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- Title
- MICROSTRUCTURAL AND MECHANICAL CHARACTERIZATION OF AL-AL2O3 NANOCOMPOSITES SYNTHESIZED BY HIGH-ENERGY MILLING.
- Creator
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Prabhu, Balaji, Challapalli, Suryanarayana, University of Central Florida
- Abstract / Description
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The twin objectives of the investigation were (i) to synthesize Al/Al2O3 metal matrix composites (MMCs) with uniform distribution of the Al2O3 reinforcement in the Al matrix and (ii) to evaluate the effect of volume fraction and size of the reinforcement on the mechanical behavior of MMCs. This was achieved by successful synthesis of Al-Al2O3 MMCs with volume fractions of 5, 10, 20, 30, and 50%, and particle sizes of 50 nm, 150 nm, and 5 µm of Al2O3 synthesized from blended component...
Show moreThe twin objectives of the investigation were (i) to synthesize Al/Al2O3 metal matrix composites (MMCs) with uniform distribution of the Al2O3 reinforcement in the Al matrix and (ii) to evaluate the effect of volume fraction and size of the reinforcement on the mechanical behavior of MMCs. This was achieved by successful synthesis of Al-Al2O3 MMCs with volume fractions of 5, 10, 20, 30, and 50%, and particle sizes of 50 nm, 150 nm, and 5 µm of Al2O3 synthesized from blended component powders by a high-energy milling technique. A uniform distribution of the Al2O3 reinforcement in the Al matrix was successfully obtained after milling the powders for a period of 20 h with a ball-to-powder weight ratio of 10:1 in a SPEX mill. The uniform distribution of Al2O3 in the Al matrix was confirmed by characterizing these nanocomposite powders by scanning electron microscopy and X-ray mapping. The energy dispersive spectroscopy and X-ray diffraction techniques were employed to determine the composition and phase analysis, respectively. The milled powders were then consolidated for subsequent mechanical characterization by (i) magnetic pulse compaction (MPC) (ii) hot-isostatic pressing (HIP), (iii) vaccum hot pressing (VHP), and (iv) a combination of vaccum hot pressing and hot-isostatic pressing (VHP+HIP). However, successful consolidation of the powders to near-full density was achieved only through VHP+HIP for the 5 and 10 vol. % Al2O3 samples with 50 nm and 150 nm particle sizes. The fully dense samples were then subjected to mechanical characterization by compression testing and nanoindentation techniques. The strength and elastic modulus values obtained from compression testing showed an increase with increasing volume fraction and decreasing particle size of the reinforcement. The nanoindentation results were, however, contradictory, and the presence of residual stresses in the samples was attributed as the cause for the deviation in values.
Show less - Date Issued
- 2005
- Identifier
- CFE0000727, ucf:46602
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0000727
- Title
- STRUCTURAL CHARACTERIZATION OF SPUTTER-DEPOSITED SS304+XAL (X = 0, 4, 7 AND 10 WT.%) COATINGS AND MECHANICALLY MILLED TI, ZR AND HF POWDERS.
- Creator
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Seelam, Uma Maheswara, Suryanarayana, Challapalli, University of Central Florida
- Abstract / Description
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Study of the metastable phases obtained by non-equilibrium processing techniques has come a long way during the past five decades. New metastable phases have often given new perspectives to the research on synthesis of novel materials systems. Metastable materials produced by two non-equilibrium processing methods were studied for this dissertation- 304-type austenitic stainless steel (SS304 or Fe-18Cr-8Ni)+aluminum coatings produced by plasma enhanced magnetron sputter-deposition (PEMS) and...
Show moreStudy of the metastable phases obtained by non-equilibrium processing techniques has come a long way during the past five decades. New metastable phases have often given new perspectives to the research on synthesis of novel materials systems. Metastable materials produced by two non-equilibrium processing methods were studied for this dissertation- 304-type austenitic stainless steel (SS304 or Fe-18Cr-8Ni)+aluminum coatings produced by plasma enhanced magnetron sputter-deposition (PEMS) and nanocrystalline Ti, Zr and Hf powders processed by mechanical milling (MM). The objective of the study was to understand the crystallographic and microstructural aspects of these materials. Four SS304+Al coatings with a nominal Al percentages of 0, 4, 7 and 10 wt.% in the coatings were deposited on an SS304 substrate by PEMS using SS304 and Al targets. The as-deposited coatings were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and three-dimensional atom probe microscopy (3DAP). Surface morphology and chemical analysis were studied by SEM. Phase identification was carried out by XRD and TEM. The microstructural features of all the coatings, as observed in the TEM, consisted of columnar grains with the columnar grain width (a measure of grain size) increasing with an increase in the Al content. The coatings had grains with average grain sizes of about 100, 290, 320 and 980 nm, respectively for 0, 4, 7 and 10 wt.% Al. The observed grain structures and increase in grain size were related to substrate temperature during deposition. XRD results indicated that the Al-free coating consisted of the non-equilibrium ferrite and sigma phases. In the 4Al, 7Al and 10Al coatings, equilibrium ferrite and B2 phases were observed but no sigma phase was found. In 10Al coating, we were able to demonstrate experimentally using 3DAP studies that NiAl phase formation is preferred over the FeAl phase at nano scale. During mechanical milling of the hexagonal close packed (HCP) metals Hf, Ti and Zr powders, unknown nanocrystalline phases with face centered cubic (FCC) structure were found. The FCC phases could be either allotropes of the respective metals or impurity stabilized phases. However, upon MM under high purity conditions, it was revealed that the FCC phases were impurity stabilized. The decrease in crystallite size down to nanometer levels, an increase in atomic volume, lattice strain, and possible contamination were the factors responsible for the transformation.
Show less - Date Issued
- 2010
- Identifier
- CFE0003161, ucf:48595
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0003161
- Title
- Printable Carbon Nanotube Based Multifunctional Nanocomposites for Strain Sensing and Self-heating.
- Creator
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Wang, Xin, Gou, Jihua, Challapalli, Suryanarayana, Xu, Yunjun, University of Central Florida
- Abstract / Description
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The unique properties of carbon nanotubes (CNTs) represent a potential for developing a piezo-resistive strain sensor and a resistive heating sheet with a smart structure. Conventional fabrication techniques of CNT based nanocomposites such as molding, casting or spray coating lack the ability to control the geometry and properties of fabricated composites. In order to meet the various requirements of strain sensing or self-heating applications, nanocomposites with complex geometry and...
