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- All Subjects: Materials Science
- Creators: Smith, David J.
- Creators: Rajagopalan, Jagannathan
Description
The alkali activation of aluminosilicate materials as binder systems derived from industrial byproducts have been extensively studied due to the advantages they offer in terms enhanced material properties, while increasing sustainability by the reuse of industrial waste and byproducts and reducing the adverse impacts of OPC production. Fly ash and ground granulated blast furnace slag are commonly used for their content of soluble silica and aluminate species that can undergo dissolution, polymerization with the alkali, condensation on particle surfaces and solidification. The following topics are the focus of this thesis: (i) the use of microwave assisted thermal processing, in addition to heat-curing as a means of alkali activation and (ii) the relative effects of alkali cations (K or Na) in the activator (powder activators) on the mechanical properties and chemical structure of these systems. Unsuitable curing conditions instigate carbonation, which in turn lowers the pH of the system causing significant reductions in the rate of fly ash activation and mechanical strength development. This study explores the effects of sealing the samples during the curing process, which effectively traps the free water in the system, and allows for increased aluminosilicate activation. The use of microwave-curing in lieu of thermal-curing is also studied in order to reduce energy consumption and for its ability to provide fast volumetric heating. Potassium-based powder activators dry blended into the slag binder system is shown to be effective in obtaining very high compressive strengths under moist curing conditions (greater than 70 MPa), whereas sodium-based powder activation is much weaker (around 25 MPa). Compressive strength decreases when fly ash is introduced into the system. Isothermal calorimetry is used to evaluate the early hydration process, and to understand the reaction kinetics of the alkali powder activated systems. A qualitative evidence of the alkali-hydroxide concentration of the paste pore solution through the use of electrical conductivity measurements is also presented, with the results indicating the ion concentration of alkali is more prevalent in the pore solution of potassium-based systems. The use of advanced spectroscopic and thermal analysis techniques to distinguish the influence of studied parameters is also discussed.
ContributorsChowdhury, Ussala (Author) / Neithalath, Narayanan (Thesis advisor) / Rajan, Subramanium D. (Committee member) / Mobasher, Barzin (Committee member) / Arizona State University (Publisher)
Created2013
Description
This dissertation is on the study of structural and optical properties of some III-V and II-VI compound semiconductors. The first part of this dissertation is a study of the deformation mechanisms associated with nanoindentation and nanoscratching of InP, GaN, and ZnO crystals. The second part is an investigation of some fundamental issues regarding compositional fluctuations and microstructure in GaInNAs and InAlN alloys. In the first part, the microstructure of (001) InP scratched in an atomic force microscope with a small diamond tip has been studied as a function of applied normal force and crystalline direction in order to understand at the nanometer scale the deformation mechanisms in the zinc-blende structure. TEM images show deeper dislocation propagation for scratches along <110> compared to <100>. High strain fields were observed in <100> scratches, indicating hardening due to locking of dislocations gliding on different slip planes. Reverse plastic flow have been observed in <110> scratches in the form of pop-up events that result from recovery of stored elastic strain. In a separate study, nanoindentation-induced plastic deformation has been studied in c-, a-, and m-plane ZnO single crystals and c-plane GaN respectively, to study the deformation mechanism in wurtzite hexagonal structures. TEM results reveal that the prime deformation mechanism is slip on basal planes and in some cases, on pyramidal planes, and strain built up along particular directions. No evidence of phase transformation or cracking was observed in both materials. CL imaging reveals quenching of near band-edge emission by dislocations. In the second part, compositional inhomogeneity in quaternary GaInNAs and ternary InAlN alloys has been studied using TEM. It is shown that exposure to antimony during growth of GaInNAs results in uniform chemical composition in the epilayer, as antimony suppresses the surface mobility of adatoms that otherwise leads to two-dimensional growth and elemental segregation. In a separate study, compositional instability is observed in lattice-matched InAlN films grown on GaN, for growth beyond a certain thickness. Beyond 200 nm of thickness, two sub-layers with different indium content are observed, the top one with lower indium content.
