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Effect of Friction-stir Processing on the Wear Behavior of Titanium (Ti-1Al-8V-5Fe) and Stainless Steel (A-286) Alloys

Description: The effect of friction stir processing (FSP) on the mechanical wear behavior was investigated for Ti-1Al-8V-5Fe (Ti-185) and stainless steel (Incoloy® A-286) alloys. The Ti-185 and A-286 alloys were tested in different processing conditions, including as rolled (AR), AR+FSP, and AR+FSP+aged. A high frequency reciprocating rig was used to simulate fretting-type wear of these alloys at room temperature. The Vickers micro-hardness and wear rates were calculated and compared for each processing condition. It was determined that along with increasing hardness in the stir zones, FSP resulted in improved wear resistance for both alloys. Specifically, wear rates in the stir zones were reduced to lowest values of 1.6 x 10-5 and 5.8 x 10-7 mm3/N·m for the AR+FSP+aged Ti-185 and A-286 alloys, respectively, despite lower hardness for A-286 alloy. Mechanistic studies were conducted to determine the reason behind these improvements in wear resistance and the effect of FSP on the microstructural evolution during wear. For the Ti-185 alloy, x-ray diffraction revealed that there was a phase transformation from β-Ti (AR+FSP) to α-Ti (AR+FSP+aged). This phase decomposition resulted in the harder and stiffer Ti phase responsible for lowering of wear rate in Ti-185. While x-ray diffraction confirmed the A-286 alloy retains its austenitic structure for all conditions, scanning electron microscopy revealed completely different wear track morphology structures. There was increased coarse abrasion (galling) with the AR+aged A-286 alloy compared to the much finer-scale abrasion with the AR+FSP+aged alloy, which was responsible for smaller and less abrasive wear debris, and hence lower wear rate. Furthermore, cross-sectional focused ion beam microscopy studies inside the stir zone of AR+FSP+aged A-286 alloy determined that a) increased micro-hardness was due to FSP-induced microscopic grain refinement, and b) the corresponding wear rate decrease was due to even finer wear-induced grain refinement. With both effects combined, the level of ...
Date: May 2015
Creator: Tinubu, Olusegun Olukunle

Nanohybrids Based on Solid and Foam Polyurethanes

Description: Polymer nanocomposites are a going part of Materials Science and Engineering. These new composite materials exhibit dimensional and thermal stability of inorganic materials and toughness and dielectric properties of polymers. Development of nanocomposites become an important approach to create high-performance composite materials. In this study silica, fly ash, silica nanotubes and carbon black particles have been added to modify polyurethane foam and thermoplastic polyurethanes. It has been found that the addition of silica can diminish the size of foam bubbles, resulting in an increased stiffness of the material, increase of the compressive strength, and greater resistance to deformation. However, the uniformity of bubbles is reduced, resulting in increased friction of the material. Fly ash added to the foam can make bubbles smaller and improve uniformity of cells. Therefore, the material stiffness and compressive strength, resistance to deformation, and has little impact on the dynamic friction of the material. Adding nanotubes make bubble size unequal, and the arrangement of the bubble uneven, resulting in decreased strength of the material, while the friction increases. After the addition of carbon black to the polyurethane foam, due to the special surface structure of the carbon black, the foam generates more bubbles during the foaming process changing the foam structure. Therefore, the material becomes soft, we obtain a flexible polyurethane foam. The results of mechanical properties determination of the thermoplastic polyurethane that adding particles may increase the stiffness and wear resistance of the thermoplastic polyurethane, while the tensile properties of the material are reduced. This phenomenon may be due to agglomeration of particles during the mixing process. Possibly the particles cannot be uniformly dispersed in the thermoplastic polyurethane.
Date: May 2015
Creator: Bo, Chong

Plasma Interactions on Organosilicate Glass Dielectric Films and Emerging Amorphous Materials- Approach to Pore Sealing and Chemical Modifications

Description: In-situ x-ray photoemission (XPS) and ex-situ FTIR studies of nanoporous organosilicate glass (OSG) films point to the separate roles of radicals vs. VUV photons in the carbon abstraction. The studies indicate that reaction with O2 in presence of VUV photons (~123 nm) result in significant carbon abstraction within the bulk and that the kinetics of this process is diffusion-limited. In contrast, OSG exposed to atomic O (no VUV) results in Si-C bond scission and Si-O bond formation, but this process is self-limiting after formation of ~1 nm thick SiO2 surface layer that inhibits further diffusion. Therefore, the diffusion-dominated kinetics of carbon abstraction observed for OSG exposed to O2 plasma is definitively attributed to the diffusion of O2 down OSG nanopores, reacting at photo-activated sites, rather than to the diffusion of atomic O. Pretreatment of OSG by 900 eV Ar+ ion bombardment also results in formation of 1 nm thick SiO2-like surface overlayer that inhibits O2 diffusion, inhibiting VUV+O2 and O2 plasma-induced reactions, and that the effectiveness of this treatment increases with ion kinetic energy. On the contrary, organosilicate glass (OSG) films with backbone carbon (-Si-R-Si-) exhibit significantly enhanced resistance to carbon loss upon exposure to O2 plasma, radicals and VUV+O2 compared to films with terminal methyl groups (Si-CH3). Films incorporating backbone carbon chains (-Si-R-Si-) were deposited from 1,2 bis (triethoxysilyl) ethane (BTESE) precursor by ebeam or plasma cross-linking. The radical effects on BTESE film indicates negligible carbon loss or Si oxidation, combined with C-O bond formation, under conditions where OSG films with terminal methyl groups exhibit > 80% carbon loss within the surface region of the film. C-O bond formation is never observed for terminal CH3 groups. Further, backbone carbon (-Si-R-Si-) films exposed to VUV+O2 exhibit self-limiting, minimal net carbon loss. This indicates that plasma-induced Si-C bond rupture still occurs ...
Date: May 2015
Creator: Kazi, Haseeb

