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- All Subjects: Materials Science
- Creators: Chawla, Nikhilesh
- Creators: Alford, Terry L.
Description
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.
ContributorsBranch Kelly, Marion (Author) / Chawla, Nikhilesh (Thesis advisor) / Ankit, Kumar (Committee member) / Antoniswamy, Aravindha (Committee member) / Arizona State University (Publisher)
Created2019
Description
III-V-bismide semiconductor alloys are a class of materials with applications in the mid and long wave infrared spectrum. The quaternary alloy InAsSbBi is attractive because it can be grown lattice-matched to commercially available GaSb substrates, and the adjustment of the Bi and Sb mole fractions enables both lattice constant and bandgap to be tuned independently. This dissertation provides a comprehensive study of the surface morphology and the structural and chemical properties of InAsSbBi alloys grown by molecular beam epitaxy.
210 nm thick InAsSbBi layers grown at temperatures from 280 °C to 430 °C on (100) on-axis, (100) offcut 1° to (011), and (100) offcut 4° to (111)A GaSb substrates are investigated using Rutherford back scattering, X-ray diffraction, transmission electron microscopy, Nomarski optical microscopy, atomic force microscopy, and photoluminescence spectroscopy. The results indicate that the layers are coherently strained and contain dilute Bi mole fractions.
Large surface droplets with diameters and densities on the order of 3 µm and 106 cm-2 are observed when the growth is performed with As overpressures around 1%. Preferential orientation of the droplets occurs along the [011 ̅] step edges offcut (100) 1° to (011) substrate. The surface droplets are not observed when the As overpressure is increased to 4%. Small crystalline droplets with diameters and densities on the order of 70 nm and 1010 cm-2 are observed between the large droplets for the growth at 430°C. Analysis of one of the small droplets indicates a misoriented zinc blende structure composed of In, Sb, and Bi, with a 6.543 ± 0.038 Å lattice constant.
Lateral variation in the Bi mole fraction is observed in InAsSbBi grown at high temperature (400 °C, 420 °C) on (100) on-axis and (100) offcut 4° to (111)A substrates, but is not observed for growth at 280 °C or on (100) substrates that are offcut 1° to (011). Improved crystal and optical quality is observed in the high temperature grown InAsSbBi and CuPtB type atomic ordering on the {111}B planes is observed in the low temperature grown InAsSbBi. Strain induced tilt is observed in coherently strained InAsSbBi grown on offcut substrates.
210 nm thick InAsSbBi layers grown at temperatures from 280 °C to 430 °C on (100) on-axis, (100) offcut 1° to (011), and (100) offcut 4° to (111)A GaSb substrates are investigated using Rutherford back scattering, X-ray diffraction, transmission electron microscopy, Nomarski optical microscopy, atomic force microscopy, and photoluminescence spectroscopy. The results indicate that the layers are coherently strained and contain dilute Bi mole fractions.
Large surface droplets with diameters and densities on the order of 3 µm and 106 cm-2 are observed when the growth is performed with As overpressures around 1%. Preferential orientation of the droplets occurs along the [011 ̅] step edges offcut (100) 1° to (011) substrate. The surface droplets are not observed when the As overpressure is increased to 4%. Small crystalline droplets with diameters and densities on the order of 70 nm and 1010 cm-2 are observed between the large droplets for the growth at 430°C. Analysis of one of the small droplets indicates a misoriented zinc blende structure composed of In, Sb, and Bi, with a 6.543 ± 0.038 Å lattice constant.
Lateral variation in the Bi mole fraction is observed in InAsSbBi grown at high temperature (400 °C, 420 °C) on (100) on-axis and (100) offcut 4° to (111)A substrates, but is not observed for growth at 280 °C or on (100) substrates that are offcut 1° to (011). Improved crystal and optical quality is observed in the high temperature grown InAsSbBi and CuPtB type atomic ordering on the {111}B planes is observed in the low temperature grown InAsSbBi. Strain induced tilt is observed in coherently strained InAsSbBi grown on offcut substrates.
