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Electron Microscopy Study of the Phase Transformation and Metal Functionalization of Titanium Oxide Nanotubes

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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

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.

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2014

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Understanding plasticity and fracture in aluminum alloys and their composites by 3D X-ray synchrotron tomography and microdiffraction

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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

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.

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2014

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Chip level implementation techniques for radiation hardened microprocessors

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Microprocessors are the processing heart of any digital system and are central to all the technological advancements of the age including space exploration and monitoring. The demands of space exploration require a special class of microprocessors called radiation hardened microprocessors

Microprocessors are the processing heart of any digital system and are central to all the technological advancements of the age including space exploration and monitoring. The demands of space exploration require a special class of microprocessors called radiation hardened microprocessors which are less susceptible to radiation present outside the earth's atmosphere, in other words their functioning is not disrupted even in presence of disruptive radiation. The presence of these particles forces the designers to come up with design techniques at circuit and chip levels to alleviate the errors which can be encountered in the functioning of microprocessors. Microprocessor evolution has been very rapid in terms of performance but the same cannot be said about its rad-hard counterpart. With the total data processing capability overall increasing rapidly, the clear lack of performance of the processors manifests as a bottleneck in any processing system. To design high performance rad-hard microprocessors designers have to overcome difficult design problems at various design stages i.e. Architecture, Synthesis, Floorplanning, Optimization, routing and analysis all the while maintaining circuit radiation hardness. The reference design `HERMES' is targeted at 90nm IBM G process and is expected to reach 500Mhz which is twice as fast any processor currently available. Chapter 1 talks about the mechanisms of radiation effects which cause upsets and degradation to the functioning of digital circuits. Chapter 2 gives a brief description of the components which are used in the design and are part of the consistent efforts at ASUVLSI lab culminating in this chip level implementation of the design. Chapter 3 explains the basic digital design ASIC flow and the changes made to it leading to a rad-hard specific ASIC flow used in implementing this chip. Chapter 4 talks about the triple mode redundant (TMR) specific flow which is used in the block implementation, delineating the challenges faced and the solutions proposed to make the flow work. Chapter 5 explains the challenges faced and solutions arrived at while using the top-level flow described in chapter 3. Chapter 6 puts together the results and analyzes the design in terms of basic integrated circuit design constraints.

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2013

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Synthesis and electrochemical characterization of silicon clathrates as anode materials for lithium ion batteries

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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

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.

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2013

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Model-based design, simulation and automatic code generation for embedded systems and robotic applications

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As the complexity of robotic systems and applications grows rapidly, development of high-performance, easy to use, and fully integrated development environments for those systems is inevitable. Model-Based Design (MBD) of dynamic systems using engineering software such as Simulink® from MathWorks®,

As the complexity of robotic systems and applications grows rapidly, development of high-performance, easy to use, and fully integrated development environments for those systems is inevitable. Model-Based Design (MBD) of dynamic systems using engineering software such as Simulink® from MathWorks®, SciCos from Metalau team and SystemModeler® from Wolfram® is quite popular nowadays. They provide tools for modeling, simulation, verification and in some cases automatic code generation for desktop applications, embedded systems and robots. For real-world implementation of models on the actual hardware, those models should be converted into compilable machine code either manually or automatically. Due to the complexity of robotic systems, manual code translation from model to code is not a feasible optimal solution so we need to move towards automated code generation for such systems. MathWorks® offers code generation facilities called Coder® products for this purpose. However in order to fully exploit the power of model-based design and code generation tools for robotic applications, we need to enhance those software systems by adding and modifying toolboxes, files and other artifacts as well as developing guidelines and procedures. In this thesis, an effort has been made to propose a guideline as well as a Simulink® library, StateFlow® interface API and a C/C++ interface API to complete this toolchain for NAO humanoid robots. Thus the model of the hierarchical control architecture can be easily and properly converted to code and built for implementation.

