Investigating the Mechanical Behavior and Deformation Mechanisms of Ultrafine-grained Metal Films Using Ex-situ and In-situ TEM Techniques

155793-Thumbnail Image.png
Description
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

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.
Date Created
2017
Agent

Revealing Anelasticity and Structural Rearrangements in Nanoscale Metallic Glass Films Using In Situ TEM Diffraction

128378-Thumbnail Image.png
Description

We used a novel diffraction-based method to extract the local, atomic-level elastic strain in nanoscale amorphous TiAl films during in situ transmission electron microscopy deformation, while simultaneously measuring the macroscopic strain. The complementary strain measurements revealed significant anelastic deformation, which

We used a novel diffraction-based method to extract the local, atomic-level elastic strain in nanoscale amorphous TiAl films during in situ transmission electron microscopy deformation, while simultaneously measuring the macroscopic strain. The complementary strain measurements revealed significant anelastic deformation, which was independently confirmed by strain rate experiments. Furthermore, the distribution of first nearest-neighbor distances became narrower during loading and permanent changes were observed in the atomic structure upon unloading, even in the absence of macroscopic plasticity. The results demonstrate the capability of in situ electron diffraction to probe structural rearrangements and decouple elastic and anelastic deformation in metallic glasses.

Date Created
2016-09-22
Agent

Electron Beam Induced Artifacts During In Situ TEM Deformation of Nanostructured Metals

128551-Thumbnail Image.png
Description

A critical assumption underlying in situ transmission electron microscopy studies is that the electron beam (e-beam) exposure does not fundamentally alter the intrinsic deformation behavior of the materials being probed. Here, we show that e-beam exposure causes increased dislocation activation

A critical assumption underlying in situ transmission electron microscopy studies is that the electron beam (e-beam) exposure does not fundamentally alter the intrinsic deformation behavior of the materials being probed. Here, we show that e-beam exposure causes increased dislocation activation and marked stress relaxation in aluminum and gold films spanning a range of thicknesses (80–400 nanometers) and grain sizes (50–220 nanometers). Furthermore, the e-beam induces anomalous sample necking, which unusually depends more on the e-beam diameter than intensity. Notably, the stress relaxation in both aluminum and gold occurs at beam energies well below their damage thresholds. More remarkably, the stress relaxation and/or sample necking is significantly more pronounced at lower accelerating voltages (120 kV versus 200 kV) in both the metals. These observations in aluminum and gold, two metals with highly dissimilar atomic weights and properties, indicate that e-beam exposure can cause anomalous behavior in a broad spectrum of nanostructured materials, and simultaneously suggest a strategy to minimize such artifacts.

Date Created
2015-11-10
Agent

Environmental-induced damage in tin (Sn) and aluminum (Al) alloys

155602-Thumbnail Image.png
Description
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

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.
Date Created
2017
Agent

Characterization of the Dynamic Strength of Aluminium at Extreme Strain Rates and Pressures

155488-Thumbnail Image.png
Description
The study of response of various materials to intense dynamic loading events,

such as shock loading due to high-velocity impacts, is extremely important in a wide

variety of military and industrial applications. Shock loading triggers extreme states,

leading to high pressures and strain

The study of response of various materials to intense dynamic loading events,

such as shock loading due to high-velocity impacts, is extremely important in a wide

variety of military and industrial applications. Shock loading triggers extreme states,

leading to high pressures and strain rates, and neglecting strength is a typical

approximation under such conditions. However, recent results have shown that strength

effects are larger than expected, so they must be taken into account. Recently,

hydrodynamic instabilities, the most common being the Rayleigh-Taylor (RTI) and

Richtmyer-Meshkov (RMI) instabilities, have been used to infer the dynamic strength of

materials at high pressure conditions. In our experiments and simulations, a novel RMI

approach is used, in which periodic surface perturbations are made on high purity

aluminium target, which was laser ablated to create a rippled shock front. Due to the

slow linear growth rate of RMI, the evolution of the perturbations on the back surface of

the sample as a result of the rippled shock can be measured via Transient Imaging

