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Description
Electromigration in metal interconnects is the most pernicious failure mechanism in semiconductor integrated circuits (ICs). Early electromigration investigations were primarily focused on aluminum interconnects for silicon-based ICs. An alternative metallization compatible with gallium arsenide (GaAs) was required in the development of high-powered radio frequency (RF) compound semiconductor devices operating at

Electromigration in metal interconnects is the most pernicious failure mechanism in semiconductor integrated circuits (ICs). Early electromigration investigations were primarily focused on aluminum interconnects for silicon-based ICs. An alternative metallization compatible with gallium arsenide (GaAs) was required in the development of high-powered radio frequency (RF) compound semiconductor devices operating at higher current densities and elevated temperatures. Gold-based metallization was implemented on GaAs devices because it uniquely forms a very low resistance ohmic contact and gold interconnects have superior electrical and thermal conductivity properties. Gold (Au) was also believed to have improved resistance to electromigration due to its higher melting temperature, yet electromigration reliability data on passivated Au interconnects is scarce and inadequate in the literature. Therefore, the objective of this research was to characterize the electromigration lifetimes of passivated Au interconnects under precisely controlled stress conditions with statistically relevant quantities to obtain accurate model parameters essential for extrapolation to normal operational conditions. This research objective was accomplished through measurement of electromigration lifetimes of large quantities of passivated electroplated Au interconnects utilizing high-resolution in-situ resistance monitoring equipment. Application of moderate accelerated stress conditions with a current density limited to 2 MA/cm2 and oven temperatures in the range of 300°C to 375°C avoided electrical overstress and severe Joule-heated temperature gradients. Temperature coefficients of resistance (TCRs) were measured to determine accurate Joule-heated Au interconnect film temperatures. A failure criterion of 50% resistance degradation was selected to prevent thermal runaway and catastrophic metal ruptures that are problematic of open circuit failure tests. Test structure design was optimized to reduce resistance variation and facilitate failure analysis. Characterization of the Au microstructure yielded a median grain size of 0.91 ìm. All Au lifetime distributions followed log-normal distributions and Black's model was found to be applicable. An activation energy of 0.80 ± 0.05 eV was measured from constant current electromigration tests at multiple temperatures. A current density exponent of 1.91 was extracted from multiple current densities at a constant temperature. Electromigration-induced void morphology along with these model parameters indicated grain boundary diffusion is dominant and the void nucleation mechanism controlled the failure time.
ContributorsKilgore, Stephen (Author) / Adams, James (Thesis advisor) / Schroder, Dieter (Thesis advisor) / Krause, Stephen (Committee member) / Gaw, Craig (Committee member) / Arizona State University (Publisher)
Created2013
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Description
Titanium oxide (TiO2), an abundant material with high photocatalytic activity and chemical stability is an important candidate for photocatalytic applications. The photocatalytic activity of the TiO2 varies with its phase. In the current project, phase and morphology changes in TiO2 nanotubes were studied using ex-situ and in-situ transmission electron microscopy

Titanium oxide (TiO2), an abundant material with high photocatalytic activity and chemical stability is an important candidate for photocatalytic applications. The photocatalytic activity of the TiO2 varies with its phase. In the current project, phase and morphology changes in TiO2 nanotubes were studied using ex-situ and in-situ transmission electron microscopy (TEM). X-ray diffraction and scanning electron microscopy studies were also performed to understand the phase and morphology of the nanotubes. As prepared TiO2 nanotubes supported on Ti metal substrate were amorphous, during the heat treatment in the ex-situ furnace nanotubes transform to anatase at 450 oC and transformed to rutile when heated to 800 oC. TiO2 nanotubes that were heat treated in an in-situ environmental TEM, transformed to anatase at 400 oC and remain anatase even up to 800 oC. In both ex-situ an in-situ case, the morphology of the nanotubes drastically changed from a continuous tubular structure to aggregates of individual nanoparticles. The difference between the ex-situ an in-situ treatments and their effect on the phase transformation is discussed. Metal doping is one of the effective ways to improve the photocatalytic performance. Several approaches were performed to get metal loading on to the TiO2 nanotubes. Mono-dispersed platinum nanoparticles were deposited on the TiO2 nanopowder and nanotubes using photoreduction method. Photo reduction for Ag and Pt bimetallic nanoparticles were also performed on the TiO2 powders.
ContributorsSantra, Sanjitarani (Author) / Crozier, Peter A. (Thesis advisor) / Carpenter, Ray (Committee member) / Buttry, Daniel (Committee member) / Arizona State University (Publisher)
Created2014
Description
The future grid will face challenges to meet an increased power demand by the consumers. Various solutions were studied to address this issue. One alternative to realize increased power flow in the grid is to use High Temperature Low Sag (HTLS) since it fulfills essential criteria of less sag and