Processing and Characterization of Polycarbonate Foams with Supercritical Co2 and 5-Phenyl-1H-tetrazole

Description: Since their discovery in the 1930s, polymeric foams have been widely used in the industry for a variety of applications such as acoustical and thermal insulation, filters, absorbents etc. The reason for this ascending trend can be attributed to factors such as cost, ease of processing and a high strength to weight ratio compared to non-foamed polymers. The purpose of this project was to develop an “indestructible” material made of polycarbonate (PC) for industrial applications. Due to the high price of polycarbonate, two foaming methods were investigated to reduce the amount of material used. Samples were foamed physically in supercritical CO2 or chemically with 5-phenyl-1H-tetrazole. After thermal characterization of the foams in differential scanning calorimetry (DSC), we saw that none of the foaming methods had an influence on the glass transition of polycarbonate. Micrographs taken in scanning electron microscopy (SEM) showed that foams obtained in physical and chemical foaming had different structures. Indeed, samples foamed in supercritical CO2 exhibited a microcellular opened-cell structure with a high cell density and a homogeneous cell distribution. On the other hand, samples foamed with 5-phenyl-1H-tetrazole had a macrocellular closed-cell structure with a much smaller cell density and a random cell distribution. Compression testing showed that polycarbonate foamed physically had a compression modulus a lot greater. Then, XLPE mesh 35 or 50 and wollastonite were added to the polymeric matrices to enhance the foaming process and the mechanical properties. DSC experiments showed that the addition of fillers changed the thermal properties of polycarbonate for both foaming methods by inducing a shift in glass transition. SEM revealed that fillers lowered the average cell diameter and increased the cell density. This phenomenon increased the compression modulus for polycarbonate foamed in supercritical CO2. However, mechanical properties decreased for samples foamed with 5-phenyl-1H-tetrazole due to their relative brittleness and ...
Date: May 2015
Creator: Cloarec, Thomas

Growth Mechanisms, and Mechanical and Thermal Properties of Junctions in 3D Carbon Nanotube-Graphene Nano-Architectures

Description: Junctions are the key component for 3D carbon nanotube (CNT)-graphene seamless hybrid nanostructures. Growth mechanism of junctions of vertical CNTs growing from graphene in the presence of iron catalysts was simulated via quantum mechanical molecular dynamics (QM/MD) methods. CNTs growth from graphene with iron catalysts is based on a ‘‘base-growth’’ mechanism, and the junctions were the mixture of C-C and Fe-C covalent bonds. Pure C-C bonded junctions could be obtained by moving the catalyst during CNT growth or etching and annealing after growth. The growth process of 3D CNT-graphene junctions on copper templates with nanoholes was simulated with molecular dynamic (MD) simulation. There are two mechanisms of junction formation: (i) CNT growth over the holes that are smaller than 3 nm, and (ii) CNT growth inside the holes that are larger than 3 nm. The growth process of multi-layer filleted CNT-graphene junctions on the Al2O3 template was also simulated with MD simulation. A simple analytical model is developed to explain that the fillet takes the particular angle (135°). MD calculations show that 135° filleted junction has the largest fracture strength and thermal conductivity at room temperature compared to junctions with 90°,120°, 150°, and 180° fillets. The tensile strengths of the as-grown C–C junctions, as well as the junctions embedded with metal nanoparticles (catalysts), were determined by a QM/MD method. Metal catalysts remaining in the junctions significantly reduce the fracture strength and fracture energy. Moreover, the thermal conductivities of the junctions were also calculated by MD method. Metal catalysts remaining in the junctions considerably lower the thermal conductivity of the 3D junctions.
Date: December 2014
Creator: Niu, Jianbing

Laser Surface Alloying of Refractory Metals on Aluminum for Enhanced Corrosion Resistance: Experimental and Computational Approaches

