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Piezoresistive Polyvinylidene Fluoride/Carbon Filled Nanocomposites

Description: This thesis examines the value of using dispersed conductive fillers as a stress/strain sensing material. The effect of the intrinsic conductivity of the filler on the ability to be effective and the influence of filler concentration on the conductivity are also examined. To meet these objectives, nanocomposites of polyvinylidene fluoride (PVDF) with carbon nanofibers (CNFs) and carbon nanotubes (CNTs) were prepared by melt-blending using a twin screw extruder. Since PVDF has a potential to be piezoresistive based on the type of crystalline phase, the effect of CNFs on PVDF crystallinity, crystalline phase, quasi static and dynamic mechanical property was studied concurrently with piezoresponse. Three time dependencies were examined for PVDF/CNTs nanocomposites: quasi-static, transient and cyclic fatigue. The transient response of the strain with time showed viscoelastic behavior and was modeled by the 4-element Burger model. Under quasi-static loading the resistance showed negative pressure coefficient below yield but changed to a positive pressure coefficient after yield. Under cyclic load, the stress-time and resistance-time were synchronous but the resistance peak value decreased with increasing cycles, which was attributed to charge storage in the nanocomposite. The outcomes of this thesis indicate that a new piezoresponsive system based on filled polymers is a viable technology for structural health monitoring.
Date: May 2011
Creator: Vidhate, Shailesh

The Influence of Ohmic Metals and Oxide Deposition on the Structure and Electrical Properties of Multilayer Epitaxial Graphene on Silicon Carbide Substrates

Description: Graphene has attracted significant research attention for next generation of semiconductor devices due to its high electron mobility and compatibility with planar semiconductor processing. In this dissertation, the influences of Ohmic metals and high dielectric (high-k) constant aluminum oxide (Al2O3) deposition on the structural and electrical properties of multi-layer epitaxial graphene (MLG) grown by graphitization of silicon carbide (SiC) substrates have been investigated. Uniform MLG was successfully grown by sublimation of silicon from epitaxy-ready, Si and C terminated, 6H-SiC wafers in high-vacuum and argon atmosphere. The graphene formation was accompanied by a significant enhancement of Ohmic behavior, and, was found to be sensitive to the temperature ramp-up rate and annealing time. High-resolution transmission electron microscopy (HRTEM) showed that the interface between the metal and SiC remained sharp and free of macroscopic defects even after 30 min, 1430 °C anneals. The impact of high dielectric constant Al2O3 and its deposition by radio frequency (RF) magnetron sputtering on the structural and electrical properties of MLG is discussed. HRTEM analysis confirms that the Al2O3/MLG interface is relatively sharp and that thickness approximation of the MLG using angle resolved X-ray photoelectron spectroscopy (ARXPS) as well as variable-angle spectroscopic ellipsometry (VASE) is accurate. The totality of results indicate that ARXPS can be used as a nondestructive tool to measure the thickness of MLG, and that RF sputtered Al2O3 can be used as a (high-k) constant gate oxide in multilayer grapheme based transistor applications.
Date: May 2011
Creator: Maneshian, Mohammad Hassan

Bioresorbable Polymer Blend Scaffold for Tissue Engineering

Description: Tissue engineering merges the disciplines of study like cell biology, materials science, engineering and surgery to enable growth of new living tissues on scaffolding constructed from implanted polymeric materials. One of the most important aspects of tissue engineering related to material science is design of the polymer scaffolds. The polymer scaffolds needs to have some specific mechanical strength over certain period of time. In this work bioresorbable aliphatic polymers (PCL and PLLA) were blended using extrusion and solution methods. These blends were then extruded and electrospun into fibers. The fibers were then subjected to FDA standard in vitro immersion degradation tests where its mechanical strength, water absorption, weight loss were observed during the eight weeks. The results indicate that the mechanical strength and rate of degradation can be tailored by changing the ratio of PCL and PLLA in the blend. Processing influences these parameters, with the loss of mechanical strength and rate of degradation being higher in electrospun fibers compared to those extruded. A second effort in this thesis addressed the potential separation of the scaffold from the tissue (loss of apposition) due to the differences in their low strain responses. This hypothesis that using knit with low tension will have better compliance was tested and confirmed.
Date: May 2011
Creator: Manandhar, Sandeep