Show moreThe unique properties of carbon nanotubes (CNTs) represent a potential for developing a piezo-resistive strain sensor and a resistive heating sheet with a smart structure. Conventional fabrication techniques of CNT based nanocomposites such as molding, casting or spray coating lack the ability to control the geometry and properties of fabricated composites. In order to meet the various requirements of strain sensing or self-heating applications, nanocomposites with complex geometry and controllable properties are in high demand. Digital printing technique is able to fabricate CNT films with precisely controlled geometry with the help of computer aided design, and their properties could also be controlled by adjusting the printing parameters. The objective of this study is to investigate the printing-structure-property relationship of CNT based multifunctional nanocomposites fabricated by digitally controlled spray deposition process for strain sensing and self-heating. A spray deposition modeling (SDM) printer that uses a 12-array inkjet nozzle attached to an x-y plotter was developed for the fabrication of CNT layers. Most of previously-reported CNT based nanocomposite strain sensors only have limited stretchability and sensitivity for measuring diverse human motions. Additionally, strain sensors fabricated by traditional techniques are only capable of measuring strain in a single direction, but for monitoring human motion with complicated strain condition, strain sensors that can measure strain from multi-direction are favorable. In this dissertation, highly stretchable (in excess of 45% strain) and sensitive (gauge factor of 35.75) strain sensors with tunable strain gauge factors were fabricated by incorporating CNT layers into polymer substrate using SDM printing technique. The cyclic loading-unloading test results revealed that the composite strain sensors exhibited excellent long-term durability. Due to the flexibility of the printing technique, rosette-typed sensors were fabricated to monitor complicated human motions. These superior sensing capabilities of the fabricated nanocomposites offer potential applications in wearable strain sensors. Resistive heating properties of CNT based nanocomposites were also investigated. The electrically resistive heating of these composites can be a desirable stimulus to activate the shape memory effect of polymer matrix. CNT based nanocomposites fabricated by traditional techniques showed a slow heating rate and same shape recovery ratio at different locations in nanocomposites. However, from the practical applications like smart skin or smart tooling perspective, programmable shape recovery ratio at specified locations are desirable. In this dissertation, the CNT based nanocomposites with a fast heating rate and controllable maximum surface temperature were fabricated using SDM technique. The study on the shape memory effect of nanocomposites showed that their shape recoverability was approximately 100% taking 30s under a low voltage of 40V. It is worth noting that through programming the number of printed CNT layers at different locations, the shape recovery rate could be controlled and localized actuation with the desired recovery ratio was achieved. The high efficiency of heating coupling with wide adjustability of surface temperature and shape recovery ratio at specified locations make the fabricated nanocomposites a promising candidate for electrical actuation applications.
Show less - Date Issued
- 2017
- Identifier
- CFE0006819, ucf:52892
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006819
- Title
- Microstructual Characteristics of Magnesium Metal Matrix Composites.
- Creator
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Shin, Dongho, Sohn, Yongho, Coffey, Kevin, Suryanarayana, Challapalli, University of Central Florida
- Abstract / Description
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Magnesium (Mg) Metal matrix composites (MMCs) reinforced by ceramic reinforcements are being developed for a variety of applications in automotive and aerospace because of their strength-to-weight ratio. Reinforcement being considered includes SiC, Al2O3, Carbon fiber and B4C in order to improve the mechanical properties of MMCs. Microstructural and interfacial characteristics of MMCs can play a critical role in controlling the MMCs' mechanical properties. This study was carried out to...
Show moreMagnesium (Mg) Metal matrix composites (MMCs) reinforced by ceramic reinforcements are being developed for a variety of applications in automotive and aerospace because of their strength-to-weight ratio. Reinforcement being considered includes SiC, Al2O3, Carbon fiber and B4C in order to improve the mechanical properties of MMCs. Microstructural and interfacial characteristics of MMCs can play a critical role in controlling the MMCs' mechanical properties. This study was carried out to understand the microstructural and interfacial development between Mg-9wt.Al-1wt.Zn (AZ91) alloy matrix and several reinforcements including SiC, Al2O3, Carbon fibers and B4C. X-ray diffraction, scanning electron microscopy and transmission electron microscopy was employed to investigate the microstructure and interfaces. Al increase in hardness due to the presence of reinforcements was also documented via Vicker's hardness measurements. Thermodynamic consideration based on Gibbs free energy was employed along with experimental results to describe the interfacial characteristics of MMCs. Reaction products from AZ91-SiC and AZ91-Al2O3 interfaces were identified as MgO, since the surface of SiC particles is typically covered with SiO2 and the MgO is the most thermodynamically stable phase in these systems. The AZ91-Carbon fiber interface consist of Al4C3 and this carbide phase is considered detrimental to the mechanical toughness of MMCs. The AZ91-B4C interface was observed to contain MgB2 and MgB2C2. In general, Vicker's hardness increased by 3X due to the presence of these reinforcements.
Show less - Date Issued
- 2012
- Identifier
- CFE0004441, ucf:49324
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004441
- Title
- Phase Field Modeling of Thermotransport in Multicomponent Systems.
- Creator
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Bush, Joshua, Sohn, Yongho, Suryanarayana, Challapalli, Coffey, Kevin, University of Central Florida
- Abstract / Description
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Nuclear and gas turbine power plants, computer chips, and other devices and industries are running hotter than ever for longer than ever. With no apparent end to the trend, the potential arises for a phenomenon known as thermotransport to cause undesirable changes in these high temperature materials. The diffuse-interface method known as the phase-field model is a useful tool in the simulation and prediction of thermotransport driven microstructure evolution in materials. The objective of...
Show moreNuclear and gas turbine power plants, computer chips, and other devices and industries are running hotter than ever for longer than ever. With no apparent end to the trend, the potential arises for a phenomenon known as thermotransport to cause undesirable changes in these high temperature materials. The diffuse-interface method known as the phase-field model is a useful tool in the simulation and prediction of thermotransport driven microstructure evolution in materials. The objective of this work is to develop a phase-field model using practical and empirical properties of thermodynamics and kinetics for simulating the interdiffusion behavior and microstructural evolution of single and multiphase binary alloy system under composition and/or temperature gradients. Simulations are carried out using thermodynamics and kinetics of real systems, such as the U-Zr solid metallic fuel, with emphasis on the temperature dependencies of the kinetics governing diffusional interactions in single-phase systems and microstructural evolution in the presence of multiple driving forces in multi-phase systems.A phase field model is developed describing thermotransport in the ? phase of the U-Zr alloy, a candidate for advanced metallic nuclear fuels. The model is derived using thermodynamics extracted from the CALPHAD database and temperature dependent kinetic parameters associated with thermotransport from the literature. Emphasis is placed upon the importance of the heat of transport, Q*, and atomic mobility, ?. Temperature dependencies of each term are estimated from empirical data obtained directly from the literature, coupled with the textbook phenomenological formulae of each parameter. A solution is obtained via a finite volume approach with the aid of the FiPy(&)#174; partial differential equation solver. Results of the simulations are described based on individual flux contributions from the gradients of both composition and temperature, and are found to be remarkably similar to experimental results from the literature.In an additional effort the thermotransport behavior of a binary two-phase alloy is modeled, for the first time, via the phase-field method for a two-phase (? + ?) U-Zr system. The model is similarly built upon CALPHAD thermodynamics describing the ? and ? phases of the U-Zr system and thermotransport parameters for the ? phase from literature. A parametric investigation of how the heats of transport for U and Zr in the ? phase affect the redistribution is performed, and the interplay between system kinetics and thermodynamics are examined. Importantly, a strict control over the microstructure that is placed into the temperature gradient (at t=0) is used to eliminate the randomness associated with microstructural evolution from an initially unstable state, allowing an examination of exactly how the ? phase thermotransport parameters affect the redistribution behavior of the system. Results are compared to a control scenario in which the system evolves only in the presence of thermodynamic driving forces, and the kinetic parameters that are associated with thermotransport are negligible. In contrast to the single-phase simulations, in the presence of a large thermodynamic drive for phase transformation and stability, the constituent redistribution caused by the thermotransport effect is comparatively smaller.
Show less - Date Issued
- 2012
- Identifier
- CFE0004363, ucf:49436
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004363
- Title
- Effects of Allotropic Transformations on Interdiffusion Behavior in Binary Systems.
- Creator
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Ewh, Ashley, Sohn, Yongho, Suryanarayana, Challapalli, Coffey, Kevin, University of Central Florida
- Abstract / Description
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Diffusion plays a significant role in most materials systems by controlling microstructural development. Consequently, the overall properties of a material can be largely dependent upon diffusion. This study investigated the interdiffusion behavior of three binary systems, namely, Mo-Zr, Fe-Mo, and Fe-Zr. The main interest in these particular metals is for application in nuclear fuel assemblies. Nuclear fuel plates generally consist of two main components which are the fuel and the cladding....