ContributorsKosireddy, Rajeev Reddy (Author) / Johnson, Shane R (Thesis advisor) / Smith, David J. (Committee member) / Alford, Terry L. (Committee member) / Soignard, Emmanuel (Committee member) / Arizona State University (Publisher)
Created2020
Description
Traditionally nanoporous gold is created by selective dissolution of silver or copper from a binary silver-gold or copper-gold alloy. These alloys serve as prototypical model systems for a phenomenon referred to as stress-corrosion cracking. Stress-corrosion cracking is the brittle failure of a normally ductile material occurring in a corrosive environment under a tensile stress. Silver-gold can experience this type of brittle fracture for a range of compositions. The corrosion process in this alloy results in a bicontinuous nanoscale morphology composed of gold-rich ligaments and voids often referred to as nanoporous gold. Experiments have shown that monolithic nanoporous gold can sustain high speed cracks which can then be injected into parent-phase alloy. This work compares nanoporous gold created from ordered and disordered copper-gold using digital image analysis and electron backscatter diffraction. Nanoporous gold from both disordered copper-gold and silver-gold, and ordered copper-gold show that grain orientation and shape remain largely unchanged by the dealloying process. Comparing the morphology of the nanoporous gold from ordered and disordered copper-gold with digital image analysis, minimal differences are found between the two and it is concluded that they are not statistically significant. This reveals the robust nature of nanoporous gold morphology against small variations in surface diffusion and parent-phase crystal structure.
Then the corrosion penetration down the grain boundary is compared to the depth of crack injections in polycrystal silver-gold. Based on statistical comparison, the crack-injections penetrate into the parent-phase grain boundary beyond the corrosion-induced porosity. To compare crack injections to stress-corrosion cracking, single crystal silver-gold samples are employed. Due to the cleavage-like nature of the fracture surfaces, electron backscatter diffraction is possible and employed to compare the crystallography of stress-corrosion crack surfaces and crack-injection surfaces. From the crystallographic similarities of these fracture surfaces, it is concluded that stress-corrosion can occur via a series of crack-injection events. This relationship between crack injections and stress corrosion cracking is further examined using electrochemical data from polycrystal silver-gold samples during stress-corrosion cracking. The results support the idea that crack injection is a mechanism for stress-corrosion cracking.
Then the corrosion penetration down the grain boundary is compared to the depth of crack injections in polycrystal silver-gold. Based on statistical comparison, the crack-injections penetrate into the parent-phase grain boundary beyond the corrosion-induced porosity. To compare crack injections to stress-corrosion cracking, single crystal silver-gold samples are employed. Due to the cleavage-like nature of the fracture surfaces, electron backscatter diffraction is possible and employed to compare the crystallography of stress-corrosion crack surfaces and crack-injection surfaces. From the crystallographic similarities of these fracture surfaces, it is concluded that stress-corrosion can occur via a series of crack-injection events. This relationship between crack injections and stress corrosion cracking is further examined using electrochemical data from polycrystal silver-gold samples during stress-corrosion cracking. The results support the idea that crack injection is a mechanism for stress-corrosion cracking.
ContributorsKarasz, Erin (Author) / Sieradzki, Karl (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Peralta, Pedro (Committee member) / Rajagopalan, Jagannathan (Committee member) / Arizona State University (Publisher)
Created2020
Description
Energy return in footwear is associated with the damping behavior of midsole foams, which stems from the combination of cellular structure and polymeric material behavior. Recently, traditional ethyl vinyl acetate (EVA) foams have been replaced by BOOST(TM) foams, thereby reducing the energetic cost of running. These are bead foams made from expanded thermoplastic polyurethane (eTPU), which have a multi-scale structure consisting of fused porous beads, at the meso-scale, and thousands of small closed cells within the beads at the micro-scale. Existing predictive models coarsely describe the macroscopic behavior but do not take into account strain localizations and microstructural heterogeneities. Thus, enhancement in material performance and optimization requires a comprehensive understanding of the foam’s cellular structure at all length scales and its influence on mechanical response.
This dissertation focused on characterization and deformation behavior of eTPU bead foams with a unique graded cell structure at the micro and meso-scale. The evolution of the foam structure during compression was studied using a combination of in situ lab scale and synchrotron x-ray tomography using a four-dimensional (4D, deformation + time) approach. A digital volume correlation (DVC) method was developed to elucidate the role of cell structure on local deformation mechanisms. The overall mechanical response was also studied ex situ to probe the effect of cell size distribution on the force-deflection behavior. The radial variation in porosity and ligament thickness profoundly influenced the global mechanical behavior. The correlation of changes in void size and shape helped in identifying potentially weak regions in the microstructure. Strain maps showed the initiation of failure in cell structure and it was found to be influenced by the heterogeneities around the immediate neighbors in a cluster of voids. Poisson’s ratio evaluated from DVC was related to the microstructure of the bead foams. The 4D approach taken here provided an in depth and mechanistic understanding of the material behavior, both at the bead and plate levels, that will be invaluable in designing the next generation of high-performance footwear.