Description: Aluminum (Al) and its alloys are widely used in various technological applications, mainly due to the excellent thermal conductivity, non-magnetic, ecofriendly, easy formability and good recyclability. However due to the inferior corrosion resistance its applications are hampered in various engineering sectors. Besides, the corrosion related failures such as leakage of gas from pipeline, catastrophic breakdown of bridges and fire accidents in processing plants further puts the human life in jeopardy. Within the United States over $ 400 billion dollars per year are spent over research to understand and prevent the corrosion related failures. Recently, the development of transition metal(TM) aluminides (AlxTMy, where, TM = Mo, W, Ta, Nb, Cr, Zr and V) has received the global attention mainly due to high strength at elevated temperatures, light-weight, excellent corrosion and wear resistance. In light of this, surface modification via laser surface alloying (LSA) is a promising engineering approach to mitigate the corrosion and wear problems. In the present study the attempts are made to study the Al-Mo, Al-W, Al-Nb, and Al-Ta systems as a potential corrosion resistant coatings on aluminum. The refractory metal (Mo, W, Nb, Ta) precursor deposit was spray coated separately on aluminum substrate and was subsequently surface alloyed using a continuous wave diode-pumped ytterbium laser at varying laser energy densities. Microstructural analysis was conducted using scanning electron microscopy and further X-ray diffractometry was carried out to evaluate the various phases evolved during laser surface alloying. Corrosion resistance of laser alloyed coatings were evaluated using open circuit potential, cyclic potentiodynamic polarization, electrochemical impedance spectroscopy measurements were performed in 0.6 M NaCl solution (pH:6.9±0.2, 23˚C). Open circuit potential measurements indicate the more stable (steady state) potential values over long periods after laser surface alloying. Cyclic polarization results indicated reduction in the corrosion current density, enhancement in the polarization resistance, and ...
Date: December 2014
Creator: Rajamure, Ravi Shanker

Silver Tantalate: a High Temperature Tribological Investigation

Description: As technology advances, mechanical and electrical systems are subjugated to intense temperature fluctuations through their service life. Designing coatings that operate in extreme temperatures is, therefore, a continuing challenge within the tribology community. Silver tantalate was chosen for investigation at the atomic level, the physical and chemical properties that influence the thermal, mechanical, and tribological behavior for moving assemblies in high temperature tribological applications. By correlating behavior of internal physical processes to the macro tribological behavior, the tribological community will potentially gain improved predicative performance of solid lubricants in future investigations. Three different approaches were explored for the creation of such materials on Inconel substrates: (1) powders produced using a solid state which were burnished on the surface; (2) monolithic silver tantalate thin films deposited by magnetron sputtering; and, (3) an adaptive tantalum nitride/silver nanocomposite sputter-deposited coating that forms a lubricious silver tantalate oxide on its surface when operated at elevated temperatures. Dry sliding wear tests of the coatings against Si3N4 counterfaces revealed friction coefficients in the 0.06 - 0.15 range at T ~ 750 °C. Reduced friction coefficients were found in nanocomposite materials that contained primarily a AgTaO3 phase with a small amount of segregated Ag phase, as suggested by structural characterization using X-ray diffraction. The presence of nanoparticles of segregated Ag in the thin films further enhanced the performance of these materials by increasing their toughness. Additional characterization of the AgTaO3 films at 750 °C under normal loads of 1, 2, 5, or 10 N revealed that the friction monotonically increased as the load was increased. These results were complemented by molecular dynamics simulations, which confirmed the increase of friction with load. Further, the simulations support the hypothesis that this trend can be explained in terms of decreased presence of Ag clusters near the sliding surface and the ...
Date: December 2014
Creator: Stone, D’Arcy S.

Structural, Thermal and Acoustic Performance of Polyurethane Foams for Green Buildings

Description: Decreasing the carbon footprint through use of renewable materials has environmental and societal impact. Foams are a valuable constituent in buildings by themselves or as a core in sandwich composites. Kenaf is a Southeast USA plant that provides renewable filler. The core of the kenaf is porous with a cell size in a 5-10 micrometer range. The use of kenaf core in foams represents a novel multiscalar cellular structural composite. Rigid polyurethane foams were made using free foaming expansion with kenaf core as filler with loadings of 5, 10 and 15 %. Free foaming was found to negatively affect the mechanical properties. An innovative process was developed to introduce a constraint to expansion during foaming. Two expansion ratios were examined: 40 and 60 % (decreasing expansion ratio). MicroCT and SEM analysis showed a varying structure of open and closed cell pores. The mechanical, thermal insulation, acoustic properties were measured. Pure PU foam showed improved cell size uniformity. Introducing kenaf core resulted in decreasing the PU performance in the free expansion case. This was reversed by introducing constraints. To understand the combined impact of having a mixed close cell and open cell architecture, finite element modeling was done using ANSYS. Models were created with varying percentages of open, closed, and bulk cells to encompass entire range of foam porosities. Net zero energy building information modelling was conducted using EnergyPlus was conducted using natural fiber composite skins. Environmental impacts for instance global warming potential, acidification, eutrophication, fossil fuel consumption, ozone depletion, and smog potential of the materials used in construction was studied using life cycle assessment. The results showed improvement on energy consumption and carbon footprint.
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Date: December 2014
Creator: Nar, Mangesh

Surface Topography and Aesthetics of Recycled Cross-Linked Polyethylene Wire and Cable Coatings

Description: Our research focuses on re-using a waste a material, cross-linked polyethylene abbreviated XLPE, which is a widely used coating for wires. XLPE is strong and has excellent thermal properties due to its chemical structure - what leads to the significance of recycling this valuable polymer. Properties of XLPE include good resistance to heat, resistance to chemical corrosion, and high impact strength. A wire is usually composed of a metal core conductor and polymeric coating layers. One creates a new coating, including little pieces of recycled XLPE in the lower layer adjacent to the wire, and virgin XLPE only in the upper layer. Industries are often wasting materials which might be useful. Mostly, some returned or excess products could be recycled to create a new type of product or enable the original use. This method helps cleaning the waste, lowers the costs, and enhances the income of the manufacturing company. With the changing of the thickness of the outer layer, the roughness changes significantly. Moreover, different processing methods result in surfaces that look differently.
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Date: December 2014
Creator: Xie, Wa