Show moreDiffusion plays a significant role in most materials systems by controlling microstructural development. Consequently, the overall properties of a material can be largely dependent upon diffusion. This study investigated the interdiffusion behavior of three binary systems, namely, Mo-Zr, Fe-Mo, and Fe-Zr. The main interest in these particular metals is for application in nuclear fuel assemblies. Nuclear fuel plates generally consist of two main components which are the fuel and the cladding. Due to diffusional interactions that can occur between these two components, a third is sometimes added between the fuel and cladding to serve as a diffusion barrier layer. Fe, Mo, and Zr can act as either cladding or barrier layer constituents and both Mo and Zr also serve as alloying additions in uranium based metallic fuels. Therefore, a fundamental understanding of the diffusional interactions in these systems is critical in predicting the performance and lifetime of these fuels. In order to study this diffusion behavior, a series of solid-to-solid diffusion couples were assembled between Fe, Mo, and Zr. These couples were then diffusion annealed isothermally for various predetermined times over a range of temperatures, including some both above and below the allotropic transformation temperatures for Fe and Zr. Following the diffusion anneal, the couples were water quenched, cross-sectioned, and prepared for microstructural and compositional characterization. A combination of scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and electron probe microanalysis (EPMA) were used to obtain micrographs showing the microstructure and to collect compositional data for identifying intermediate phases and determining concentration profiles across the interdiffusion zone.Based on this characterization, the phases that developed in the diffusion zones were identified. In the Mo-Zr system, a large Zr solid solution layer developed in the couples annealed at and above 850(&)deg;C and a thin (~1-2 ?m) layer of Mo2Zr formed in all couples. Growth constants and concentration dependent interdiffusion coefficients were calculated for the Mo2Zr and Zr solid solution phases, respectively. In the Fe-Mo system, both the ?-Fe2Mo and ?-Fe7Mo6 phases were observed in couples annealed at 900(&)deg;C and below while ?-Fe7Mo6 and ?-Fe solid solution layers were observed in couples annealed above 900(&)deg;C. The relevant growth constants and activation energies for growth were calculated. In the Fe-Zr system, the couple annealed at 750(&)deg;C developed an FeZr2 and an FeZr3 layer while the couple annealed at 850(&)deg;C developed an Fe2Zr and Fe23Zr6 layer in the diffusion zone. The results of this analysis were then compared to available information from literature and the corresponding binary phase diagrams for each system. The results are discussed with respect to the effects of the allotropic transformations of Fe and Zr on the interdiffusion behavior in these systems.
Show less - Date Issued
- 2012
- Identifier
- CFE0004374, ucf:49422
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004374
- Title
- Enhanced Structure and Crystallinity of Semiconducting Polymer Films Through Electrospray Deposition.
- Creator
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Rodriguez, Johan, Deng, Weiwei, Challapalli, Suryanarayana, Orlovskaya, Nina, University of Central Florida
- Abstract / Description
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Electrospray atomization is a method that uses electrical stresses as the means of generatingcharged droplets. The fundamental working principles of electrospray have previously been extensivelystudied and demonstrated to have monodisperse droplet size distribution, good stabilityand scalability. Electrospray is a bottom-up deposition method which opens up the possibility of aroll-to-roll compatible process and is functional at regular atmospheric conditions. Due to this setof positive...
Show moreElectrospray atomization is a method that uses electrical stresses as the means of generatingcharged droplets. The fundamental working principles of electrospray have previously been extensivelystudied and demonstrated to have monodisperse droplet size distribution, good stabilityand scalability. Electrospray is a bottom-up deposition method which opens up the possibility of aroll-to-roll compatible process and is functional at regular atmospheric conditions. Due to this setof positive qualities, this atomization method holds promise as a means of solution based materialprocessing that is cost effective and scalable. Conjugated polymers are among the solution processablematerials of most interest, poly(3-hexylthiophene)(P3HT) standing out as one of the mostextensively studied. Applications of P3HT as a p-type semiconductor have been demonstrated indevices like organic solar cells, light emitting diodes and transistors. Improvements in the performanceof the mentioned devices have been correlated with a higher degree of crystallinity as wellas the film structure in the case of organic solar cells.The effects of different electrospray process parameters are investigated and various P3HT filmstructures are presented in this study. Electric repulsion present within the droplets in electrosprayand evaporation of the solvent were used to obtain high aspect ratio features on the P3HT films. Aclever design for the electrospray nozzle devised to improve the process stability is presented. Also,the crystallinity of the films was characterized using grazing incidence x-ray diffraction (GIXRD)and ultraviolet visible spectroscopy. All results in this study are presented as a comparison tospin coated control process. The GIXRD results suggest that the electrospray process producescrystallites that have an orientation opposite of the orientation observed in the spin coated process.Analysis of the ultraviolet visible spectroscopy absorption spectrum shows a red-shift, signalingan increase in the crystallinity. Lastly, good contact between the deposited P3HT and the substratewas confirmed using conductive atomic force microscopy (CAFM).iii
Show less - Date Issued
- 2015
- Identifier
- CFE0005879, ucf:50881
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0005879
- Title
- Phase Transformations and Microstructural Evolution in the U-10 wt.% Mo Alloy with Various Zr Additions at 900C and 650C.
- Creator
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Eriksson, Nicholas, Sohn, Yongho, Challapalli, Suryanarayana, Coffey, Kevin, University of Central Florida
- Abstract / Description
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The Reduced Enrichment for Research and Test Reactor (RERTR) now known as the Material Minimization and Management Reactor Control program (MMMRC) seeks to replace the use of highly enriched uranium (HEU) fuels used in research and test nuclear reactors around the world. The low enriched uranium (LEU) fuels must have fissionable uranium densities comparable to the HEU fuels. After extensive investigation by various researchers around the world, the U-Mo alloys were selected as a promising...
Show moreThe Reduced Enrichment for Research and Test Reactor (RERTR) now known as the Material Minimization and Management Reactor Control program (MMMRC) seeks to replace the use of highly enriched uranium (HEU) fuels used in research and test nuclear reactors around the world. The low enriched uranium (LEU) fuels must have fissionable uranium densities comparable to the HEU fuels. After extensive investigation by various researchers around the world, the U-Mo alloys were selected as a promising candidate. The Mo alloyed with U allows for the stabilization of the face-centered cubic ?-U phase, which demonstrated favorable irradiation behavior. However, deleterious diffusional interaction between the fuel and the cladding, typically Al-base alloy, remain a challenge to overcome for application of U-Mo alloys as the LEU fuel. Zr has been identified as a potential diffusion barrier between monolithic U-10 wt.% Mo (U10Mo) metallic fuel and AA6061 cladding alloys for the development of a LEU fuel system. However, interdiffusion and reaction between the Zr barrier and U10Mo fuel can produce phases such as Mo2Zr, and promote the destabilization of ?-U phase into ?'-U (U2Mo) and ?-U. In order to better understand this phenomenon, this study examined the phases that are present in the U10Mo alloys with varying Zr concentration, 0, 0.5, 1.0, 2.0, 5.0, 10.0, 20.0 wt.% at room temperature after heat treatment at 900(&)deg;C for 168 hours and 650(&)deg;C for 3 hours. These two temperatures are relevant to fuel plate fabrication process of homogenization and hot-rolling, respectively. Scanning electron microscopy and X-ray diffraction were employed to identify and quantitatively document the constituent phases and microstructure to elucidate the nature of phase transformations. For U10Mo alloys containing less than 1.0 wt.% Zr, there was no significant formation of Mo2Zr after 900?C homogenization and subsequent heat treatment at 650?C for 3 hours. The ?-U phase also remained stable correspondingly for these alloys containing less than 1.0 wt.% Zr. For U10Mo alloys containing 2 wt.% or more Zr, a significant amount of Mo2Zr formation was observed after 900?C homogenization and subsequent heat treatment at 650?C for 3 hours. For these alloys, destabilization of ?-U into ?'-U (U2Mo), UZr2 and ?-U was observed. The alloy containing 20 wt.% Zr, however, did not demonstrate ?-U decomposition even though Mo2Zr was observed after heat treatments. The formation of Mo2Zr effectively reduced the stability of the metastable ?-U phase by depleting the ?-stabilizing Mo. The destabilization of ?-U phase into the ?-U phase is not favorable due to anisotropic and poor irradiation behavior of ?-U phase. Therefore the formation of Mo2Zr at the interface between U10Mo fuel and Zr diffusion barrier must be carefully controlled during the fabrication of monolithic LEU fuel system for successful implementation.