The future grid will face challenges to meet an increased power demand by the consumers. Various solutions were studied to address this issue. One alternative to realize increased power flow in the grid is to use High Temperature Low Sag (HTLS) since it fulfills essential criteria of less sag and good material performance with temperature. HTLS conductors like Aluminum Conductor Composite Reinforced (ACCR) and Aluminum Conductor Carbon Composite (ACCC) are expected to face high operating temperatures of 150-200 degree Celsius in order to achieve the desired increased power flow. Therefore, it is imperative to characterize the material performance of these conductors with temperature. The work presented in this thesis addresses the characterization of carbon composite core based and metal matrix core based HTLS conductors. The thesis focuses on the study of variation of tensile strength of the carbon composite core with temperature and the level of temperature rise of the HTLS conductors due to fault currents cleared by backup protection. In this thesis, Dynamic Mechanical Analysis (DMA) was used to quantify the loss in storage modulus of carbon composite cores with temperature. It has been previously shown in literature that storage modulus is correlated to the tensile strength of the composite. Current temperature relationships of HTLS conductors were determined using the IEEE 738-2006 standard. Temperature rise of these conductors due to fault currents were also simulated. All simulations were performed using Microsoft Visual C++ suite. Tensile testing of metal matrix core was also performed. Results of DMA on carbon composite cores show that the storage modulus, hence tensile strength, decreases rapidly in the temperature range of intended use. DMA on composite cores subjected to heat treatment were conducted to investigate any changes in the variation of storage modulus curves. The experiments also indicates that carbon composites cores subjected to temperatures at or above 250 degree Celsius can cause permanent loss of mechanical properties including tensile strength. The fault current temperature analysis of carbon composite based conductors reveal that fault currents eventually cleared by backup protection in the event of primary protection failure can cause damage to fiber matrix interface.
ContributorsBanerjee, Koustubh (Author) / Gorur, Ravi (Committee member) / Karady, George G. (Committee member) / Ayyanar, Raja (Committee member) / Arizona State University (Publisher)
Created2014
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Description
Aluminum alloys and their composites are attractive materials for applications requiring high strength-to-weight ratios and reasonable cost. Many of these applications, such as those in the aerospace industry, undergo fatigue loading. An understanding of the microstructural damage that occurs in these materials is critical in assessing their fatigue resistance. Two

Aluminum alloys and their composites are attractive materials for applications requiring high strength-to-weight ratios and reasonable cost. Many of these applications, such as those in the aerospace industry, undergo fatigue loading. An understanding of the microstructural damage that occurs in these materials is critical in assessing their fatigue resistance. Two distinct experimental studies were performed to further the understanding of fatigue damage mechanisms in aluminum alloys and their composites, specifically fracture and plasticity. Fatigue resistance of metal matrix composites (MMCs) depends on many aspects of composite microstructure. Fatigue crack growth behavior is particularly dependent on the reinforcement characteristics and matrix microstructure. The goal of this work was to obtain a fundamental understanding of fatigue crack growth behavior in SiC particle-reinforced 2080 Al alloy composites. In situ X-ray synchrotron tomography was performed on two samples at low (R=0.1) and at high (R=0.6) R-ratios. The resulting reconstructed images were used to obtain three-dimensional (3D) rendering of the particles and fatigue crack. Behaviors of the particles and crack, as well as their interaction, were analyzed and quantified. Four-dimensional (4D) visual representations were constructed to aid in the overall understanding of damage evolution. During fatigue crack growth in ductile materials, a plastic zone is created in the region surrounding the crack tip. Knowledge of the plastic zone is important for the understanding of fatigue crack formation as well as subsequent growth behavior. The goal of this work was to quantify the 3D size and shape of the plastic zone in 7075 Al alloys. X-ray synchrotron tomography and Laue microdiffraction were used to non-destructively characterize the volume surrounding a fatigue crack tip. The precise 3D crack profile was segmented from the reconstructed tomography data. Depth-resolved Laue patterns were obtained using differential-aperture X-ray structural microscopy (DAXM), from which peak-broadening characteristics were quantified. Plasticity, as determined by the broadening of diffracted peaks, was mapped in 3D. Two-dimensional (2D) maps of plasticity were directly compared to the corresponding tomography slices. A 3D representation of the plastic zone surrounding the fatigue crack was generated by superimposing the mapped plasticity on the 3D crack profile.
ContributorsHruby, Peter (Author) / Chawla, Nikhilesh (Thesis advisor) / Solanki, Kiran (Committee member) / Liu, Yongming (Committee member) / Arizona State University (Publisher)
Created2014
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Description
Thiol functionalization is one potentially useful way to tailor physical and chemical properties of graphene oxides (GOs) and reduced graphene oxides (RGOs). Despite the ubiquitous presence of thiol functional groups in diverse chemical systems, efficient thiol functionalization has been challenging for GOs and RGOs, or for carbonaceous materials in general.