Atomistic Computer Simulations of Diffusion Mechanisms in Lithium Lanthanum Titanate Solid State Electrolytes for Lithium Ion Batteries

Description: Solid state lithium ion electrolytes are important to the development of next generation safer and high power density lithium ion batteries. Perovskite-structured LLT is a promising solid electrolyte with high lithium ion conductivity. LLT also serves as a good model system to understand lithium ion diffusion behaviors in solids. In this thesis, molecular dynamics and related atomistic computer simulations were used to study the diffusion behavior and diffusion mechanism in bulk crystal and grain boundary in lithium lanthanum titanate (LLT) solid state electrolytes. The effects of defect concentration on the structure and lithium ion diffusion behaviors in LLT were systematically studied and the lithium ion self-diffusion and diffusion energy barrier were investigated by both dynamic simulations and static calculations using the nudged elastic band (NEB) method. The simulation results show that there exist an optimal vacancy concentration at around x=0.067 at which lithium ions have the highest diffusion coefficient and the lowest diffusion energy barrier. The lowest energy barrier from dynamics simulations was found to be around 0.22 eV, which compared favorably with 0.19 eV from static NEB calculations. It was also found that lithium ions diffuse through bottleneck structures made of oxygen ions, which expand in dimension by 8-10% when lithium ions pass through. By designing perovskite structures with large bottleneck sizes can lead to materials with higher lithium ion conductivities. The structure and diffusion behavior of lithium silicate glasses and their interfaces, due to their importance as a grain boundary phase, with LLT crystals were also investigated by using molecular dynamics simulations. The short and medium range structures of the lithium silicate glasses were characterized and the ceramic/glass interface models were obtained using MD simulations. Lithium ion diffusion behaviors in the glass and across the glass/ceramic interfaces were investigated. It was found that there existed a minor segregation ...
Date: August 2014
Creator: Chen, Chao-Hsu

Comparative Coarsening Kinetics of Gamma Prime Precipitates in Nickel and Cobalt Base Superalloys

Description: The increasing technological need to push service conditions of structural materials to higher temperatures has motivated the development of several alloy systems. Among them, superalloys are an excellent candidate for high temperature applications because of their ability to form coherent ordered precipitates, which enable the retention of high strength close to their melting temperature. The accelerated kinetics of solute diffusion, with or without an added component of mechanical stress, leads to coarsening of the precipitates, and results in microstructural degradation, limiting the durability of the materials. Hence, the coarsening of precipitates has been a classical research problem for these alloys in service. The prolonged hunt for an alternative of nickel base superalloys with superior traits has gained hope after the recent discovery of Co-Al-W based alloys, which readily form high temperature g precipitates, similar to Ni base superalloys. In the present study, coarsening behavior of g precipitates in Co-10Al-10W (at. %) has been carried out at 800°C and 900°C. This study has, for the first time, obtained critical coarsening parameters in cobalt-base alloys. Apart from this, it has incorporated atomic scale compositional information across the g/g interfaces into classical Cahn-Hilliard model for a better model of coarsening kinetics. The coarsening study of g precipitates in Ni-14Al-7 Cr (at. %) has shown the importance of temporal evolution of the compositional width of the g/g interfaces to the coarsening kinetics of g precipitates. This study has introduced a novel, reproducible characterization method of crystallographic study of ordered phase by coupling of orientation microscopy with atom probe tomography (APT). Along with the detailed analysis of field evaporation behaviors of Ni and Co superalloys in APT, the present study determines the site occupancy of various solutes within ordered g precipitates in both Ni and Co superalloys. This study has explained the role of structural ...
Date: August 2014
Creator: Meher, Subhashish

Computational Studies on Structures and Ionic Diffusion of Bioactive Glasses

Description: Bioactive glasses are a class of synthetic inorganic material that have wide orthopedics, dentistry, tissue engineering and other biomedical applications. The origin of the bioactivity is closely related to the atomic structures of these novel glass materials, which otherwise lack long range order and defies any direct experimental measurements due to their amorphous nature. The structure of bioactive glasses is thus essential for the understanding of bioactive behaviors and eventually rational design of glass compositions. In this dissertation, molecular dynamics (MD) and reverse monte carlo (RMC) based computer simulations have been used to systematically study the atomic structure of three classes of new bioactive glasses: strontium doped 45S5 Bioglass®, ZnO-SrO containing bioactive glasses, and Cao-MgO-P2O5-SiO2 bioactive glasses. Properties such as ionic diffusion that are important to glass dissolution behaviors are also examined as a function of glass compositions. The accuracy of structure model generated by simulation was validated by comparing with various experimental measurements including X-ray/neutron diffraction, NMR and Raman spectroscopy. It is shown in this dissertation that atomistic computer simulations, when integrated with structural and property characterizations, is an effective tool in understanding the structural origin of bioactivity and other properties of amorphous bioactive materials that can lead to design of novel materials for biomedical applications.
Date: August 2014
Creator: Xiang, Ye