Show less - Date Issued
- 2015
- Identifier
- CFE0005943, ucf:50812
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0005943
- Title
- Quantification of the Effect of Degassing on the Microstructure, Chemistry and Estimated Strength of Nanocrystalline AA5083 Powder.
- Creator
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Hofmeister, Clara, Sohn, Yongho, Challapalli, Suryanarayana, Coffey, Kevin, University of Central Florida
- Abstract / Description
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Degassing is a critical heat treatment process in aluminum powder metallurgy, where powders are subjected to high temperature in vacuum to remove volatile gaseous species absorbed in and adsorbed on powders. For cryomilled aluminum alloy powders with nanoscale features, degassing can cause accelerated microstructural and chemical changes including removal of volatiles, grain growth, dislocation annihilation, and formation of dispersoids. These changes can significantly alter the mechanical...
Show moreDegassing is a critical heat treatment process in aluminum powder metallurgy, where powders are subjected to high temperature in vacuum to remove volatile gaseous species absorbed in and adsorbed on powders. For cryomilled aluminum alloy powders with nanoscale features, degassing can cause accelerated microstructural and chemical changes including removal of volatiles, grain growth, dislocation annihilation, and formation of dispersoids. These changes can significantly alter the mechanical behavior of consolidated components based on their contributions to strength. In this study, cryomilled AA5083 (0.4 wt.% Mn; 4.5 wt.% Mg; minor Si, Fe, Cu, Cr, Zn, Ti; balance Al) powders were degassed at 200, 300, 350, 410 and 500(&)deg;C at a ramp rate of 68.3 (&)deg;C?hr-1 for a soak time of 8 hours with a vacuum at or below 6.5 x 10-3 Pa. Grain size, dislocation density and dispersoid phase constituents were examined as a function of degassing temperature by X-ray diffraction, scanning electron microscopy and transmission electron microscopy, equipped with high angle annular dark field detector and X-ray energy dispersive spectroscopy. Inert gas fusion and thermal conductivity analysis were employed to determine the oxygen, nitrogen and hydrogen concentrations as a function of degassing temperature. Grain size in as-cryomilled powders (21 ~ 34 nm) increased as a function of degassing temperature, and reached a maximum value of 70 ~ 80 nm for powders degassed at 500(&)deg;C for 8 hours. The dislocation density of 1.11 x 1015 m-2 in as-cryomilled powders decreased to 1.56 x 1014 m-2 for powders degassed at 500(&)deg;C for 8 hours. The Al6(MnFeCr) phase was the most commonly observed dispersoid, mostly on samples degassed at or above 300(&)deg;C. Volume fraction increased with degassing temperature up to 5 vol.% and the size of the dispersoids grew up to ~ 280 nm. Oxygen and nitrogen content after cryomilling were unaffected by the change in degassing temperature, but the hydrogen content decreased and reached a minimum of 45 (&)#177; 3.16 ppm for cryomilled powders degassed at 500(&)deg;C for 8 hours. Grain growth was quantitatively analyzed based on the general grain growth formula and Burke's model in the presence of pinning forces. Degassing occurred in two different kinetic regimes: Harrison A kinetics at higher temperatures and Harrison B in the lower with a transition temperature of about 287(&)deg;C. Burke's model exhibited a poor fit to the experimental results in higher temperature regime. Desorption of impurities during degassing was analyzed using Fickian diffusion in a spherical coordinate system and an empirical expression based on the exponential decay of average concentration. The activation energy for degassing was estimated to be 16.2 (&)#177; 1.5 kJ?mol-1. Evolutions in composition and microstructure in cryomilled powders as a function of degassing temperature were further analyzed and quantitatively correlated to the strengthening mechanisms of solid solution, grain size reduction (i.e., Hall-Petch), dislocation forest and Orowan. For consolidated AA5083 derived from cryomilled powders, strengthening by grain size reduction was the dominant mechanism of strengthening.
Show less - Date Issued
- 2016
- Identifier
- CFE0006461, ucf:51426
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006461
- Title
- The Influence of Alloying Additions on Diffusion and Strengthening of Magnesium.
- Creator
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Kammerer, Catherine, Sohn, Yongho, Coffey, Kevin, Challapalli, Suryanarayana, Gordon, Ali, University of Central Florida
- Abstract / Description
-
Magnesium alloys are being developed as advanced materials for structural applications where reduced weight is a primary motivator. Alloying can enhance the properties of magnesium without significantly affecting its density. Essential to alloy development, inclusive of processing parameters, is knowledge of thermodynamic, kinetic, and mechanical behavior of the alloy and its constituents. Appreciable progress has been made through conventional development processes, but to accelerate...
Show moreMagnesium alloys are being developed as advanced materials for structural applications where reduced weight is a primary motivator. Alloying can enhance the properties of magnesium without significantly affecting its density. Essential to alloy development, inclusive of processing parameters, is knowledge of thermodynamic, kinetic, and mechanical behavior of the alloy and its constituents. Appreciable progress has been made through conventional development processes, but to accelerate development of suitable wrought Mg alloys, an integrated Materials Genomic approach must be taken where thermodynamics and diffusion kinetic parameters form the basis of alloy design, process development, and properties-driven applications.The objective of this research effort is twofold: first, to codify the relationship between diffusion behavior, crystal structure, and mechanical properties; second, to provide fundamental data for the purpose of wrought Mg alloy development. Together, the principal deliverable of this work is an advanced understanding of Mg systems. To that end, the objective is accomplished through an aggregate of studies. The solid-to-solid diffusion bonding technique is used to fabricate combinatorial samples of Mg-Al-Zn ternary and Mg-Al, Mg-Zn, Mg-Y, Mg-Gd, and Mg-Nd binary systems. The combinatorial samples are subjected to structural and compositional characterization via Scanning Electron Microscopy with X-ray Energy Dispersive Spectroscopy, Electron Probe Microanalysis, and analytical Transmission Electron Microscopy. Interdiffusion in binary Mg systems is determined by Sauer-Freise and Boltzmann-Matano methods. Kirkaldy's extension of the Boltzmann-Matano method, on the basis of Onsager's formalism, is employed to quantify the main- and cross-interdiffusion coefficients in ternary Mg solid solutions. Impurity diffusion coefficients are determined by way of the Hall method. The intermetallic compounds and solid solutions formed during diffusion bonding of the combinatorial samples are subjected to nanoindentation tests, and the nominal and compositionally dependent mechanical properties are extracted by the Oliver-Pharr method.In addition to bolstering the scantly available experimental data and first-principles computations, this work delivers several original contributions to the state of Mg alloy knowledge. The influence of Zn concentration on Al impurity diffusion in binary Mg(Zn) solid solution is quantified to impact both the pre-exponential factor and activation energy. The main- and cross-interdiffusion coefficients in the ternary Mg solid solution of Mg-Al-Zn are reported wherein the interdiffusion of Zn is shown to strongly influence the interdiffusion of Mg and Al. A critical examination of rare earth element additions to Mg is reported, and a new phase in thermodynamic equilibrium with Mg-solid solution is identified in the Mg-Gd binary system. It is also demonstrated that Mg atoms move faster than Y atoms. For the first time the mechanical properties of intermetallic compounds in several binary Mg systems are quantified in terms of hardness and elastic modulus, and the influence of solute concentration on solid solution strengthening in binary Mg alloys is reported. The most significant and efficient solid solution strengthening is achieved by alloying Mg with Gd. The Mg-Nd and Mg-Gd intermetallic compounds exhibited better room temperature creep resistance than intermetallic compounds of Mg-Al. The correlation between the concentration dependence of mechanical properties and atomic diffusion is deliberated in terms of electronic nature of the atomic structure.
