earth. Their success is driven in part by a structure called the rostrum, which gives weevil heads a characteristic "snout-like" appearance. Nut weevils in the genus Curculio use the rostrum to drill holes into developing fruits and nuts, wherein they deposit their eggs. During oviposition this exceedingly slender structure is bent into a straightened configuration - in some species up to 90° - but does not suffer any damage during this process. The performance of the snout is explained in terms of cuticle biomechanics and rostral curvature, as presented in a series of four interconnected studies. First, a micromechanical constitutive model of the cuticle is defined to predict and reconstruct the mechanical behavior of each region in the exoskeleton. Second, the effect of increased endocuticle thickness on the stiffness and fracture strength of the rostrum is assessed using force-controlled tensile testing. In the third chapter, these studies are integrated into finite element models of the snout, demonstrating that the Curculio rostrum is only able to withstand repeated, extreme bending because of

modifications to the composite structure of the cuticle in the rostral apex. Finally, interspecific differences in the differential geometry of the snout are characterized to elucidate the role of biomechanical constraint in the evolution of rostral morphology for both males and females. Together these studies highlight the significance of cuticle biomechanics - heretofore unconsidered by others - as a source of constraint on the evolution of the rostrum and the mechanobiology of the genus Curculio.

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.

Being a remarkably versatile and inexpensive building material, concrete has found tremendous use in development of modern infrastructure and is the most widely used material in the world. Extensive research in the field of concrete has led to the development of a wide array of concretes with applications ranging from building of skyscrapers to paving of highways. These varied applications require special cementitious composites which can satisfy the demand for enhanced functionalities such as high strength, high durability and improved thermal characteristics among others.

The current study focuses on the fundamental understanding of such functional composites, from their microstructural design to macro-scale application. More specifically, this study investigates three different categories of functional cementitious composites. First, it discusses the differences between cementitious systems containing interground and blended limestone with and without alumina. The interground systems are found to outperform the blended systems due to differential grinding of limestone. A novel approach to deduce the particle size distribution of limestone and cement in the interground systems is proposed. Secondly, the study delves into the realm of ultra-high performance concrete, a novel material which possesses extremely high compressive-, tensile- and flexural-strength and service life as compared to regular concrete. The study presents a novel first principles-based paradigm to design economical ultra-high performance concretes using locally available materials. In the final part, the study addresses the thermal benefits of a novel type of concrete containing phase change materials. A software package was designed to perform numerical simulations to analyze temperature profiles and thermal stresses in concrete structures containing PCMs.

The design of these materials is accompanied by material characterization of cementitious binders. This has been accomplished using techniques that involve measurement of heat evolution (isothermal calorimetry), determination and quantification of reaction products (thermo-gravimetric analysis, x-ray diffraction, micro-indentation, scanning electron microscopy, energy-dispersive x-ray spectroscopy) and evaluation of pore-size distribution (mercury intrusion porosimetry). In addition, macro-scale testing has been carried out to determine compression, flexure and durability response. Numerical simulations have been carried out to understand hydration of cementitious composites, determine optimum particle packing and determine the thermal performance of these composites.

Additive manufacturing (AM) describes an array of methods used to create a 3D object layer by layer. The increasing popularity of AM in the past decade has been due to its demonstrated potential to increase design flexibility, produce rapid prototypes, and decrease material waste. Temporary supports are an inconvenient necessity in many metal AM parts. These sacrificial structures are used to fabricate large overhangs, anchor the part to the build substrate, and provide a heat pathway to avoid warping. Polymers AM has addressed this issue by using support material that is soluble in an electrolyte that the base material is not. In contrast, metals AM has traditionally approached support removal using time consuming, costly methods such as electrical discharge machining or a dremel.

This work introduces dissolvable supports to single- and multi-material metals AM. The multi-material approach uses material choice to design a functionally graded material where corrosion is the functionality being varied. The single-material approach is the primary focus of this thesis, leveraging already common post-print heat treatments to locally alter the microstructure near the surface. By including a sensitizing agent in the ageing heat treatment, carbon is diffused into the part decreasing the corrosion resistance to a depth equal to at least half the support thickness. In a properly chosen electrolyte, this layer is easily chemically, or electrochemically removed. Stainless steel 316 (SS316) and Inconel 718 are both investigated to study this process using two popular alloys. The microstructure evolution and corrosion properties are investigated for both. For SS316, the effect of applied electrochemical potential is investigated to describe the varying corrosion phenomena induced, and the effect of potential choice on resultant roughness. In summary, a new approach to remove supports from metal AM parts is introduced to decrease costs and further the field of metals AM by expanding the design space.