Computational Study of Dislocation Based Mechanisms in FCC Materials

Description: Understanding the relationships between microstructures and properties of materials is a key to developing new materials with more suitable qualities or employing the appropriate materials in special uses. In the present world of material research, the main focus is on microstructural control to cost-effectively enhance properties and meet performance specifications. This present work is directed towards improving the fundamental understanding of the microscale deformation mechanisms and mechanical behavior of metallic alloys, particularly focusing on face centered cubic (FCC) structured metals through a unique computational methodology called three-dimensional dislocation dynamics (3D-DD). In these simulations, the equations of motion for dislocations are mathematically solved to determine the evolution and interaction of dislocations. Microstructure details and stress-strain curves are a direct observation in the simulation and can be used to validate experimental results. The effect of initial dislocation microstructure on the yield strength has been studied. It has been shown that dislocation density based crystal plasticity formulations only work when dislocation densities/numbers are sufficiently large so that a statistically accurate description of the microstructure can be obtainable. The evolution of the flow stress for grain sizes ranging from 0.5 to 10 µm under uniaxial tension was simulated using an improvised model by integrating dislocation pile-up mechanism at grain boundaries has been performed. This study showed that for a same initial dislocation density, the Hall–Petch relationship holds well at small grain sizes (0.5–2 µm), beyond which the yield strength remains constant as the grain size increases.
Date: August 2014
Creator: Yellakara, Ranga Nikhil

Gamma Prime Precipitation Mechanisms and Solute Partitioning in Ni-base Alloys

Description: Nickel-base superalloys have been emerged as materials for gas turbines used for jet propulsion and electricity generation. The strength of the superalloys depends mainly from an ordered precipitates of L12 structure, so called gamma prime (γ’) dispersed within the disorder γ matrix. The Ni-base alloys investigated in this dissertation comprise both model alloy systems based on Ni-Al-Cr and Ni-Al-Co as well as the commercial alloy Rene N5. Classical nucleation and growth mechanism dominates the γ’ precipitation process in slowed-cooled Ni-Al-Cr alloys. The effect of Al and Cr additions on γ’ precipitate size distribution as well as morphological and compositional development of γ’ precipitates were characterized by coupling transmission electron microscopy (TEM) and 3D atom probe (3DAP) techniques. Rapid quenching Ni-Al-Cr alloy experiences a non-classical precipitation mechanism. Structural evolution of the γ’ precipitates formed and subsequent isothermal annealing at 600 °C were investigated by coupling TEM and synchrotron-based high-energy x-ray diffraction (XRD). Compositional evolution of the non-classically formed γ’ precipitates was determined by 3DAP and Langer, Bar-on and Miller (LBM) method. Besides homogeneous nucleation, the mechanism of heterogeneous γ’ precipitation involving a discontinuous precipitation mechanism, as a function of temperature, was the primary focus of study in case of the Ni-Al-Co alloy. This investigation coupled SEM, SEM-EBSD, TEM and 3DAP techniques. Lastly, solute partitioning and enrichment of minor refractory elements across/at the γ/ γ’ interfaces in the commercially used single crystal Rene N5 superalloy was investigated by using an advantage of nano-scale composition investigation of 3DAP technique.
Date: August 2014
Creator: Rojhirunsakool, Tanaporn

Processing, Structure and Tribological Property Relations of Ternary Zn-Ti-O and Quaternary Zn-Ti-Zr-O Nanocrystalline Coatings

Description: Conventional liquid lubricants are faced with limitations under extreme cyclic operating conditions, such as in applications that require lubrication when changing from atmospheric pressure to ultrahigh vacuum and ambient air to dry nitrogen (e.g., satellite components), and room to elevated (>500°C) temperatures (e.g., aerospace bearings). Alternatively, solid lubricant coatings can be used in conditions where synthetic liquid lubricants and greases are not applicable; however, individual solid lubricant phases usually perform best only for a limited range of operating conditions. Therefore, solid lubricants that can adequately perform over a wider range of environmental conditions are needed, especially during thermal cycling with temperatures exceeding 500°C. One potential material class investigated in this dissertation is lubricious oxides, because unlike other solid lubricant coatings they are typically thermodynamically stable in air and at elevated temperatures. While past studies have been focused on binary metal oxide coatings, such as ZnO, there have been very few ternary oxide and no reported quaternary oxide investigations. The premise behind the addition of the third and fourth refractory metals Ti and Zr is to increase the number of hard and wear resistant phases while maintaining solid lubrication with ZnO. Therefore, the major focus of this dissertation is to investigate the processing-structure-tribological property relations of composite ZnO, TiO2 and ZrO2 phases that form ternary (ZnTi)xOy and quaternary (ZnTiZr)xOy nanocrystalline coatings. The coatings were processed by atomic layer deposition (ALD) using a selective variation of ALD parameters. The growth structure and chemical composition of as-deposited and ex situ annealed ternary and quaternary oxide coatings were studied by combined x-ray diffraction/focused ion beam microscopy/cross-sectional transmission electron microscopy, and x-ray photoelectron spectroscopy/Auger electron spectroscopy, respectively. It was determined that the structure varied from purely nanocrystalline (ternary oxides) to composite amorphous/nanocrystalline (quaternary oxides) depending on ALD parameters and annealing temperatures. In particular, the ZnTiO3 ...
Date: August 2014
Creator: Ageh, Victor