Show less - Date Issued
- 2015
- Identifier
- CFE0005815, ucf:50043
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0005815
- Title
- Development of Nitrogen Concentration During Cryomilling of Aluminum Composites.
- Creator
-
Hofmeister, Clara, Sohn, Yongho, Suryanarayana, Challapalli, Coffey, Kevin, University of Central Florida
- Abstract / Description
-
The ideal properties of a structural material are light weight with extensive strength and ductility. A composite with high strength and tailorable ductility was developed consisting of nanocrystalline AA5083, boron carbide and coarser grained AA5083. The microstructure was determined through optical microscopy and transmission electron microscopy. A technique was developed to determine the nitrogen concentration of an AA5083 composite from secondary ion mass spectrometry utilizing a nitrogen...
Show moreThe ideal properties of a structural material are light weight with extensive strength and ductility. A composite with high strength and tailorable ductility was developed consisting of nanocrystalline AA5083, boron carbide and coarser grained AA5083. The microstructure was determined through optical microscopy and transmission electron microscopy. A technique was developed to determine the nitrogen concentration of an AA5083 composite from secondary ion mass spectrometry utilizing a nitrogen ion-implanted standard. Aluminum nitride and amorphous nitrogen-rich dispersoids were found in the nanocrystalline aluminum grain boundaries. Nitrogen concentration increased as a function of cryomilling time up to 72hours. A greater nitrogen concentration resulted in an enhanced thermal stability of the nanocrystalline aluminum phase and a resultant increase in hardness. The distribution of the nitrogen-rich dispersoids may be estimated considering their size and the concentration of nitrogen in the composite. Contributions to strength and ductility from the Orowan relation can be more accurately modeled with the quantified nitrogen concentration.
Show less - Date Issued
- 2013
- Identifier
- CFE0004864, ucf:49702
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004864
- Title
- PROCESSING AND CHARACTERIZATION OF MULTIFUNCTIONAL THERMOPLASTIC NANOCOMPOSITE FILMS.
- Creator
-
Wang, Xin, Gou, Jihua, Challapalli, Suryanarayana, Xu, Yunjun, University of Central Florida
- Abstract / Description
-
Nanoparticles reinforced polymer composite films have been widely studied for their enhanced mechanical, electrical and thermal properties compared with host polymer matrix. However, most research was conducted on incorporation of nanoparticles in polymer films to improve single property and there is a lack of research on the multifunctional polymer nanocomposite films. In this work, a scalable and continuous spray deposition process was developed for the production of nanoparticles...
Show moreNanoparticles reinforced polymer composite films have been widely studied for their enhanced mechanical, electrical and thermal properties compared with host polymer matrix. However, most research was conducted on incorporation of nanoparticles in polymer films to improve single property and there is a lack of research on the multifunctional polymer nanocomposite films. In this work, a scalable and continuous spray deposition process was developed for the production of nanoparticles reinforced multifunctional thermoplastic nanocomposite films. This process is capable of making a thin sheet of thermoplastic nanocomposites with high nanoparticle loadings. The smallest thickness can be 40um.The objective of this study is to design and optimize the thermoplastic nanocomposite films by utilizing nanoclay and helical carbon nanotube for multifunctional application: a) high electrical conductivity and thermal stability. Helical carbon nanotube paper based thermoplastic polyurethane nanocomposite films have been studied. The electrical conductivity and thermal stability of nanocomposite films increase a lot due to the incorporation of helical carbon nanotube paper with high electrical and thermal conductivity. The peculiar helical configuration of carbon nanotubes could greatly improve the interfacial bonding between carbon nanotubes and polymer matrix. b)High wear resistance and thermal stability. A nanoclay reinforced thermoplastic polyurethane nanocomposite coating was applied on the surface of leather. Due to the high hardness and thermal stability of nanoclay, the leather coated with nanocomposite film showed an improvement of wear resistance and thermal stability.
Show less - Date Issued
- 2014
- Identifier
- CFE0005734, ucf:50105
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0005734
- Title
- Nanoscale Spectroscopy in Energy and Catalytic Applications.
- Creator
-
Ding, Yi, Tetard, Laurene, Challapalli, Suryanarayana, Zhai, Lei, Thomas, Jayan, Lyakh, Arkadiy, Blair, Richard, University of Central Florida
- Abstract / Description
-
Emerging societal challenges such as the need for more sustainable energy and catalysis are requiring more sensitive and versatile measurements at the nanoscale. This is the case in the design and optimization of new materials for energy harvesting (solar cells) and energy storage devices (batteries and capacitors), or for the development of new catalysts for carbon sequestration or other reactions of interest. Hence, the ability to advance spectroscopy with nanoscale spatial resolution and...
Show moreEmerging societal challenges such as the need for more sustainable energy and catalysis are requiring more sensitive and versatile measurements at the nanoscale. This is the case in the design and optimization of new materials for energy harvesting (solar cells) and energy storage devices (batteries and capacitors), or for the development of new catalysts for carbon sequestration or other reactions of interest. Hence, the ability to advance spectroscopy with nanoscale spatial resolution and high sensitivity holds great promises to meet the demands of deeper fundamental understanding to boost the development and deployment of nano-based devices for real applications. In this dissertation, the impact of nanoscale characterization on energy-related and catalytic materials is considered. Firstly an introduction of the current energy and environmental challenges and our motivations are presented. We discuss how revealing nanoscale properties of solar cell active layers and supercapacitor electrodes can greatly benefit the performance of devices, and ponder on the advantages over conventional characterization techniques. Next, we focus on two dimensional materials as promising alternative catalysts to replace conventional noble metals for carbon sequestration and its conversion to added-value products. Defect-laden hexagonal boron nitride (h-BN) has been identified as a good catalyst candidate for carbon sequestration. Theoretically, defects exhibit favorable properties as reaction sites. However, the detailed mechanism pathways cannot be readily probed experimentally, due to the lack of tools with sufficient sensitivity and time resolution. A comprehensive study of the design and material processes used to introduce defects in h-BN in view of improving the catalytic properties is presented. The processing-structure-property relationships are investigated using a combination of conventional characterization and advanced nanoscale techniques. In addition to identifying favorable conditions for defect creation, we also report on the first signs of local reactions at defect sites obtained with nanoscale spectroscopy. Next, we explore avenues to improve the sensitivity and time-resolution of nanoscale measurements using light-assisted AFM-based nanomechanical spectroscopy. For each configuration, we evaluate the new system by comparing its performance to the commercial capabilities.Lastly, we provide a perspective on the opportunities for state-of-the-art characterization to impact the fields of catalysis and sustainable energy, as well as the urge for highly sensitive functional capabilities and time-resolution for nanoscale studies.