ContributorsHuang, Jingyi (Author) / Ponce, Fernando A. (Thesis advisor) / Carpenter, Ray W (Committee member) / Smith, David J. (Committee member) / Yu, Hongbin (Committee member) / Treacy, Michael Mj (Committee member) / Arizona State University (Publisher)
Created2013
Description
High electron mobility transistors (HEMTs) based on Group III-nitride heterostructures have been characterized by advanced electron microscopy methods including off-axis electron holography, nanoscale chemical analysis, and electrical measurements, as well as other techniques. The dissertation was organized primarily into three topical areas: (1) characterization of near-gate defects in electrically stressed AlGaN/GaN HEMTs, (2) microstructural and chemical analysis of the gate/buffer interface of AlN/GaN HEMTs, and (3) studies of the impact of laser-liftoff processing on AlGaN/GaN HEMTs. The electrical performance of stressed AlGaN/GaN HEMTs was measured and the devices binned accordingly. Source- and drain-side degraded, undegraded, and unstressed devices were then prepared via focused-ion-beam milling for examination. Defects in the near-gate region were identified and their correlation to electrical measurements analyzed. Increased gate leakage after electrical stressing is typically attributed to "V"-shaped defects at the gate edge. However, strong evidence was found for gate metal diffusion into the barrier layer as another contributing factor. AlN/GaN HEMTs grown on sapphire substrates were found to have high electrical performance which is attributed to the AlN barrier layer, and robust ohmic and gate contact processes. TEM analysis identified oxidation at the gate metal/AlN buffer layer interface. This thin a-oxide gate insulator was further characterized by energy-dispersive x-ray spectroscopy and energy-filtered TEM. Attributed to this previously unidentified layer, high reverse gate bias up to −30 V was demonstrated and drain-induced gate leakage was suppressed to values of less than 10−6 A/mm. In addition, extrinsic gm and ft * LG were improved to the highest reported values for AlN/GaN HEMTs fabricated on sapphire substrates. Laser-liftoff (LLO) processing was used to separate the active layers from sapphire substrates for several GaN-based HEMT devices, including AlGaN/GaN and InAlN/GaN heterostructures. Warpage of the LLO samples resulted from relaxation of the as-grown strain and strain arising from dielectric and metal depositions, and this strain was quantified by both Newton's rings and Raman spectroscopy methods. TEM analysis demonstrated that the LLO processing produced no detrimental effects on the quality of the epitaxial layers. TEM micrographs showed no evidence of either damage to the ~2 μm GaN epilayer generated threading defects.
ContributorsJohnson, Michael R. (Author) / Mccartney, Martha R (Thesis advisor) / Smith, David J. (Committee member) / Goodnick, Stephen (Committee member) / Shumway, John (Committee member) / Chen, Tingyong (Committee member) / Arizona State University (Publisher)
Created2012
Description
HgCdTe is currently the dominant material for infrared sensing and imaging, and is usually grown on lattice-matched bulk CdZnTe (CZT) substrates. There have been significant recent efforts to identify alternative substrates to CZT as well as alternative detector materials to HgCdTe. In this dissertation research, a wide range of transmission electron microscopy (TEM) imaging and analytical techniques was used in the characterization of epitaxial HgCdTe and related materials and substrates for third generation IR detectors. ZnTe layers grown on Si substrates are considered to be promising candidates for lattice-matched, large-area, and low-cost composite substrates for deposition of II-VI and III-V compound semiconductors with lattice constants near 6.1 Å. After optimizing MBE growth conditions including substrate pretreatment prior to film growth, as well as nucleation and growth temperatures, thick ZnTe/Si films with high crystallinity, low defect density, and excellent surface morphology were achieved. Changes in the Zn/Te flux ratio used during growth were also investigated. Small-probe microanalysis confirmed that a small amount of As was present at the ZnTe/Si interface. A microstructural study of HgCdTe/CdTe/GaAs (211)B and CdTe/GaAs (211)B heterostructures grown using MBE was carried out. High quality MBE-grown CdTe on GaAs(211)B substrates was demonstrated to be a viable composite substrate platform for HgCdTe growth. In addition, analysis of interfacial misfit dislocations and residual strain showed that the CdTe/GaAs interface was fully relaxed. In the case of HgCdTe/CdTe/ GaAs(211)B, thin HgTe buffer layers between HgCdTe and CdTe were also investigated for improving the HgCdTe crystal quality. A set of ZnTe layers epitaxially grown on GaSb(211)B substrates using MBE was studied using high resolution X-ray diffraction (HRXRD) measurements and TEM characterization in order to investigate conditions for defect-free growth. HRXRD results gave critical thickness estimates between 350 nm and 375 nm, in good agreement with theoretical predictions. Moreover, TEM results confirmed that ZnTe layers with thicknesses of 350 nm had highly coherent interfaces and very low dislocation densities, unlike samples with the thicker ZnTe layers.