Synthesis and Characterization of Crystalline Assemblies of Functionalized Hydrogel Nanoparticles

Description: Two series monodispersed nanoparticles of hydroxylpropyl cellulose (HPC) and functionalized poly-N-isopropylamide (PNIPAM) particles have been synthesized and used as building blocks for creating three-dimensional networks, with two levels of structural hierarchy. The first level is HPC nanoparticles were made from methacrylated or degradable cross-linker attached HPC. These nanoparticles could be stabilized at room temperature by residual methacrylate or degradable groups are present both within and on the exterior of HPC nanoparticles. Controlled release studies have been performed on the particle and networks .The nearly monodispersed nanoparticles have been synthesized on the basis of a natural polymer of hydropropylcellulose (HPC) with a high molecular weight using the precipitation polymerization method and self-assembly of these particles in water results in bright colors. The HPC nanoparticles can be potential using as crosslinkers to increase the hydrogels mechanical properties, such as high transparency and rapid swelling/de-swelling kinetics. The central idea is to prepare colloidal particles containing C=C bonds and to use them as monomers - vinylparticles, to form stable particle assemblies with various architectures. This is accomplished by mixing an aqueous suspension of hydrogel nanoparticles (PNIPAM-co-allylamine) with the organic solvent (dichloromethane) to grow columnar crystals. The hydrogels with such a unique crystal structure behavior not only like the hydrogel opals, but also have a unique property: anisotropy.
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Date: December 2005
Creator: Cai, Tong

Growth, Structure and Tribological Properties of Atomic Layer Deposited Lubricious Oxide Nanolaminates

Description: Friction and wear mitigation is typically accomplished by introducing a shear accommodating layer (e.g., a thin film of liquid) between surfaces in sliding and/or rolling contacts. When the operating conditions are beyond the liquid realm, attention turns to solid coatings. Solid lubricants have been widely used in governmental and industrial applications for mitigation of wear and friction (tribological properties). Conventional examples of solid lubricants are MoS2, WS2, h-BN, and graphite; however, these and some others mostly perform best only for a limited range of operating conditions, e.g. ambient air versus dry nitrogen and room temperature versus high temperatures. Conversely, lubricious oxides have been studied lately as good potential candidates for solid lubricants because they are thermodynamically stable and environmentally robust. Oxide surfaces are generally inert and typically do not form strong adhesive bonds like metals/alloys in tribological contacts. Typical of these oxides is ZnO. The interest in ZnO is due to its potential for utility in a variety of applications. To this end, nanolaminates of ZnO, Al2O3, ZrO2 thin films have been deposited at varying sequences and thicknesses on silicon substrates and high temperature (M50) bearing steels by atomic layer deposition (ALD). The top lubricious, nanocrystalline ZnO layer was structurally-engineered to achieve low surface energy {0002}-orientated grain that provided low sliding friction coefficients (0.2 to 0.3), wear factors (range of 10-7 to 10-8 mm3/Nm) and good rolling contact fatigue resistance. The Al2O3 was intentionally made amorphous to achieve the {0002} preferred orientation while {101}-orientated tetragonal ZrO2 acted as a high toughness/load bearing layer. It was determined that the ZnO defective structure (oxygen sub-stoichiometric with growth stacking faults) aided in shear accommodation by re-orientating the nanocrystalline grains where they realigned to create new friction-reducing surfaces. Specifically, high resolution transmission electron microscopy (HRTEM) inside the wear surfaces revealed in an increase in ...
Date: December 2010
Creator: Mensah, Benedict Anyamesem

Effects of Plasma, Temperature and Chemical Reactions on Porous Low Dielectric Films for Semiconductor Devices