This dissertation focused on characterization and deformation behavior of eTPU bead foams with a unique graded cell structure at the micro and meso-scale. The evolution of the foam structure during compression was studied using a combination of in situ lab scale and synchrotron x-ray tomography using a four-dimensional (4D, deformation + time) approach. A digital volume correlation (DVC) method was developed to elucidate the role of cell structure on local deformation mechanisms. The overall mechanical response was also studied ex situ to probe the effect of cell size distribution on the force-deflection behavior. The radial variation in porosity and ligament thickness profoundly influenced the global mechanical behavior. The correlation of changes in void size and shape helped in identifying potentially weak regions in the microstructure. Strain maps showed the initiation of failure in cell structure and it was found to be influenced by the heterogeneities around the immediate neighbors in a cluster of voids. Poisson’s ratio evaluated from DVC was related to the microstructure of the bead foams. The 4D approach taken here provided an in depth and mechanistic understanding of the material behavior, both at the bead and plate levels, that will be invaluable in designing the next generation of high-performance footwear.
ContributorsSundaram Singaravelu, Arun Sundar (Author) / Chawla, Nikhilesh (Thesis advisor) / Emady, Heather (Committee member) / Jiao, Yang (Committee member) / Arizona State University (Publisher)
Created2020
Description
The chemical, structural, and electrical properties of niobium-silicon, niobium-germanium, and YBCO-dielectric interfaces are characterized. Reduction in the concentration of interfacial defects in these structures can improve the performance of (i) many devices including low-loss coplanar, microstrip, and stripline microwave resonators used in next-generation cryogenic communication, sensor, and quantum information technologies and (ii) layers used in device isolation, inter-wiring dielectrics, and passivation in microwave and Josephson junction circuit fabrication.
Methods were developed to synthesize amorphous-Ge (a-Ge) and homoepitaxial-Si dielectric thin-films with loss tangents of 1–2×10 -6 and 0.6–2×10 -5 at near single-photon powers and sub-Kelvin temperatures (≈40 mK), making them potentially a better choice over undoped silicon and sapphire substrates used in quantum devices. The Nb/Ge interface has 20 nm of chemical intermixing, which is reduced by a factor of four using 10 nm Ta diffusion layers. Niobium coplanar resonators using this structure exhibit reduced microwave losses.
The nature and concentration of defects near Nb-Si interfaces prepared with commonly-used Si surface treatments were characterized. All samples have H, C, O, F, and Cl in the Si within 50 nm of the interface, and electrically active defects with activation energies of 0.147, 0.194, 0.247, 0.339, and 0.556 eV above the valence band maximum (E vbm ), with concentrations dominated by a hole trap at E vbm +0.556 eV (presumably Nb Si ). The optimum surface treatment is an HF etch followed by an in-situ 100 eV Ar ion mill. RCA etches, and higher energy ion milling processes increase the concentration of electrically active defects.
A thin SrTiO 3 buffer layer used in YBa 2 Cu 3 O 7-δ superconductor/high-performance Ba(Zn 1/3 Ta 2/3 )O 3 and Ba(Cd 1/3 Ta 2/3 )O 3 microwave dielectric trilayers improves the structural quality of the layers and results in 90 K superconductor critical temperatures. This advance enables the production of more compact high-temperature superconductor capacitors, inductors, and microwave microstrip and stripline devices.
Methods were developed to synthesize amorphous-Ge (a-Ge) and homoepitaxial-Si dielectric thin-films with loss tangents of 1–2×10 -6 and 0.6–2×10 -5 at near single-photon powers and sub-Kelvin temperatures (≈40 mK), making them potentially a better choice over undoped silicon and sapphire substrates used in quantum devices. The Nb/Ge interface has 20 nm of chemical intermixing, which is reduced by a factor of four using 10 nm Ta diffusion layers. Niobium coplanar resonators using this structure exhibit reduced microwave losses.