Investigations in the Mechanism of Carbothermal Reduction of Yttria Stabilized Zirconia for Ultra-high Temperature Ceramics Application and Its Influence on Yttria Contained in It

Description: Zirconium carbide (ZrC) is a high modulus ceramic with an ultra-high melting temperature and, consequently, is capable of withstanding extreme environments. Carbon-carbon composites (CCCs) are important structural materials in future hypersonic aircraft; however, these materials may be susceptible to degradation when exposed to elevated temperatures during extreme velocities. At speeds of exceeding Mach 5, intense heating of leading edges of the aircraft triggers rapid oxidation of carbon in CCCs resulting in degradation of the structure and probable failure. Environmental/thermal barrier coatings (EBC/TBC) are employed to protect airfoil structures from extreme conditions. Yttria stabilized zirconia (YSZ) is a well-known EBC/TBC material currently used to protect metallic turbine blades and other aerospace structures. In this work, 3 mol% YSZ has been studied as a potential EBC/TBC on CCCs. However, YSZ is an oxygen conductor and may not sufficiently slow the oxidation of the underlying CCC. Under appropriate conditions, ZrC can form at the interface between CCC and YSZ. Because ZrC is a poor oxygen ion conductor in addition to its stability at high temperatures, it can reduce the oxygen transport to the CCC and thus increase the service lifetime of the structure. This dissertation investigates the thermodynamics and kinetics of the YSZ/ZrC/CCC system and the resulting structural changes across multiple size scales. A series of experiments were conducted to understand the mechanisms and species involved in the carbothermal reduction of ZrO2 to form ZrC. 3 mol% YSZ and graphite powders were uniaxially pressed into pellets and reacted in a graphite (C) furnace. Rietveld x-ray diffraction phase quantification determined that greater fractions of ZrC were formed when carbon was the majority mobile species. These results were validated by modeling the process thermochemically and were confirmed with additional experiments. Measurements were conducted to examine the effect of carbothermal reduction on the bond lengths in ...
Date: May 2014
Creator: Sondhi, Anchal

Laser Surface Treatment of Amorphous Metals

Description: Amorphous materials are used as soft magnetic materials and also as surface coatings to improve the surface properties. Furthermore, the nanocrystalline materials derived from their amorphous precursors show superior soft magnetic properties than amorphous counter parts for transformer core applications. In the present work, laser based processing of amorphous materials will be presented. Conventionally, the nanocrystalline materials are synthesized by furnace heat treatment of amorphous precursors. Fe-based amorphous/nanocrystalline materials due to their low cost and superior magnetic properties are the most widely used soft magnetic materials. However, achieving nanocrystalline microstructure in Fe-Si-B ternary system becomes very difficult owing its rapid growth rate at higher temperatures and sluggish diffusion at low temperature annealing. Hence, nanocrystallization in this system is achieved by using alloying additions (Cu and Nb) in the ternary Fe-Si-B system. Thus, increasing the cost and also resulting in reduction of saturation magnetization. laser processing technique is used to achieve extremely fine nanocrystalline microstructure in Fe-Si-B amorphous precursor. Microstructure-magnetic Property-laser processing co-relationship has been established for Fe-Si-B ternary system using analytical techniques. Laser processing improved the magnetic properties with significant increase in saturation magnetization and near zero coercivity values. Amorphous materials exhibit excellent corrosion resistance by virtue of their atomic structure. Fe-based amorphous materials are economical and due to their ease of processing are of potential interest to synthesize as coatings materials for wear and corrosion resistance applications. Fe-Cr-Mo-Y-C-B amorphous system was used to develop thick coatings on 4130 Steel substrate and the corrosion resistance of the amorphous coatings was improved. It is also shown that the mode of corrosion depends on the laser processing conditions. The microstructure evolution and the corrosion mechanisms operating are evaluated using post processing and post corrosion analysis.
Date: May 2014
Creator: Katakam, Shravana K.