Thiol functionalization is one potentially useful way to tailor physical and chemical properties of graphene oxides (GOs) and reduced graphene oxides (RGOs). Despite the ubiquitous presence of thiol functional groups in diverse chemical systems, efficient thiol functionalization has been challenging for GOs and RGOs, or for carbonaceous materials in general. In this work, thionation of GOs has been achieved in high yield through two new methods that also allow concomitant chemical reduction/thermal reduction of GOs; a solid-gas metathetical reaction method with boron sulfides (BxSy) gases and a solvothermal reaction method employing phosphorus decasulfide (P4S10). The thionation products, called "mercapto reduced graphene oxides (m-RGOs)", were characterized by employing X-ray photoelectron spectroscopy, powder X-ray diffraction, UV-Vis spectroscopy, FT-IR spectroscopy, Raman spectroscopy, electron probe analysis, scanning electron microscopy, (scanning) transmission electron microscopy, nano secondary ion mass spectrometry, Ellman assay and atomic force microscopy. The excellent dispersibility of m-RGOs in various solvents including alcohols has allowed fabrication of thin films of m-RGOs. Deposition of m-RGOs on gold substrates was achieved through solution deposition and the m-RGOs were homogeneously distributed on gold surface shown by atomic force microscopy. Langmuir-Blodgett (LB) films of m-RGOs were obtained by transferring their Langmuir films, formed by simple drop casting of m-RGOs dispersion on water surface, onto various substrates including gold, glass and indium tin oxide. The m-RGO LB films showed low sheet resistances down to about 500 kΩ/sq at 92% optical transparency. The successful results make m-RGOs promising for applications in transparent conductive coatings, biosensing, etc.
ContributorsJeon, Kiwan (Author) / Seo, Dong-Kyun (Thesis advisor) / Jones, Anne K (Committee member) / Yarger, Jeffery (Committee member) / Arizona State University (Publisher)
Created2013
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Description
In this dissertation, combined photo-induced and thermionic electron emission from low work function diamond films is studied through low energy electron spectroscopy analysis and other associated techniques. Nitrogen-doped, hydrogen-terminated diamond films prepared by the microwave plasma chemical vapor deposition method have been the most focused material. The theme of this

In this dissertation, combined photo-induced and thermionic electron emission from low work function diamond films is studied through low energy electron spectroscopy analysis and other associated techniques. Nitrogen-doped, hydrogen-terminated diamond films prepared by the microwave plasma chemical vapor deposition method have been the most focused material. The theme of this research is represented by four interrelated issues. (1) An in-depth study describes combined photo-induced and thermionic emission from nitrogen-doped diamond films on molybdenum substrates, which were illuminated with visible light photons, and the electron emission spectra were recorded as a function of temperature. The diamond films displayed significant emissivity with a low work function of ~ 1.5 eV. The results indicate that these diamond emitters can be applied in combined solar and thermal energy conversion. (2) The nitrogen-doped diamond was further investigated to understand the physical mechanism and material-related properties that enable the combined electron emission. Through analysis of the spectroscopy, optical absorbance and photoelectron microscopy results from sample sets prepared with different configurations, it was deduced that the photo-induced electron generation involves both the ultra-nanocrystalline diamond and the interface between the diamond film and metal substrate. (3) Based on results from the first two studies, possible photon-enhanced thermionic emission was examined from nitrogen-doped diamond films deposited on silicon substrates, which could provide the basis for a novel approach for concentrated solar energy conversion. A significant increase of emission intensity was observed at elevated temperatures, which was analyzed using computer-based modeling and a combination of different emission mechanisms. (4) In addition, the electronic structure of vanadium-oxide-terminated diamond surfaces was studied through in-situ photoemission spectroscopy. Thin layers of vanadium were deposited on oxygen-terminated diamond surfaces which led to oxide formation. After thermal annealing, a negative electron affinity was found on boron-doped diamond, while a positive electron affinity was found on nitrogen-doped diamond. A model based on the barrier at the diamond-oxide interface was employed to analyze the results. Based on results of this dissertation, applications of diamond-based energy conversion devices for combined solar- and thermal energy conversion are proposed.
ContributorsSun, Tianyin (Author) / Nemanich, Robert (Thesis advisor) / Ponce, Fernando (Committee member) / Peng, Xihong (Committee member) / Spence, John (Committee member) / Treacy, Michael (Committee member) / Arizona State University (Publisher)
Created2013
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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