Displacement Interferometry (TIDI). The velocity history at the free surface was

recorded by spatially resolved laser velocimetry. These measurements were compared

with the results from the simulations, which were implemented using rate independent

and rate dependent material models, to characterize the dynamic strength of the

material. Simulations using the elastic-perfectly plastic model, which is rate

independent, failed to provide a value of dynamic yield strength that would match

experimental measurements of perturbation amplitudes. The Preston-Tonks-Wallace

(PTW) model, which is rate dependent model, worked well for aluminium. This model

was, in turn, used as a reference for calibrating the rate dependent Steinberg-Lund

model and the results from simulations using the calibration models were also compared

to experimental measurements.
Date Created
2017
Agent

Creep-Fatigue Damage Investigation and Modeling of Alloy 617 at High Temperatures

155431-Thumbnail Image.png
Description
The Very High Temperature Reactor (VHTR) is one of six conceptual designs proposed for Generation IV nuclear reactors. Alloy 617, a solid solution strengthened Ni-base superalloy, is currently the primary candidate material for the tubing of the Intermediate Heat Exchanger

The Very High Temperature Reactor (VHTR) is one of six conceptual designs proposed for Generation IV nuclear reactors. Alloy 617, a solid solution strengthened Ni-base superalloy, is currently the primary candidate material for the tubing of the Intermediate Heat Exchanger (IHX) in the VHTR design. Steady-state operation of the nuclear power plant at elevated temperatures leads to creep deformation, whereas loading transients including startup and shutdown generate fatigue. A detailed understanding of the creep-fatigue interaction in Alloy 617 is necessary before it can be considered as a material for nuclear construction in ASME Boiler and Pressure Vessel Code. Current design codes for components undergoing creep-fatigue interaction at elevated temperatures require creep-fatigue testing data covering the entire range from fatigue-dominant to creep-dominant loading. Classical strain-controlled tests, which produce stress relaxation during the hold period, show a saturation in cycle life with increasing hold periods due to the rapid stress-relaxation of Alloy 617 at high temperatures. Therefore, applying longer hold time in these tests cannot generate creep-dominated failure. In this study, uniaxial isothermal creep-fatigue tests with non-traditional loading waveforms were designed and performed at 850 and 950°C, with an objective of generating test data in the creep-dominant regime. The new loading waveforms are hybrid strain-controlled and force-controlled testing which avoid stress relaxation during the creep hold. The experimental data showed varying proportions of creep and fatigue damage, and provided evidence for the inadequacy of the widely-used time fraction rule for estimating creep damage under creep-fatigue conditions. Micro-scale damage features in failed test specimens, such as fatigue cracks and creep voids, were quantified using a Scanning Electron Microscope (SEM) to find a correlation between creep and fatigue damage. Quantitative statistical imaging analysis showed that the microstructural damage features (cracks and voids) are correlated with a new mechanical driving force parameter. The results from this image-based damage analysis were used to develop a phenomenological life-prediction methodology called the effective time fraction approach. Finally, the constitutive creep-fatigue response of the material at 950°C was modeled using a unified viscoplastic model coupled with a damage accumulation model. The simulation results were used to validate an energy-based constitutive life-prediction model, as a mechanistic model for potential component and structure level creep-fatigue analysis.
Date Created
2017
Agent

CFD analysis of wind power potential across rooftop gaps of tall buildings

155407-Thumbnail Image.png
Description
This study uses Computational Fluid Dynamics (CFD) modeling to analyze the

dependence of wind power potential and turbulence intensity on aerodynamic design of a

special type of building with a nuzzle-like gap at its rooftop. Numerical simulations using

ANSYS Fluent are carried out

This study uses Computational Fluid Dynamics (CFD) modeling to analyze the

dependence of wind power potential and turbulence intensity on aerodynamic design of a

special type of building with a nuzzle-like gap at its rooftop. Numerical simulations using

ANSYS Fluent are carried out to quantify the above-mentioned dependency due to three

major geometric parameters of the building: (i) the height of the building, (ii) the depth of

the roof-top gap, and (iii) the width of the roof-top gap. The height of the building is varied

from 8 m to 24 m. Likewise, the gap depth is varied from 3 m to 5 m and the gap width

from 2 m to 4 m. The aim of this entire research is to relate these geometric parameters of

the building to the maximum value and the spatial pattern of wind power potential across

the roof-top gap. These outcomes help guide the design of the roof-top geometry for wind

power applications and determine the ideal position for mounting a micro wind turbine.