ContributorsKim, Jae Jin (Author) / Smith, David J. (Thesis advisor) / McCartney, Martha R. (Committee member) / Alford, Terry L. (Committee member) / Crozier, Peter A. (Committee member) / Arizona State University (Publisher)
Created2012
Description
In engineering, buckling is mechanical instability of walls or columns under compression and usually is a problem that engineers try to prevent. In everyday life buckles (wrinkles) on different substrates are ubiquitous -- from human skin to a rotten apple they are a commonly observed phenomenon. It seems that buckles with macroscopic wavelengths are not technologically useful; over the past decade or so, however, thanks to the widespread availability of soft polymers and silicone materials micro-buckles with wavelengths in submicron to micron scale have received increasing attention because it is useful for generating well-ordered periodic microstructures spontaneously without conventional lithographic techniques. This thesis investigates the buckling behavior of thin stiff films on soft polymeric substrates and explores a variety of applications, ranging from optical gratings, optical masks, energy harvest to energy storage. A laser scanning technique is proposed to detect micro-strain induced by thermomechanical loads and a periodic buckling microstructure is employed as a diffraction grating with broad wavelength tunability, which is spontaneously generated from a metallic thin film on polymer substrates. A mechanical strategy is also presented for quantitatively buckling nanoribbons of piezoelectric material on polymer substrates involving the combined use of lithographically patterning surface adhesion sites and transfer printing technique. The precisely engineered buckling configurations provide a route to energy harvesters with extremely high levels of stretchability. This stiff-thin-film/polymer hybrid structure is further employed into electrochemical field to circumvent the electrochemically-driven stress issue in silicon-anode-based lithium ion batteries. It shows that the initial flat silicon-nanoribbon-anode on a polymer substrate tends to buckle to mitigate the lithiation-induced stress so as to avoid the pulverization of silicon anode. Spontaneously generated submicron buckles of film/polymer are also used as an optical mask to produce submicron periodic patterns with large filling ratio in contrast to generating only ~100 nm edge submicron patterns in conventional near-field soft contact photolithography. This thesis aims to deepen understanding of buckling behavior of thin films on compliant substrates and, in turn, to harness the fundamental properties of such instability for diverse applications.