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
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Description
ABSTRACT Electronics especially mobile electronics such as smart phones, tablet PCs, notebooks and digital cameras are undergoing rapid development nowadays and have thoroughly changed our lives. With the requirement of more transistors, higher power, smaller size, lighter weight and even bendability, thermal management of these devices became one of the

ABSTRACT Electronics especially mobile electronics such as smart phones, tablet PCs, notebooks and digital cameras are undergoing rapid development nowadays and have thoroughly changed our lives. With the requirement of more transistors, higher power, smaller size, lighter weight and even bendability, thermal management of these devices became one of the key challenges. Compared to active heat management system, heat pipe, which is a passive fluidic system, is considered promising to solve this problem. However, traditional heat pipes have size, weight and capillary limitation. Thus new type of heat pipe with smaller size, lighter weight and higher capillary pressure is needed. Nanofiber has been proved with superior properties and has been applied in multiple areas. This study discussed the possibility of applying nanofiber in heat pipe as new wick structure. In this study, a needleless electrospinning device with high productivity rate was built onsite to systematically investigate the effect of processing parameters on fiber properties as well as to generate nanofiber mat to evaluate its capability in electronics cooling. Polyethylene oxide (PEO) and Polyvinyl Alcohol (PVA) nanofibers were generated. Tensiometer was used for wettability measurement. The results show that independent parameters including spinneret type, working distance, solution concentration and polymer type are strongly correlated with fiber morphology compared to other parameters. The results also show that the fabricated nanofiber mat has high capillary pressure.
ContributorsSun, Tianwei (Author) / Jiang, Hanqing (Thesis advisor) / Yu, Hongyu (Committee member) / Chen, Kangping (Committee member) / Arizona State University (Publisher)
Created2014
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Description
Novel materials for Li-ion batteries is one of the principle thrust areas for current research in energy storage, more so than most, considering its widespread use in portable electronic gadgets and plug-in electric and hybrid cars. One of the major limiting factors in a Li-ion battery's energy density is the