Description: Low-dielectric (k) films are one of the performance drivers for continued scaling of integrated circuit devices. These films are needed in microelectronic device interconnects to lower power consumption and minimize cross talk between metal lines that "interconnect" transistors. Low-k materials currently in production for the 45 and 65 nm node are most often organosilicate glasses (OSG) with dielectric constants near 2.8 and nominal porosities of 8-10%. The next generation of low-k materials will require k values 2.6 and below for the 45 nm device generation and beyond. The continuous decrease in device dimensions in ultra large scale integrated (ULSI) circuits have brought about the replacement of the silicon dioxide interconnect dielectric (ILD), which has a dielectric constant (k) of approximately 4.1, with low dielectric constant materials. Lowering the dielectric constant reduces the propagation delays, RC constant (R = the resistance of the metal lines; C = the line capacitance), and metal cross-talk between wires. In order to reduce the RC constants, a number of low-k materials have been studied for use as intermetal dielectrics. The k values of these dielectric materials can be lowered by replacing oxide films with carbon-based polymer films, incorporating hydrocarbon functional groups into oxide films (SiOCH films), or introducing porogens in the film during processing to create pores. However, additional integration issues such as damage to these materials caused by plasma etch, plasma ash, and wet etch processes are yet to be overcome. This dissertation reports the effects of plasma, temperature and chemical reactions on low-k SiOCH films. Plasma ash processes have been known to cause hydrophobic films to lose their hydrophobic methyl groups, rendering them to be hydrophilic. This allows the films to readily absorb moisture. Supercritical carbon dioxide (SC-CO2) can be used to transport silylating agents, hexamethyldisilazane (HMDS) and diethoxy-dimethlysilane (DEDMS), to functionalize the ...
Date: December 2010
Creator: Osei-Yiadom, Eric

Synthesis and characterization of crystalline assembly of poly Nisopropylacry-lamide)-co-acrylic acid nanoparticles.

Description: In this study, crystalline poly(N-isopropylacrylamide-co-acrylic acid) (PNIPAm-co-AAc) nanoparticle network in organic solvents was obtained by self assembling precursor particles in acetone/epichlorohydrin mixture at room temperature followed by inter-sphere crosslinking at ~98 °C. The crystals thus formed can endure solvent exchanges or large distortions under a temporary compressing force with the reoccurrence of crystalline structures. In acetone, the crystals were stable, independent of temperature, while in water crystals could change their colors upon heating or changing pH values. By passing a focused white light beam through the crystals, different colors were displayed at different observation angles, indicating typical Bragg diffraction. Shear moduli of the gel nanoparticle crystals were measured in the linear stress-yield ranges for the same gel crystals in both acetone and water. Syntheses of particles of different sizes and the relationship between particle size and the color of the gel nanoparticle networks at a constant solid content were also presented. Temperature- and pH- sensitive crystalline PNIPAm-co-AAc hydrogel was prepared using osmosis crosslinking method. Not only the typical Bragg diffraction phenomenon was observed for the hydrogel but also apparent temperature- and pH- sensitive properties were performed. The phase behavior of PNIPAm nanoparticles dispersed in water was also investigated using a thermodynamic perturbation theory combined with lightscattering and spectrometer measurements. It was shown how the volume transition of PNIPAM particles affected the interaction potential and determined a novel phase diagram that had not been observed in conventional colloids. Because both particle size and attractive potential depended on temperature, PNIPAM aqueous dispersion exhibited phase transitions at a fixed particle number density by either increasing or decreasing temperature. The phase transition of PNIPAm-co-AAc colloids was also studied. The results from the comparison between pure PNIPAm and charged PNIPAm colloids showed that the introducing of carboxyl (-COOH) group not only contributed to the synthesis ...
Date: December 2004
Creator: Zhou, Bo

Hydrophobic, fluorinated silica xerogel for low-k applications.

Description: A new hydrophobic hybrid silica film was synthesized by introducing one silicon precursor (as modifiers) into another precursor (network former). Hybrid films have improved properties. Hydrolysis and condensation of dimethyldiethoxysilane (DMDES) (solvent (EtOH) to DMDES molar ratio R = 4, water to DMDES molar ratio r = 4, 0.01 N HCl catalyst) was analyzed using high-resolution liquid 29Si NMR. It was found that after several hours, DMDES hydrolyzed and condensed into linear and cyclic species. Films from triethoxyfluorosilane (TEFS) have been shown to be promising interlayer dielectric materials for future integrated circuit applications due to their low dielectric constant and high mechanical properties (i.e., Young's modulus (E) and hardness (H)). Co-condensing with TEFS, linear structures from DMDES hydrolysis and condensation reactions rendered hybrid films hydrophobic, and cyclic structures induced the formation of pores. Hydrophobicity characterized by contact angle, thermal stability by thermogravimetric analysis (TGA), Fourier transform Infrared spectroscopy (FTIR), contact angle, and dynamic secondary ion mass spectroscopy (DSIMS), dielectric constant determined by impedance measurement, and mechanical properties (E and H) determined by nanoindentation of TEFS and TEFS + DMDES films were compared to study the effect of DMDES on the TEFS structure. Hybrid films were more hydrophobic and thermally stable. DMDES incorporation affected the dielectric constant, but showed little enhancement of mechanical properties.
Date: May 2004
Creator: Zhang, Zhengping