ContributorsMa, Teng (Author) / Jiang, Hanqing (Thesis advisor) / Yu, Hongyu (Committee member) / Yu, Hongbin (Committee member) / Poon, Poh Chieh Benny (Committee member) / Rajagopalan, Jagannathan (Committee member) / Arizona State University (Publisher)
Created2014
Description
The research described in this dissertation involved the use of transmission electron microscopy (TEM) to characterize II-VI and III-V compound semiconductor quantum dots (QDs) and dilute-nitride alloys grown by molecular beam epitaxy (MBE) and intended for photovoltaic applications. The morphology of CdTe QDs prepared by the post-annealing MBE method were characterized by various microscopy techniques including high-resolution transmission electron microscopy (HR-TEM), and high-angle annular-dark-field scanning transmission electron microscopy (HAADF-STEM). Extensive observations revealed that the of QD shapes were not well-defined, and the QD size and spatial distribution were not determined by the amount of CdTe deposition. These results indicated that the formation of II-VI QDs using a post-annealing treatment did not follow the conventional growth mechanism for III-V and IV-IV materials. The structural properties of dilute-nitride GaAsNx films grown using plasma-assisted MBE were characterized by TEM and HAADF-STEM. A significant amount of the nitrogen incorporated into the dilute nitride films was found to be interstitial, and that fluctuations in local nitrogen composition also occurred during growth. Post-growth partial relaxation of strain resulted in the formation of {110}-oriented microcracks in the sample with the largest substitutional nitrogen composition. Single- and multi-layered InAs QDs grown on GaAsSb/GaAs composite substrates were investigated using HR-TEM and HAADF-STEM. Correlation between the structural and optoelectronic properties revealed that the GaAsSb barrier layers had played an important role in tuning the energy-band alignments but without affecting the overall structural morphology. However, according to both XRD measurement and electron microscopy the densities of dislocations increased as the number of QD layers built up. An investigation of near-wetting layer-free InAs QDs incorporated with AlAs/GaAs spacer layers was carried out. The microscopy observations revealed that both embedded and non-embedded near-wetting layer-free InAs QDs did not have well-defined shapes unlike conventional InAs QDs. According to AFM analysis and plan-view TEM characterization, the InAs QDs incorporated with spacer layers had smaller dot density and more symmetrical larger sizes with an apparent bimodal size distribution (two distinct families of large and small dots) in comparison with conventional InAs QDs grown without any spacer layer.
ContributorsTang, Dinghao (Author) / Smith, David J. (Thesis advisor) / Crozier, Peter A. (Committee member) / Liu, Jingyue (Committee member) / Mccartney, Martha R (Committee member) / Arizona State University (Publisher)
Created2014
Description
Concrete is the most widely used infrastructure material worldwide. Production of portland cement, the main binding component in concrete, has been shown to require significant energy and account for approximately 5-7% of global carbon dioxide production. The expected continued increased use of concrete over the coming decades indicates this is an ideal time to implement sustainable binder technologies. The current work aims to explore enhanced sustainability concretes, primarily in the context of limestone and flow. Aspects such as hydration kinetics, hydration product formation and pore structure add to the understanding of the strength development and potential durability characteristics of these binder systems. Two main strategies for enhancing this sustainability are explored in this work: (i) the use of high volume limestone in combination with other alternative cementitious materials to decrease the portland cement quantity in concrete and (ii) the use of geopolymers as the binder phase in concrete. The first phase of the work investigates the use of fine limestone as cement replacement from the perspective of hydration, strength development, and pore structure. The nature of the potential synergistic benefit of limestone and alumina will be explored. The second phase will focus on the rheological characterization of these materials in the fresh state, as well as a more general investigation of the rheological characterization of suspensions. The results of this work indicate several key ideas. (i) There is a potential synergistic benefit for strength, hydration, and pore structure by using alumina and in portland limestone cements, (ii) the limestone in these systems is shown to react to some extent, and fine limestone is shown to accelerate hydration, (iii) rheological characteristics of cementitious suspensions are complex, and strongly dependent on several key parameters including: the solid loading, interparticle forces, surface area of the particles present, particle size distribution of the particles, and rheological nature of the media in which the particles are suspended, and (iv) stress plateau method is proposed for the determination of rheological properties of concentrated suspensions, as it more accurately predicts apparent yield stress and is shown to correlate well with other viscoelastic properties of the suspensions.