The nature and concentration of defects near Nb-Si interfaces prepared with commonly-used Si surface treatments were characterized. All samples have H, C, O, F, and Cl in the Si within 50 nm of the interface, and electrically active defects with activation energies of 0.147, 0.194, 0.247, 0.339, and 0.556 eV above the valence band maximum (E vbm ), with concentrations dominated by a hole trap at E vbm +0.556 eV (presumably Nb Si ). The optimum surface treatment is an HF etch followed by an in-situ 100 eV Ar ion mill. RCA etches, and higher energy ion milling processes increase the concentration of electrically active defects.
A thin SrTiO 3 buffer layer used in YBa 2 Cu 3 O 7-δ superconductor/high-performance Ba(Zn 1/3 Ta 2/3 )O 3 and Ba(Cd 1/3 Ta 2/3 )O 3 microwave dielectric trilayers improves the structural quality of the layers and results in 90 K superconductor critical temperatures. This advance enables the production of more compact high-temperature superconductor capacitors, inductors, and microwave microstrip and stripline devices.
ContributorsKopas, Cameron Joseph (Author) / Newman, Nathan (Thesis advisor) / Alford, Terry L. (Committee member) / Carpenter, Ray W (Committee member) / Williams, Peter (Committee member) / Arizona State University (Publisher)
Created2020
Description
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.
ContributorsNiverty, Sridhar (Author) / Chawla, Nikhilesh (Thesis advisor) / Liu, Yongming (Committee member) / Ankit, Kumar (Committee member) / Xiao, Xianghui (Committee member) / Arizona State University (Publisher)
Created2020
Description
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.
ContributorsGao, Tianxiang (Author) / Emady, Heather N (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Jiao, Yang (Committee member) / Pradhan, Shankali (Committee member) / Oka, Sarang (Committee member) / Arizona State University (Publisher)
Created2020
Description
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.
ContributorsVemulapalli, Sree Shivani (Author) / Ankit, Kumar (Thesis advisor) / Chawla, Nikhilesh (Committee member) / Singh, Arunima (Committee member) / Arizona State University (Publisher)
Created2020
Description
Layer-wise extrusion of soft-solid like cement pastes and mortars is commonly used in 3D printing of concrete. Rheological and mechanical characterization of the printable binder for on-demand flow and subsequent structuration is a critical challenge. This research is an effort to understand the mechanics of cementitious binders as soft solids in the fresh state, towards establishing material-process relationships to enhance print quality. This study introduces 3D printable binders developed based on rotational and capillary rheology test parameters, and establish the direct influence of packing coefficients, geometric ratio, slip velocities, and critical print velocities on the extrudate quality. The ratio of packing fraction to the square of average particle diameter (0.01-0.02), and equivalent microstructural index (5-20) were suitable for printing, and were directly related to the cohesion and extrusional yield stress of the material. In fact, steady state pressure for printing (30-40 kPa) is proportional to the extrusional yield stress, and increases with the geometric ratio (0-60) and print velocity (5-50 mm/s). Higher print velocities results in higher wall shear stresses and was exponentially related to the slip layer thickness (estimated between 1-5μ), while the addition of superplasticizers improve the slip layer thickness and the extrudate flow. However, the steady state pressure and printer capacity limits the maximum print velocity while the deadzone length limits the minimum velocity allowable (critical velocity regime) for printing. The evolution of buildability with time for the fresh state mortars was characterized with digital image correlation using compressive strain and strain rate in printed layers. The fresh state characteristics (interlayer and interfilamentous) and process parameters (layer height and fiber dimensions) influence the hardened mechanical properties. A lower layer height generally improves the mechanical properties and slight addition of fiber (up to 0.3% by volume) results in a 15-30% increase in the mechanical properties. 3D scanning and point-cloud analysis was also used to assess the geometric tolerance of a print based on mean error distances, print accuracy index, and layer-wise percent overlap. The research output will contribute to a synergistic material-process design and development of test methods for printability in the context of 3D printing of concrete.
ContributorsAmbadi Omanakuttan Nair, Sooraj Kumar (Author) / Neithalath, Narayanan (Thesis advisor) / Rajan, Subramaniam (Committee member) / Mobasher, Barzin (Committee member) / Hoover, Christian (Committee member) / Chawla, Nikhilesh (Committee member) / Arizona State University (Publisher)
Created2021