Show less - Date Issued
- 2018
- Identifier
- CFE0007751, ucf:52387
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0007751
- Title
- Fabrication and Characterization of Nonlinear Optical Ceramics for Random Quasi-Phase-Matching.
- Creator
-
Chen, Xuan, Gaume, Romain, Richardson, Kathleen, Challapalli, Suryanarayana, Sohn, Yongho, Kuebler, Stephen, University of Central Florida
- Abstract / Description
-
A number of technologies rely on the conversion of short laser pulses from one spectral domain to another. Efficient frequency conversion is currently obtained in ordered nonlinear optical materials and requires a periodic spatial modulation of their nonlinear coefficient which results in a narrow bandwidth. One can trade off efficiency for more spectral bandwidth by relaxing the strict phase-matching conditions and achieve nonlinear interaction in carefully engineered disordered crystalline...
Show moreA number of technologies rely on the conversion of short laser pulses from one spectral domain to another. Efficient frequency conversion is currently obtained in ordered nonlinear optical materials and requires a periodic spatial modulation of their nonlinear coefficient which results in a narrow bandwidth. One can trade off efficiency for more spectral bandwidth by relaxing the strict phase-matching conditions and achieve nonlinear interaction in carefully engineered disordered crystalline aggregates, in a so-called random quasi-phase-matching (rQPM) process. In this dissertation, we examine appropriate fabrication pathways for (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 (PMN-PT) and ZnSe transparent ceramics for applications in the mid-IR. The main challenge associated with the fabrication of high transparency PMN-PT ceramics is to avoid the parasitic pyrochlore phase. The most effective method to suppress the formation of this undesired phase is to use magnesium niobate (MgNb2O6) as the starting material. We have found that, contrary to commercially available lead oxide powders, nanopowders synthesized in our lab by the combustion method help improve the densification of ceramics and their overall optical quality. The effects of dopants on the microstructure evolution and phase-purity control in PMN-PT ceramics are also investigated and show that La3+ helps control grain-growth and get a pure perovskite phase, thereby improving the samples transparency. With large second order susceptibility coefficients and wide transmission window from 0.45 to 21 (&)#181;m, polycrystalline zinc selenide is also an ideal candidate material for accessing the MWIR spectrum through rQPM nonlinear interaction. We have investigated non-stoichiometric heat-treatment conditions necessary to develop adequate microstructure for rQPM from commercial CVD-grown ZnSe ceramics. We have been able to demonstrate the world's first optical parametric oscillation (OPO) based on rQPM in ZnSe transparent ceramic, enabling broadband frequency combs spanning 3-7.5 (&)#181;m.
Show less - Date Issued
- 2018
- Identifier
- CFE0007748, ucf:52403
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0007748
- Title
- Developing surface engineered liquid crystal droplets for sensing applications.
- Creator
-
Bera, Tanmay, Fang, Jiyu, Suryanarayana, Challapalli, Huo, Qun, Cho, Hyong, Deng, Weiwei, Wu, Shintson, University of Central Florida
- Abstract / Description
-
Diagnosis plays a very crucial role in medicine and health care, which makes biosensors extremely important in modern technological context. Till date, various types of biosensors have been developed that are capable of detecting a wide range of biologically important species with great sensitivity and selectivity. However, most of these sensing units require highly sophisticated instrumentation and often lack the desired portability. Liquid crystal (LC) droplets, on the other hand, are a new...
Show moreDiagnosis plays a very crucial role in medicine and health care, which makes biosensors extremely important in modern technological context. Till date, various types of biosensors have been developed that are capable of detecting a wide range of biologically important species with great sensitivity and selectivity. However, most of these sensing units require highly sophisticated instrumentation and often lack the desired portability. Liquid crystal (LC) droplets, on the other hand, are a new type of functional material that are finding increasing research attention as a new sensing unit due to their tunable optical property, high surface area, portability and cost-effectiveness. In this dissertation, functionalized LC droplets for biosensing at aqueous-LC interface are highlighted. Chemically functionalized LC droplets dispersed in aqueous solution were prepared by the self-assembly of amphiphilic molecules at the aqueous/LC interface. These functionalized LC droplets showed a well-defined director of configuration and a specific optical pattern when observed with a polarizing light microscope. It was discovered that the interaction of chemically functionalized LC droplets with an analyte triggers transition of the director of configuration of the LC within the droplets, providing a simple and unique optical sign for the detection of the analyte. Moreover, the director of configuration transition happened in a concentration dependent manner, allowing both qualitative and quantitative detection of the analyte. The sensitivity of chemically functionalized LC droplets depends not only on the nature of amphiphilic molecules but also the size and number of the droplets.The dissertation essentially deals with the application of these chemically functionalized LC droplets in detecting several biologically important species. It was observed that the adsorption of charged macromolecules (dendrimers, proteins, and viruses) on polyelectrolyte functionalized LC droplets triggered a bipolar-to-radial configuration transition based on the polar verses non-polar interaction. By using a simple optical microscope, microgram per milliliter concentrations of bovine serum albumin, cowpea mosaic virus, and tobacco mosaic virus could be detected in aqueous solution. The detection limit of Mastoparan X polypeptide decorated LC droplets in detecting E. coli could reach to approximately 10 bacteria per milliliter. In this case, the high affinity of the polypeptide towards the bacterial causes the former to detach from the LC droplets, triggering the director of configuration transition of the LC inside the droplets. Finally, surfactant decorated LC droplets were used to detect lithocholic acid (LCA), a toxic bile acid used as a specific biomarker for colon cancers. In this case, the director of configuration transition of the LC inside the droplets is a result of the replacement of the surfactant from the aqueous/LC interface by LCA. The microgram per milliliter concentration of LCA, a clinically significant concentration, could be easily detected by changing the length of surfactants. These studies highlight the novel use of surface functionalized LC droplets to detect biologically important species. Due to their tunable optical property, coupled with high surface area and portability, surface functionalized LC droplets have great potentials in the design of next generation biosensors.
Show less - Date Issued
- 2012
- Identifier
- CFE0004307, ucf:49471
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004307
- Title
- High Volume Fraction Mg-based Nanocomposites: Processing, Microstructure and Mechanical Behavior.
- Creator
-
Liu, Jinling, An, Linan, Suryanarayana, Challapalli, Fang, Jiyu, Bai, Yuanli, Lin, Kuo-Chi, University of Central Florida
- Abstract / Description
-
Mg-based metal matrix nanocomposites (MMNCs) with mechanical properties, superior to those of coarse-grained composites, are promising structural materials for applications in the automotive and aerospace industries. The research in this area was primarily focused earlier on either micro-scaled reinforcements or nano-scaled reinforcements with very low volume fractions. MMNCs with high volume fractions have not been explored yet. In this research, we study the processing, microstructures and...