ContributorsVance, Kirk (Author) / Neithalath, Narayanan (Thesis advisor) / Rajan, Subramaniam D. (Committee member) / Mobasher, Barzin (Committee member) / Chawla, Nikhilesh (Committee member) / Marzke, Robert (Committee member) / Arizona State University (Publisher)
Created2014
Description
The main objective of this study is to investigate the behaviour and applications of strain hardening cement composites (SHCC). Application of SHCC for use in slabs of common configurations was studied and design procedures are prepared by employing yield line theory and integrating it with simplified tri-linear model developed in Arizona State University by Dr. Barzin Mobasher and Dr. Chote Soranakom. Intrinsic material property of moment-curvature response for SHCC was used to derive the relationship between applied load and deflection in a two-step process involving the limit state analysis and kinematically admissible displacements. For application of SHCC in structures such as shear walls, tensile and shear properties are necessary for design. Lot of research has already been done to study the tensile properties and therefore shear property study was undertaken to prepare a design guide. Shear response of textile reinforced concrete was investigated based on picture frame shear test method. The effects of orientation, volume of cement paste per layer, planar cross-section and volume fraction of textiles were investigated. Pultrusion was used for the production of textile reinforced concrete. It is an automated set-up with low equipment cost which provides uniform production and smooth final surface of the TRC. A 3-D optical non-contacting deformation measurement technique of digital image correlation (DIC) was used to conduct the image analysis on the shear samples by means of tracking the displacement field through comparison between the reference image and deformed images. DIC successfully obtained full-field strain distribution, displacement and strain versus time responses, demonstrated the bonding mechanism from perspective of strain field, and gave a relation between shear angle and shear strain.
ContributorsAswani, Karan (Author) / Mobasher, Barzin (Thesis advisor) / Dharmarajan, Subramaniam (Committee member) / Neithalath, Narayanan (Committee member) / Arizona State University (Publisher)
Created2014
Description
For decades, microelectronics manufacturing has been concerned with failures related to electromigration phenomena in conductors experiencing high current densities. The influence of interconnect microstructure on device failures related to electromigration in BGA and flip chip solder interconnects has become a significant interest with reduced individual solder interconnect volumes. A survey indicates that x-ray computed micro-tomography (µXCT) is an emerging, novel means for characterizing the microstructures' role in governing electromigration failures. This work details the design and construction of a lab-scale µXCT system to characterize electromigration in the Sn-0.7Cu lead-free solder system by leveraging in situ imaging.
In order to enhance the attenuation contrast observed in multi-phase material systems, a modeling approach has been developed to predict settings for the controllable imaging parameters which yield relatively high detection rates over the range of x-ray energies for which maximum attenuation contrast is expected in the polychromatic x-ray imaging system. In order to develop this predictive tool, a model has been constructed for the Bremsstrahlung spectrum of an x-ray tube, and calculations for the detector's efficiency over the relevant range of x-ray energies have been made, and the product of emitted and detected spectra has been used to calculate the effective x-ray imaging spectrum. An approach has also been established for filtering `zinger' noise in x-ray radiographs, which has proven problematic at high x-ray energies used for solder imaging. The performance of this filter has been compared with a known existing method and the results indicate a significant increase in the accuracy of zinger filtered radiographs.
The obtained results indicate the conception of a powerful means for the study of failure causing processes in solder systems used as interconnects in microelectronic packaging devices. These results include the volumetric quantification of parameters which are indicative of both electromigration tolerance of solders and the dominant mechanisms for atomic migration in response to current stressing. This work is aimed to further the community's understanding of failure-causing electromigration processes in industrially relevant material systems for microelectronic interconnect applications and to advance the capability of available characterization techniques for their interrogation.
In order to enhance the attenuation contrast observed in multi-phase material systems, a modeling approach has been developed to predict settings for the controllable imaging parameters which yield relatively high detection rates over the range of x-ray energies for which maximum attenuation contrast is expected in the polychromatic x-ray imaging system. In order to develop this predictive tool, a model has been constructed for the Bremsstrahlung spectrum of an x-ray tube, and calculations for the detector's efficiency over the relevant range of x-ray energies have been made, and the product of emitted and detected spectra has been used to calculate the effective x-ray imaging spectrum. An approach has also been established for filtering `zinger' noise in x-ray radiographs, which has proven problematic at high x-ray energies used for solder imaging. The performance of this filter has been compared with a known existing method and the results indicate a significant increase in the accuracy of zinger filtered radiographs.