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2013

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Electronic excitations in topological insulators studied by Electron Energy Loss Spectroscopy

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Topological insulators with conducting surface states yet insulating bulk states have generated a lot of interest amongst the physics community due to their varied characteristics and possible applications. Doped topological insulators have presented newer physical states of matter where topological

Topological insulators with conducting surface states yet insulating bulk states have generated a lot of interest amongst the physics community due to their varied characteristics and possible applications. Doped topological insulators have presented newer physical states of matter where topological order co&ndashexists; with other physical properties (like magnetic order). The electronic states of these materials are very intriguing and pose problems and the possible solutions to understanding their unique behaviors. In this work, we use Electron Energy Loss Spectroscopy (EELS) – an analytical TEM tool to study both core&ndashlevel; and valence&ndashlevel; excitations in Bi2Se3 and Cu(doped)Bi2Se3 topological insulators. We use this technique to retrieve information on the valence, bonding nature, co-ordination and lattice site occupancy of the undoped and the doped systems. Using the reference materials Cu(I)Se and Cu(II)Se we try to compare and understand the nature of doping that copper assumes in the lattice. And lastly we utilize the state of the art monochromated Nion UltraSTEM 100 to study electronic/vibrational excitations at a record energy resolution from sub-nm regions in the sample.

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2013

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Alkali activated systems: understanding the influence of curing conditions and activator type/chemistry on the mechanical strength and chemical structure of fly ash/slag systems

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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

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.

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2013

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Effect of helium ion irradiation on the tunneling behavior in niobium/aluminum/aluminum oxide/niobium Josephson junctions

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The study of high energy particle irradiation effect on Josephson junction tri-layers is relevant to applications in space and radioactive environments. It also allows us to investigate the influence of defects and interfacial intermixing on the junction electrical characteristics. In

The study of high energy particle irradiation effect on Josephson junction tri-layers is relevant to applications in space and radioactive environments. It also allows us to investigate the influence of defects and interfacial intermixing on the junction electrical characteristics. In this work, we studied the influence of 2MeV Helium ion irradiation with doses up to 5.2×1016 ions/cm2 on the tunneling behavior of Nb/Al/AlOx/Nb Josephson junctions. Structural and analytical TEM characterization, combined with SRIM modeling, indicates that over 4nm of intermixing occurred at the interfaces. EDX analysis after irradiation, suggests that the Al and O compositions from the barrier are collectively distributed together over a few nanometers. Surprisingly, the IV characteristics were largely unchanged. The normal resistance, Rn, increased slightly (<20%) after the initial dose of 3.5×1015 ions/cm2 and remained constant after that. This suggests that tunnel barrier electrical properties were not affected much, despite the significant changes in the chemical distribution of the barrier's Al and O shown in SRIM modeling and TEM pictures. The onset of quasi-particle current, sum of energy gaps (2Δ), dropped systematically from 2.8meV to 2.6meV with increasing dosage. Similarly, the temperature onset of the Josephson current dropped from 9.2K to 9.0K. This suggests that the order parameter at the barrier interface has decreased as a result of a reduced mean free path in the Al proximity layer and a reduction in the transition temperature of the Nb electrode near the barrier. The dependence of Josephson current on the magnetic field and temperature does not change significantly with irradiation, suggesting that intermixing into the Nb electrode is significantly less than the penetration depth.