From these outcomes, it is suggested that the wind power potential is greatly affected by

the increasing gap width or gap depth. It, however, remains insensitive to the increasing

building height, unlike turbulence intensity which increases with increasing building

height. After performing a set of simulations with varying building geometry to quantify

the wind power potential before the installation of a turbine, another set of simulations is

conducted by installing a static turbine within the roof-top gap. The results from the latter

are used to further adjust the estimate of wind power potential. Recommendations are made

for future applications based on the findings from the numerical simulations.
Date Created
2017
Agent

Synthesis and in situ characterization of nanostructured and amorphous metallic films

Description
Nanocrystalline (nc) thin films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. Furthermore, the mechanical behavior and microstructure of nc films is intimately related. Thus, precise control of the size, aspect ratio and spatial

Nanocrystalline (nc) thin films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. Furthermore, the mechanical behavior and microstructure of nc films is intimately related. Thus, precise control of the size, aspect ratio and spatial distribution of grains can enable the synthesis of thin films with exceptional mechanical properties. However, conventional bottom-up techniques for synthesizing thin films are incapable of achieving the microstructural control required to explicitly tune their properties. This dissertation focuses on developing a novel technique to synthesize metallic alloy thin films with precisely controlled microstructures and subsequently characterizing their mechanical properties using in situ transmission electron microscopy (TEM). Control over the grain size and distribution was achieved by controlling the recrystallization process of amorphous films by the use of thin crystalline seed layers. The novel technique was used to manipulate the microstructure of structural (TiAl) and functional (NiTi) thin films thereby exhibiting its capability and versatility. Following the synthesis of thin films with tailored microstructures, in situ TEM techniques were employed to probe their mechanical properties. Firstly, a novel technique was developed to measure local atomic level elastic strains in metallic glass thin films during in situ TEM straining. This technique was used to detect structural changes and anelastic deformation in metallic glass thin films. Finally, as the electron beam (e-beam) in TEMs is known to cause radiation damage to specimen, systematic experiments were carried out to quantify the effect of the e-beam on the stress-strain response of nc metals. Experiments conducted on Al and Au films revealed that the e-beam enhances dislocation activity leading to stress relaxation.
Date Created
2017
Agent

In situ electromigration and reliability of Pb-free solders at extremely small length scales

155189-Thumbnail Image.png
Description
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

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.
Date Created
2016
Agent

3D modeling of void nucleation and initial void growth due to tin diffusion as a result of electromigration in polycrystalline lead-free solders

154995-Thumbnail Image.png
Description
Electromigration (EM) has been a serious reliability concern in microelectronics packaging for close to half a century now. Whenever the challenges of EM are overcome newer complications arise such as the demand for better performance due to increased miniaturization of

Electromigration (EM) has been a serious reliability concern in microelectronics packaging for close to half a century now. Whenever the challenges of EM are overcome newer complications arise such as the demand for better performance due to increased miniaturization of semiconductor devices or the problems faced due to undesirable properties of lead-free solders. The motivation for the work is that there exists no fully computational modeling study on EM damage in lead-free solders (and also in lead-based solders). Modeling techniques such as one developed here can give new insights on effects of different grain features and offer high flexibility in varying parameters and study the corresponding effects. In this work, a new computational approach has been developed to study void nucleation and initial void growth in solders due to metal atom diffusion. It involves the creation of a 3D stochastic mesoscale model of the microstructure of a polycrystalline Tin structure. The next step was to identify regions of current crowding or ‘hot-spots’. This was done through solving a finite difference scheme on top of the 3D structure. The nucleation of voids due to atomic diffusion from the regions of current crowding was modeled by diffusion from the identified hot-spot through a rejection free kinetic Monte-Carlo scheme. This resulted in the net movement of atoms from the cathode to the anode. The above steps of identifying the hotspot and diffusing the atoms at the hot-spot were repeated and this lead to the initial growth of the void. This procedure was studied varying different grain parameters. In the future, the goal is to explore the effect of more grain parameters and consider other mechanisms of failure such as the formation of intermetallic compounds due to interstitial diffusion and dissolution of underbump metallurgy.
Date Created
2016
Agent