The obtained results indicate the conception of a powerful means for the study of failure causing processes in solder systems used as interconnects in microelectronic packaging devices. These results include the volumetric quantification of parameters which are indicative of both electromigration tolerance of solders and the dominant mechanisms for atomic migration in response to current stressing. This work is aimed to further the community's understanding of failure-causing electromigration processes in industrially relevant material systems for microelectronic interconnect applications and to advance the capability of available characterization techniques for their interrogation.
ContributorsMertens, James Charles Edwin (Author) / Chawla, Nikhilesh (Thesis advisor) / Alford, Terry (Committee member) / Jiao, Yang (Committee member) / Neithalath, Narayanan (Committee member) / Arizona State University (Publisher)
Created2015
Description
The studies on aluminosilicate materials to replace traditional construction materials such as ordinary Portland cement(OPC) to reduce the effects caused has been an important research area for the past decades. Many properties like strength have already been studied and the primary focus is to learn about the reaction mechanism and the effect of the parameters on the formed products. The aim of this research was to explore the structural changes and reaction product analysis of geopolymers (Slag & Fly Ash) using Fourier transform infrared spectroscopy (FTIR) and deconvolution
techniques. Spectroscopic techniques give valuable information at a molecular level but not all methods are economic and simple. To understand the mechanisms of alkali activated aluminosilicate materials, attenuated total reflectance (ATR) FTIR has been used where the effect of the parameters on the reaction products have been analyzed. To analyze complex systems like geopolymers using FTIR, deconvolution techniques help to obtain the properties of a particular peak attributed to a certain molecular vibration.
Time and temperature dependent analysis were done on slag pastes to understand the polymerization of reactive silica in the system with time and temperature variance. For time dependent analysis slag has been activated with sodium and potassium silicates using two different `n'values and three different silica modulus [Ms- (SiO2 /M2O)] values. The temperature dependent analysis was done by curing the samples at 60C and 80C. Similarly fly ash has been studied by activating with alkali hydroxides and alkali silicates. Under the same curing conditions the fly ash samples were evaluated to analyze the effects of added silicates for alkali activation.
The peak shifts in the FTIR explains the changes in the structural nature of the matrix and can be identified using the deconvolution technique. A strong correlation is found between the concentrations of silicate monomer in the activating position of the main Si-O-T (where T is Al/Si) stretching band in the FTIR spectrum, which
gives an indication of the relative changes in the Si/Al ratio. Also, the effect of the cation and silicate concentration in the activating solution has been discussed using the Fourier self deconvolution technique.
techniques. Spectroscopic techniques give valuable information at a molecular level but not all methods are economic and simple. To understand the mechanisms of alkali activated aluminosilicate materials, attenuated total reflectance (ATR) FTIR has been used where the effect of the parameters on the reaction products have been analyzed. To analyze complex systems like geopolymers using FTIR, deconvolution techniques help to obtain the properties of a particular peak attributed to a certain molecular vibration.
Time and temperature dependent analysis were done on slag pastes to understand the polymerization of reactive silica in the system with time and temperature variance. For time dependent analysis slag has been activated with sodium and potassium silicates using two different `n'values and three different silica modulus [Ms- (SiO2 /M2O)] values. The temperature dependent analysis was done by curing the samples at 60C and 80C. Similarly fly ash has been studied by activating with alkali hydroxides and alkali silicates. Under the same curing conditions the fly ash samples were evaluated to analyze the effects of added silicates for alkali activation.
The peak shifts in the FTIR explains the changes in the structural nature of the matrix and can be identified using the deconvolution technique. A strong correlation is found between the concentrations of silicate monomer in the activating position of the main Si-O-T (where T is Al/Si) stretching band in the FTIR spectrum, which
gives an indication of the relative changes in the Si/Al ratio. Also, the effect of the cation and silicate concentration in the activating solution has been discussed using the Fourier self deconvolution technique.
ContributorsMadavarapu, Sateesh Babu (Author) / Neithalath, Narayanan (Thesis advisor) / Rajan, Subramaniam D. (Committee member) / Marzke, Robert (Committee member) / Arizona State University (Publisher)
Created2014