Processing and Characterization of Nickel-Carbon Base Metal Matrix Composites

Description: Carbon nanotubes (CNTs) and graphene nanoplatelets (GNPs) are attractive reinforcements for lightweight and high strength metal matrix composites due to their excellent mechanical and physical properties. The present work is an attempt towards investigating the effect of CNT and GNP reinforcements on the mechanical properties of nickel matrix composites. The CNT/Ni (dry milled) nanocomposites exhibiting a tensile yield strength of 350 MPa (about two times that of SPS processed monolithic nickel ~ 160 MPa) and an elongation to failure ~ 30%. In contrast, CNT/Ni (molecular level mixed) exhibited substantially higher tensile yield strength (~ 690 MPa) but limited ductility with an elongation to failure ~ 8%. The Ni-1vol%GNP (dry milled) nanocomposite exhibited the best balance of properties in terms of strength and ductility. The enhancement in the tensile strength (i.e. 370 MPa) and substantial ductility (~40%) of Ni-1vol%GNP nanocomposites was achieved due to the combined effects of grain refinement, homogeneous dispersion of GNPs in the nickel matrix, and well-bonded Ni-GNP interface, which effectively transfers stress across metal-GNP interface during tensile deformation. A second emphasis of this work was on the detailed 3D microstructural characterization of a new class of Ni-Ti-C based metal matrix composites, developed using the laser engineered net shaping (LENSTM) process. These composites consist of an in situ formed and homogeneously distributed titanium carbide (TiC) as well as graphite phase reinforcing the nickel matrix. 3D microstructure helps in determining true morphology and spatial distribution of TiC and graphite phase as well as the phase evolution sequence. These Ni-TiC-C composites exhibit excellent tribological properties (low COF), while maintaining a relatively high hardness.
Date: May 2014
Creator: Borkar, Tushar Murlidhar

Thermoplastic and Thermoset Natural Fiber Composite and Sandwich Performance

Description: The objective of this thesis is to investigate the effects of adding natural fiber (kenaf fiber, retted kenaf fiber, and sugarcane fiber) into polymer materials. The effects are obtained by considering three main parts. 1. Performance in thermoplastic composites. The effect of fiber retting on polymer composite crystallization and mechanical performance was investigated. PHBV/PBAT in 80/20 blend ratio was modified using 5% by weight kenaf fiber. Dynamic mechanical analysis of the composites was done to investigate the glass transition and the modulus at sub-ambient and ambient temperatures. ESEM was conducted to analyze fiber topography which revealed smoother surfaces on the pectinase retted fibers. 2. Performance in thermoset composites. The effect of the incorporation of natural fibers of kenaf and of sugarcane combined with the polyester resin matrix is investigated. A comparison of mechanical properties of kenaf polyester composite, sugarcane polyester composite and pure polyester in tensile, bending, dynamic mechanical thermal analysis (DMA) and moisture test on performance is measured.. 3. Performance in sandwich composites. The comparison of the performance characteristics and mechanical properties of natural fiber composites panels with soft and rigid foam cores are evaluated. A thorough test of the mechanical behavior of composites sandwich materials in tensile, bending and DCB is presented here.
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Date: May 2014
Creator: Yang, Bing

Dynamic Adhesion and Self-cleaning Mechanisms of Gecko Setae and Spatulae

Description: Geckos can freely climb on walls and ceilings against their body weight at speed of over 1ms-1. Switching between attachment and detachment seem simple and easy for geckos, without considering the surface to be dry or wet, smooth or rough, dirty or clean. In addition, gecko can shed dirt particles during use, keeping the adhesive pads clean. Mimicking this biological system can lead to a new class of dry adhesives for various applications. However, gecko’s unique dry self-cleaning mechanism remains unknown, which impedes the development of self-cleaning dry adhesives. In this dissertation we provide new evidence and self-cleaning mechanism to explain how gecko shed particles and keep its sticky feet clean. First we studied the dynamic enhancement observed between micro-sized particles and substrate under dry and wet conditions. The adhesion force of soft (polystyrene) and hard (SiO2 and Al2O3) micro-particles on soft (polystyrene) and hard (fused silica and sapphire) substrates was measured using an atomic force microscope (AFM) with retraction (z-piezo) speed ranging over 4 orders of magnitude. The adhesion is strongly enhanced by the dynamic effect. When the retraction speeds varies from 0.02 µm/s to 156 µm/s, the adhesion force increases by 10% ~ 50% in dry nitrogen while it increases by 15%~70% in humid air. A dynamic model was developed to explain this dynamic effect, which agrees well with the experimental results. Similar dynamic enhancement was also observed in aqueous solution. The influence of dynamic factors related to the adhesion enhancement, such as particle inertia, viscoelastic deformations and crack propagation, was discussed to understand the dynamic enhancement mechanisms. Although particles show dynamic enhancement, Gecko fabrillar hair shows a totally different trend. The pull off forces of a single gecko seta and spatula was tested by AFM under different pull-off velocities. The result shows that both the spatula and ...
Date: December 2013
Creator: Xu, Quan

Dynamic Precipitation of Second Phase Under Deformed Condition in Mg-nd Based Alloy

Description: Magnesium alloys are the lightweight structural materials with high strength to weigh ratio that permits their application in fuel economy sensitive automobile industries. Among the several flavors of of Mg-alloys, precipitation hardenable Mg-rare earth (RE) based alloys have shown good potential due to their favorable creep resistance within a wide window of operating temperatures ranging from 150°C to 300°C. A key aspect of Mg-RE alloys is the presence of precipitate phases that leads to strengthening of such alloys. Several notable works, in literature, have been done to examine the formation of such precipitate phases. However, there are very few studies that evaluated the effect stress induced deformation on the precipitation in Mg-RE alloys. Therefore, the objective of this work is to examine influence of deformation on the precipitation of Mg-Nd based alloys. To address this problem, precipitation in two Mg-Nd based alloys, subjected to two different deformation conditions, and was examined via transmission electron microscopy (TEM) and atom probe tomography (APT). In first deformation condition, Md-2.6wt%Nd alloy was subjected to creep deformation (90MPa / 177ºC) to failure. Effect of stress-induced deformation was examined by comparing and contrasting with precipitation in non-creep tested specimens subjected to isothermal annealing (at 177ºC). In second condition, Mg-4.0Y-3.0Nd-0.5Zr (wt %) or WE43 alloy (with comparable Nd content as model Mg-Nd system) was subjected to hot rolling deformation at a sub-solvus temperature.
Date: December 2013
Creator: Dendge, Nilesh Bajirao