Show moreMg-based metal matrix nanocomposites (MMNCs) with mechanical properties, superior to those of coarse-grained composites, are promising structural materials for applications in the automotive and aerospace industries. The research in this area was primarily focused earlier on either micro-scaled reinforcements or nano-scaled reinforcements with very low volume fractions. MMNCs with high volume fractions have not been explored yet. In this research, we study the processing, microstructures and properties of MMNCs containing ceramic nanoparticles up to 30 vol.%.We first investigated the mechanical alloying of Al2O3 nanoparticles and pure Mg under high-energy ball milling conditions. The phase evolution and their distribution were evaluated as a function of milling time. Then, the thermal stability of the formed nanocomposites was investigated by annealing it at high temperatures. It indicated that an exchange reaction had occurred to a large extent between Mg and Al2O3 resulting in the formation of Al and MgO phases. Additionally, the reaction between Al and un-reacted Mg led to the formation of Mg-Al intermetallics.Due to the reaction between Mg and Al2O3 during the milling and annealing process, we attempted to synthesize Mg/SiC nanocomposites. The mixed powders containing 0, 5, 10 and 15 vol.% SiC were produced by high energy ball milling and then the powders were consolidated via spark plasma sintering. The phase constitutions and microstructures of the Mg/SiC nanocomposites were characterized. SiC nanoparticles (average particle size ~14 nm) appear to be homogeneously dispersed within the matrix, and the average inter-particle spacings of all the Mg/SiC nanocomposites were smaller than 50 nm. Microscopic methods, even at high magnifications did not reveal any significant porosity in the as-processed MMNCs.Mechanical characterization of the Mg/SiC nanocomposites was conducted using the microindentation test. Besides the microhardness test, different intermediate pause times and loading rates were used to evaluate the stiffness and loading rate sensitivity of our samples. The abnormal microhardness and loading rate sensitivity were showed for the Mg-15 vol.% SiC samples. At the same time, the monotonic increase of stiffness with volume fraction was exhibited in the Mg/SiC nanocomposites.Finally, we investigated the quasi-static and dynamic response of Mg/SiC nanocomposites and microcomposites, and discussed the underlying mechanisms. Strain softening was noticed in the milled Mg sample under quasi-static compression. Similarly, the strengthening effect leveling off was also observed in the Mg-15 vol.% SiC samples under either quasi-static or high-strain rate uniaxial compression conditions. No significant plastic deformation was observed in the Mg/SiC nanocomposites. The estimated strain rate sensitivity of all the Mg/SiC nanocomposites in this work was around 0.03, which is much smaller than 0.3 and 0.6, observed for 100 nm and 45 nm grain size pure Mg individually. In particular, the existing models fail in predicting the inverse volume fraction effect, and other mechanisms are yet to be explored. The presence of SiC nanoparticles may play an important role that leads to this difference.
Show less - Date Issued
- 2013
- Identifier
- CFE0004879, ucf:49672
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004879
- Title
- SYNTHESIS AND CHARACTERIZATION OF STABLE AND METASTABLE PHASES IN Ni- AND Fe-BASED ALLOY SYSTEMS BY MECHANICAL ALLOYING.
- Creator
-
Al-Joubori, Ahmed, Challapalli, Suryanarayana, Vaidyanathan, Raj, Gou, Jihua, Bai, Yuanli, Lin, Kuo-Chi, University of Central Florida
- Abstract / Description
-
Mechanical Alloying (MA) is a process that involves repeated cold welding, fracturing and rewelding of powder particles in a high-energy ball mill and has been used extensively to synthesize both stable (equilibrium) and metastable phases in a number of alloy systems. This is due to its ability to achieve many effects simultaneously, viz., reduction in grain size, introduction of a variety of crystal defects, disordering of the lattice, and modifying the crystal structures of materials; all...
Show moreMechanical Alloying (MA) is a process that involves repeated cold welding, fracturing and rewelding of powder particles in a high-energy ball mill and has been used extensively to synthesize both stable (equilibrium) and metastable phases in a number of alloy systems. This is due to its ability to achieve many effects simultaneously, viz., reduction in grain size, introduction of a variety of crystal defects, disordering of the lattice, and modifying the crystal structures of materials; all these allowing alloying and phase transformations to occur in powders. In this Dissertation, we have synthesized a number of different alloy phases in Ni- and Fe-based alloy systems using MA.The as-received, blended, and milled powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy techniques to obtain information about the overall microstructure and chemical compositions. The NiX2 (X = Ge and Si) phases were synthesized in the Ni-Ge and Ni-Si systems. MA of Ni-Ge powder blends was investigated to study phase evolution as a function of milling time. On milling the powders for 5 h, the equilibrium NiGe phase started to form, and its amount in the powder increased with increasing milling time. On milling for about 60 h, the equilibrium intermetallic NiGe and Ge powder particles reacted to form the metastable NiGe2 phase. However, on milling for a longer time (75 h), the metastable phase transformed back to the equilibrium NiGe phase.Synthesis of the NiSi2 intermetallic phase depended on the Si content in the initial powder blend. For example, while in the Ni-60 at.% Si powder blend, only the NiSi phase was present homogeneously, the powder blend of the Ni-67 at.% Si composition contained the NiSi phase along with a small amount of unreacted Si. But in the Ni-75 at.% Si and Ni-80 at% compositions, the NiSi phase that had formed earlier (after 2 h of milling) and the remaining free Si powder reacted to form the equilibrium intermetallic NiSi2 phase. This constitution in the milled powder has been attributed to a partial loss of Si content during MA. Formation of Ni(Si) solid solutions with a solubility of about 18.2 at.% and 20.6 at.% for the Ni-75 at.% Si and Ni-80 at.% Si powder blends, respectively, was also achieved in the early stages of MA.In the Fe-C system, we were able to synthesize ferrite, cementite, and mixtures of the two phases. We were able to obtain the Fe-C solid solution phase (ferrite) with a BCC structure and the cementite phase with an orthorhombic structure in the eutectoid Fe-0.8 wt. % C composition, while a homogeneous cementite phase had formed at the higher carbon content of Fe-7.0 wt. % C after 30 h of milling time.In the case of the Fe-18Cr-xNi (x = 8, 12, and 20) system, the current investigation showed that the phase constitution depended significantly on the Ni content in the powder blend. Whereas mostly the martensite or the ferrite and austenite phase mixture was present at lower Ni contents, a completely homogeneous austenite phase was present in the alloy with 20% Ni.
Show less - Date Issued
- 2016
- Identifier
- CFE0006244, ucf:51059
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006244
- Title
- X-ray Scattering Investigations of Metallic Thin Films.
- Creator
-
Warren, Andrew, Coffey, Kevin, Sohn, Yongho, Suryanarayana, Challapalli, Heinrich, Helge, Barmak, Katayun, Toney, Michael, University of Central Florida
- Abstract / Description
-
Nanometric thin films are used widely throughout various industries and for various applications. Metallic thin films, specifically, are relied upon extensively in the microelectronics industry, among others. For example, alloy thin films are being investigated for CMOS applications, tungsten films find uses as contacts and diffusion barriers, and copper is used often as interconnect material. Appropriate metrology methods must therefore be used to characterize the physical properties of...