Novel materials for Li-ion batteries is one of the principle thrust areas for current research in energy storage, more so than most, considering its widespread use in portable electronic gadgets and plug-in electric and hybrid cars. One of the major limiting factors in a Li-ion battery's energy density is the low specific capacities of the active materials in the electrodes. In the search for high-performance anode materials for Li-ion batteries, many alternatives to carbonaceous materials have been studied. Both cubic and amorphous silicon can reversibly alloy with lithium and have a theoretical capacity of 3500 mAh/g, making silicon a potential high density anode material. However, a large volume expansion of 300% occurs due to changes in the structure during lithium insertion, often leading to pulverization of the silicon. To this end, a class of silicon based cage compounds called clathrates are studied for electrochemical reactivity with lithium. Silicon-clathrates consist of silicon covalently bonded in cage structures comprised of face sharing Si20, Si24 and/or Si28 clusters with guest ions occupying the interstitial positions in the polyhedra. Prior to this, silicon clathrates have been studied primarily for their superconducting and thermoelectric properties. In this work, the synthesis and electrochemical characterization of two categories of silicon clathrates - Type-I silicon clathrate with aluminum framework substitution and barium guest ions (Ba8AlxSi46-x) and Type-II silicon clathrate with sodium guest ions (Nax Si136), are explored. The Type-I clathrate, Ba8AlxSi46-x consists of an open framework of aluminium and silicon, with barium (guest) atoms occupying the interstitial positions. X-ray diffraction studies have shown that a crystalline phase of clathrate is obtained from synthesis, which is powdered to a fine particle size to be used as the anode material in a Li-ion battery. Electrochemical measurements of these type of clathrates have shown that capacities comparable to graphite can be obtained for up to 10 cycles and lower capacities can be obtained for up to 20 cycles. Unlike bulk silicon, the clathrate structure does not undergo excessive volume change upon lithium intercalation, and therefore, the crystal structure is morphologically stable over many cycles. X-ray diffraction of the clathrate after cycling showed that crystallinity is intact, indicating that the clathrate does not collapse during reversible intercalation with lithium ions. Electrochemical potential spectroscopy obtained from the cycling data showed that there is an absence of formation of lithium-silicide, which is the product of lithium alloying with diamond cubic silicon. Type II silicon clathrate, NaxSi136, consists of silicon making up the framework structure and sodium (guest) atoms occupying the interstitial spaces. These clathrates showed very high capacities during their first intercalation cycle, in the range of 3,500 mAh/g, but then deteriorated during subsequent cycles. X-ray diffraction after one cycle showed the absence of clathrate phase and the presence of lithium-silicide, indicating the disintegration of clathrate structure. This could explain the silicon-like cycling behavior of Type II clathrates.
ContributorsRaghavan, Rahul (Author) / Chan, Candace K. (Thesis advisor) / Crozier, Peter (Committee member) / Petuskey, William T (Committee member) / Arizona State University (Publisher)
Created2013
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Description
This thesis describes the fabrication of several new classes of Ge1-x-ySixSny materials with the required compositions and crystal quality to engineer the band gaps above and below that of elemental Ge (0.8 eV) in the near IR. The work initially focused on Ge1-x-ySixSny (1-5% Sn, 4-20% Si) materials grown on

This thesis describes the fabrication of several new classes of Ge1-x-ySixSny materials with the required compositions and crystal quality to engineer the band gaps above and below that of elemental Ge (0.8 eV) in the near IR. The work initially focused on Ge1-x-ySixSny (1-5% Sn, 4-20% Si) materials grown on Ge(100) via gas-source epitaxy of Ge4H10, Si4H10 and SnD4. Both intrinsic and doped layers were produced with defect-free microstructure and viable thickness, allowing the fabrication of high-performance photodetectors. These exhibited low ideality factors, state-of-the-art dark current densities and adjustable absorption edges between 0.87 and 1.03 eV, indicating that the band gaps span a significant range above that of Ge. Next Sn-rich Ge1-x-ySixSny alloys (2-4% Si and 4-10% Sn) were fabricated directly on Si and were found to show significant optical emission using photoluminescence measurements, indicating that the alloys have direct band gaps below that of pure Ge in the range of 0.7-0.55 eV. A series of Sn-rich Ge1-x-ySixSny analogues (y>x) with fixed 3-4% Si content and progressively increasing Sn content in the 4-10% range were then grown on Ge buffered Si platforms for the purpose of improving the material's crystal quality. The films in this case exhibited lower defect densities than those grown on Si, allowing a meaningful study of both the direct and indirect gaps. The results show that the separation of the direct and indirect edges can be made smaller than in Ge even for non-negligible 3-4% Si content, confirming that with a suitable choice of Sn compositions the ternary Ge1-x-ySixSny reproduces all features of the electronic structure of binary Ge1-ySny, including the sought-after indirect-to-direct gap cross over. The above synthesis of optical quality Ge1-x-ySixSny on virtual Ge was made possible by the development of high quality Ge-on-Si buffers via chemical vapor deposition of Ge4H10. The resultant films exhibited structural and electrical properties significantly improved relative to state-of-the-art results obtained using conventional approaches. It was found that pure Ge4H10 facilitates the control of residual doping and enables p-i-n devices whose dark currents are not entirely determined by defects and whose zero-bias collection efficiencies are higher than those obtained from samples fabricated using alternative Ge-on-Si approaches.
ContributorsXu, Chi (Author) / Kouvetakis, John (Thesis advisor) / Menéndez, Jose (Thesis advisor) / Chizmeshya, Andrew (Committee member) / Drucker, Jeffrey (Committee member) / Ponce, Fernando (Committee member) / Arizona State University (Publisher)
Created2013