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2012

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Optical properties and electrochemical dealloying of gold-silver alloy nanoparticles immobilized on composite thin-tilm electrodes

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Gold-silver alloy nanoparticles (NPs) capped with adenosine 5'-triphosphate were synthesized by borohydride reduction of dilute aqueous metal precursors. High-resolution transmission electron microscopy showed the as-synthesized particles to be spherical with average diameters ~4 nm. Optical properties were measured by UV-Visible

Gold-silver alloy nanoparticles (NPs) capped with adenosine 5'-triphosphate were synthesized by borohydride reduction of dilute aqueous metal precursors. High-resolution transmission electron microscopy showed the as-synthesized particles to be spherical with average diameters ~4 nm. Optical properties were measured by UV-Visible spectroscopy (UV-Vis), and the formation of alloy NPs was verified across all gold:silver ratios by a linear shift in the plasmon band maxima against alloy composition. The molar absorptivities of the NPs decreased non-linearly with increasing gold content from 2.0 x 108 M-1 cm-1 (fÉmax = 404 nm) for pure silver to 4.1 x 107 M-1 cm-1 (fÉmax = 511 nm) for pure gold. The NPs were immobilized onto transparent indium-tin oxide composite electrodes using layer-by-layer (LbL) deposition with poly(diallyldimethylammonium) acting as a cationic binder. The UV-Vis absorbance of the LbL film was used to calculate the surface coverage of alloy NPs on the electrode. Typical preparations had average NP surface coverages of 2.8 x 10-13 mol NPs/cm2 (~5% of cubic closest packing) with saturated films reaching ~20% of ccp for single-layer preparations (1.0 ~ 10-12 mol NPs/cm2). X-ray photoelectron spectroscopy confirmed the presence of alloy NPs in the LbL film and showed silver enrichment of the NP surfaces by ~9%. Irreversible oxidative dissolution (dealloying) of the less noble silver atoms from the NPs on LbL electrodes was performed by cyclic voltammetry (CV) in sulfuric acid. Alloy NPs with higher gold content required larger overpotentials for silver dealloying. Dealloying of the more-noble gold atoms from the alloy NPs was also achieved by CV in sodium chloride. The silver was oxidized first to cohesive silver chloride, and then gold dealloyed to soluble HAuCl4- at higher potentials. Silver oxidation was inhibited during the first oxidative scan, but subsequent cycles showed typical, reversible silver-to-silver chloride voltammetry. The potentials for both silver oxidation and gold dealloying also shifted to more oxidizing potentials with increasing gold content, and both processes converged for alloy NPs with >60% gold content. Charge-mediated electrochemistry of silver NPs immobilized in LbL films, using Fc(meOH) as the charge carrier, showed that 67% of the NPs were electrochemically inactive.

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2014

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Estimation of complex permittivity of silicon at 2.45 GHz microwave frequency

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Estimation of complex permittivity of arsenic-doped silicon is the primary topic of discussion in this thesis presentation. The frequency that is of interest is 2.45 GHz, frequency typically used in conventional microwave ovens. The analysis is based on closed-form analytical

Estimation of complex permittivity of arsenic-doped silicon is the primary topic of discussion in this thesis presentation. The frequency that is of interest is 2.45 GHz, frequency typically used in conventional microwave ovens. The analysis is based on closed-form analytical expressions of cylindrical symmetry. A coaxial/radial line junction with the central conductor sheathed in dielectric material, which is As-doped silicon in this case, are analyzed. Electrical and magnetic field equations governing the wave propagation in this setup are formulated by applying the necessary boundary conditions. Input admittance is computed using the fields in the device and reflection coefficient is calculated at the input. This analytical solution is matched to the reflection coefficient acquired by experiments conducted, using VNA as the input source. The contemplation is backed by simulation using High Frequency Structural Simulator, HFSS. Susceptor-assisted microwave heating has been shown to be a faster and easier method of annealing arsenic-doped silicon samples. In that study, it was noticed that the microwave power absorbed by the sample can directly be linked to the heat power required for the annealing process. It probes the validity of the statement that for arsenic-doped silicon the heating curve depends only on its sheet properties and not on the bulk as such and the results presented here gives more insight to it as to why this assumption is true. The results obtained here can be accepted as accurate since it is known that this material is highly conductive and electromagnetic waves do not penetrate in to the material beyond a certain depth, which is given by the skin depth of the material. Hall measurements and four-point-probe measurements are performed on the material in support of the above contemplation.

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2014