Show moreNanometric thin films are used widely throughout various industries and for various applications. Metallic thin films, specifically, are relied upon extensively in the microelectronics industry, among others. For example, alloy thin films are being investigated for CMOS applications, tungsten films find uses as contacts and diffusion barriers, and copper is used often as interconnect material. Appropriate metrology methods must therefore be used to characterize the physical properties of these films. X-ray scattering experiments are well suited for the investigation of nano-scaled systems, and are the focus of this doctoral dissertation. Emphasis is placed on (1) phase identification of polycrystalline thin films, (2) the evaluation of the grain size and microstrain of metallic thin films by line profile analysis, and (3) the study of morphological evolution in solid/solid interfaces.To illustrate the continued relevance of x-ray diffraction for phase identification of simple binary alloy systems, Pt-Ru thin films, spanning the compositional range from pure Pt to pure Ru were investigated. In these experiments, a meta-stable extension of the HCP phase is observed in which the steepest change in the electronic work function coincides with a rapid change in the c/a ratio of the HCP phase.For grain size and microstrain analysis, established line profile methods are discussed in terms of Cu and W thin film analysis. Grain sizes obtained by x-ray diffraction are compared to transmission electron microscopy based analyses. Significant discrepancies between x-ray and electron microscopy are attributed to sub-grain misorientations arising from dislocation core spreading at the film/substrate interface. A novel "residual" full width half max parameter is introduced for examining the contribution of strain to x-ray peak broadening. The residual width is subsequently used to propose an empirical method of line profile analysis for thin films on substrates.X-ray reflectivity was used to study the evolution of interface roughness with annealing for a series of Cu thin films that were encapsulated in both SiO2 and Ta/SiO2. While all samples follow similar growth dynamics, notable differences in the roughness evolution with high temperature ex-situ annealing were observed. The annealing resulted in a smoothing of only one interface for the SiO2 encapsulated films, while neither interface of the Ta/SiO2 encapsulated films evolved significantly. The fact that only the upper Cu/SiO2 interface evolves is attributed to mechanical pinning of the lower interface to the rigid substrate. The lack of evolution of the Cu/Ta/SiO2 interface is consistent with the lower diffusivity expected of Cu in a Cu/Ta interface as compared to that in a Cu/SiO2 interface. The smoothing of the upper Cu/SiO2 interface qualitatively follows that expected for capillarity driven surface diffusion but with notable quantitative deviation.
Show less - Date Issued
- 2013
- Identifier
- CFE0004770, ucf:49784
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004770
- Title
- Interdiffusion and Impurity Diffusion in Magnesium Solid Solutions.
- Creator
-
Kammerer, Catherine, Sohn, Yongho, Coffey, Kevin, Suryanarayana, Challapalli, Gordon, Ali, University of Central Florida
- Abstract / Description
-
Magnesium, being lightweight, offers potential to be developed into extensive structural applications. The transportation segment has particular interest in Mg and Mg alloy for applications where reduced vehicle weight is proportional to increased fuel efficiency. Aluminum and zinc are two of the most common alloying elements in commercial Mg alloys. They improve the physical properties of Mg through solid solution strengthening and precipitation hardening. Diffusion plays a key role in the...
Show moreMagnesium, being lightweight, offers potential to be developed into extensive structural applications. The transportation segment has particular interest in Mg and Mg alloy for applications where reduced vehicle weight is proportional to increased fuel efficiency. Aluminum and zinc are two of the most common alloying elements in commercial Mg alloys. They improve the physical properties of Mg through solid solution strengthening and precipitation hardening. Diffusion plays a key role in the kinetics of and microstructural development during solidification and heat treatment. However, there is limited diffusion data available for Mg and Mg alloys. In particular, because Al is mono-isotopic, tracer diffusion data is not available. Interdiffusion of Mg solid solution with Zn also does not exist in literature. The diffusional interaction of Al and Zn in Mg solid solution at temperatures ranging from 623 (-) 723K was examined using solid-to-solid diffusion couple method. The objective of this thesis is two-fold: first, is the examination of interdiffusion in the Mg solid solution phase of the binary Mg-Al and Mg-Zn systems; second, is to explore non-conventional analytical methods to determine impurity diffusion coefficients. The quality of diffusion bonding was examined by optical microscopy and scanning electron microscopy with X-ray energy dispersive spectroscopy, and concentration profiles were determined using electron probe microanalysis with pure standards and ZAF matrix correction. Analytical methods of concentration profiles based on Boltzmann-Matano analysis for binary alloys are presented along with compositional dependent interdiffusion coefficients. As the concentration of Al or Zn approaches the dilute ends, an analytical approach based on the Hall method was employed to estimate the impurity diffusion coefficients.Zinc was observed to diffuse faster than Al, and in fact, the impurity diffusion coefficient of Al was smaller than the self-diffusion coefficient of Mg. In the Mg solid solution with Al, interdiffusion coefficients increased by an order of magnitude with an increase in Al concentration. Activation energy and pre-exponential factor for the average effective interdiffusion coefficient in Mg solid solution with Al was determined to be 186.8 KJ/mole and 7.69 x 10-1 m^2/sec. On the other hand, in the Mg solid solution with Zn, interdiffusion coefficients did not vary significantly as a function of Zn concentration. Activation energy and pre-exponential factor for the average effective interdiffusion coefficient in Mg solid solution with Zn was determined to be 129.5 KJ/mole and 2.67 x 10-4 m^2/sec. Impurity diffusion coefficients of Al in Mg was determined to have activation energy and pre-exponential factor of 144.1 KJ/mole and 1.61 x 10-4 m^2/sec. Impurity diffusion coefficients of Zn in Mg was determined to have activation energy and pre-exponential factor of 109.8 KJ/mole and 1.03 x 10-5 m^2/sec. Temperature and composition-dependence of interdiffusion coefficients and impurity diffusion coefficients are examined with respect to reported values in literature, thermodynamic factor, ?, diffusion mechanisms in hexagonal close packed structure, and experimental uncertainty.
Show less - Date Issued
- 2013
- Identifier
- CFE0004699, ucf:49851
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0004699
- Title
- Enhanced Microwave Hyperthermia using Nanoparticles.
- Creator
-
Urdaneta, Maryory, Wahid, Parveen, Sundaram, Kalpathy, Richie, Samuel, Gong, Xun, Challapalli, Suryanarayana, University of Central Florida
- Abstract / Description
-
In this dissertation a study of enhanced hyperthermia for cancer treatment through the use of magnetic nanoparticles is presented. Hyperthermia has been in use for many years, as a potential alternative method in cancer treatment, and high frequency microwave radiation has been used successfully to raise the tumor temperature to around 42(&)deg;C in superficial tumors without causing damage to surrounding healthy tissues. Magnetic fluid hyperthermia involves the use of magnetic nanoparticles...
Show moreIn this dissertation a study of enhanced hyperthermia for cancer treatment through the use of magnetic nanoparticles is presented. Hyperthermia has been in use for many years, as a potential alternative method in cancer treatment, and high frequency microwave radiation has been used successfully to raise the tumor temperature to around 42(&)deg;C in superficial tumors without causing damage to surrounding healthy tissues. Magnetic fluid hyperthermia involves the use of magnetic nanoparticles injected into the tumor before exposure to microwave radiation. The magnetic energy in the nanoparticles is converted into heat allowing for a more rapid rise of temperature in the tumor to the desired level. In addition, the nanoparticles allow the electromagnetic absorption to be focused in the tumor and can be used to treat deep tumors in organs, such as the liver. Iron oxide magnetic nanoparticles were considered for this study as they are non-toxic and bio-compatible. For the case of breast cancer, the values for the temperature and specific absorption rate (SAR) in the tumor and in the healthy tissue were obtained through simulations and validated by measurement done on phantom models. Various characteristics of the nanoparticles such as radius, magnetic susceptibility and concentration were considered. In order to take the effect of the blood flow, which causes cooling and helps maintain the body temperature, various blood perfusion rates for a tumor in the liver were studied. A human male model in SEMCAD X, in which blood flow can be adjusted, was used for simulations. The tumor was injected with the nanoparticles and the change in temperature upon exposure to electromagnetic radiation was observed. The simulated results were compared with measured results on a liver phantom model in which saline solution was used to model blood flow. There was good agreement between the measured and simulated results.
Show less - Date Issued
- 2015
- Identifier
- CFE0005731, ucf:50093
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0005731