Integrated Computational and Experimental Approach to Control Physical Texture During Laser Machining of Structural Ceramics

Description: The high energy lasers are emerging as an innovative material processing tool to effectively fabricate complex shapes on the hard and brittle structural ceramics, which previously had been near impossible to be machined effectively using various conventional machining techniques. In addition, the in-situ measurement of the thermo-physical properties in the severe laser machining conditions (high temperature, short time duration, and small interaction volume) is an extremely difficult task. As a consequence, it is extremely challenging to investigate the evolution of surface topography through experimental analyses. To address this issue, an integrated experimental and computational (multistep and multiphysics based finite-element modeling) approach was employed to understand the influence of laser processing parameters to effectively control the various thermo-physical effects (recoil pressure, Marangoni convection, and surface tension) during transient physical processes (melting, vaporization) for controlled surface topography (surface finish). The results indicated that the material lost due to evaporation causes an increase in crater depth of machined cavity, whereas liquid expulsion created by the recoil pressure increases the material pileup height around the lip of machined cavity, the major attributes of surface topography (roughness). Also, it was found that the surface roughness increased with increase in laser energy density and pulse rate (from 10 to 50Hz), and with the decrease in distance between two pulses (from 0.6 to 0.1mm) or the increase in lateral and transverse overlap (0, 17, 33, 50, 67, and 83%). The results of the computational model are also validated by experimental observations with reasonably close agreement.
Date: December 2013
Creator: Vora, Hitesh D.

Laser Surface Modification on Az31b Mg Alloy for Bio-wettability

Description: Laser surface modification of AZ31B Magnesium alloy changes surface composition and roughness to provide improved surface bio-wettability. Laser processing resulted in phase transformation and grain refinement due to rapid quenching effect. Furthermore, instantaneous heating and vaporization resulted in removal of material, leading the textured surface generation. A study was conducted on a continuum-wave diode-pumped ytterbium laser to create multiple tracks for determining the resulting bio-wettability. Five different laser input powers were processed on Mg alloy, and then examined by XRD, SEM, optical profilometer, and contact angle measurement. A finite element based heat transfer model was developed using COMSOL multi-physics package to predict the temperature evolution during laser processing. The thermal histories predicted by the model are used to evaluate the cooling rates and solidification rate and the associated changes in the microstructure. The surface energy of laser surface modification samples can be calculated by measuring the contact angle with 3 different standard liquid (D.I water, Formamide, and 1-Bromonaphthalen). The bio-wettability of the laser surface modification samples can be conducted by simulated body fluid contact angle measurement. The results of SEM, 3D morphology, XRD, and contact angle measurement show that the grain size and roughness play role for wetting behavior of laser processing Mg samples. Surface with low roughness and large grain size performs as hydrophilicity. On the contrast, surface with high roughness and small grain size performs as hydrophobicity.
Date: December 2013
Creator: Ho, YeeHsien

Nano-crystallization Inhibition in 5 Nm Ru Film Diffusion Barriers for Advanced Cu-interconnect

Description: As the semiconductor industries are moving beyond 22 nm node technology, the currently used stacked Ta/TaN diffusion barrier including a copper seed will be unable to fulfill the requirements for the future technologies. Due to its low resistivity and ability to perform galvanic copper fill without a seed layer, ruthenium (Ru) has emerged as a potential copper diffusion barrier. However, its crystallization and columnar nanostructure have been the main cause of barrier failures even at low processing temperatures (300 oC -350 oC). In this study, we have proposed and evaluated three different strategies to improve the performance of the ultrathin Ru film as a diffusion barrier for copper. The first study focused on shallow surface plasma irradiation/amorphization and nitridation of 5 nm Ru films. Systematic studies of amorphization and nitrogen incorporation versus sample bias were performed. XPS, XRD and RBS were used to determine the physico-chemical, crystallization and barrier efficiency of the plasma modified Ru barrier. The nitrogen plasma surface irradiation of Ru films at substrate bias voltage of -350 V showed an improved barrier performance up to 400 oC annealing temperatures. The barrier barely started failing at 450 oC due mainly to nitrogen instability. The second study involved only amorphization of the Ru thin film without any nitrogen incorporation. A low energy ion beam irradiation/amorphization on Ru thin film was carried out by using 60 KeV carbon ions with different irradiation doses. The irradiation energy was chosen high enough so that the irradiation ions pass through the whole Ru thin film and stop in the SiO2/Si support substrate. The C-ion fluence of 5×1016 atoms/cm2 at 60 KeV made the Ru film near amorphous without changing its composition. XRD and RBS were used to determine the relationship between crystallization and barrier efficiency of the carbon irradiated Ru barrier. The amorphized ...
Date: December 2013
Creator: Sharma, Bed P.