Electrical and Structure Properties of High-κ Barium Tantalite and Aluminum Oxide Interface with Zinc Oxide for Applications in Transparent Thin Film Transistors

Description: ZnO has generated interest for flexible electronics/optoelectronic applications including transparent thin film transistors (TFTs). For this application, low temperature processes that simultaneously yield good electrical conductivity and optical transparency and that are compatible with flexible substrates such as plastic, are of paramount significance. Further, gate oxides are a critical component of TFTs, and must exhibit low leakage currents and self-healing breakdown in order to ensure optimal TFTs switching performance and reliability. Thus, the objective of this work was twofold: (1) develop an understanding of the processing-structure-property relationships of ZnO and high-κ BaTa2O6 and Al2O3 (2) understand the electronic defect structure of BaTa2O6 /ZnO and Al2O3/ZnO interfaces and develop insight to how such interfaces may impact the switching characteristics (speed and switching power) of TFTs featuring these materials. Of the ZnO films grown by atomic layer deposition (ALD), pulsed laser deposition (PLD) and magnetron sputtering at 100-200 °C, the latter method exhibited the best combination of n-type electrical conductivity and optical transparency. These determinations were made using a combination of photoluminescence, photoluminescence excitation, absorption edge and Hall measurements. Metal-insulator-semiconductor devices were then fabricated with sputtered ZnO and high-κ BaTa2O6 and Al2O3 and the interfaces of high-κ BaTa2O6 and Al2O3 with ZnO were analyzed using frequency dependent C-V and G-V measurements. The insulator films were deposited at room temperature by magnetron sputtering using optimized processing conditions. Although the Al2O3 films exhibited a lower breakdown strength and catastrophic breakdown behavior compared to BaTa2O6/ZnO interface, the Al2O3/ZnO interface was characterized by more than an order of magnitude smaller density of interface traps and interface trapped charge. The BaTa2O6 films in addition were characterized by a significantly higher concentration of fixed oxide charge. The transition from accumulation to inversion in the Al2O3 MIS structure was considerably sharper, and occurred at less than one tenth of ...
Date: August 2011
Creator: Kuo, Fang-Ling

Mechanisms of Ordered Gamma Prime Precipitation in Nickel Base Superalloys

Description: Commercial superalloys like Rene88DT are used in high temperature applications like turbine disk in aircraft jet engines due to their excellent high temperature properties, including strength, ductility, improved fracture toughness, fatigue resistance, enhanced creep and oxidation resistance. Typically this alloy's microstructure has L12-ordered precipitates dispersed in disordered face-centered cubic γ matrix. A typical industrially relevant heat-treatment often leads to the formation of multiple size ranges of γ¢ precipitates presumably arising from multiple nucleation bursts during the continuous cooling process. The morphology and distribution of these γ′ precipitates inside γ matrix influences the mechanical properties of these materials. Therefore, the study of thermodynamic and kinetic factors influencing the evolution of these precipitates and subsequent effects is both relevant for commercial applications as well as for a fundamental understanding of the underlying phase transformations. The present research is primarily focused on understanding the mechanism of formation of different generations of γ′ precipitates during continuous cooling by coupling scanning electron microscopy (SEM), energy filtered TEM and atom probe tomography (APT). In addition, the phase transformations leading to nucleation of γ′ phase has been a topic of controversy for decades. The present work, for the first time, gives a novel insight into the mechanism of order-disorder transformations and associated phase separation processes at atomistic length scales, by coupling high angle annular dark field (HAADF) - STEM imaging and APT. The results indicate that multiple competing mechanisms can operate during a single continuous cooling process leading to different generations of γ′ including a non-classical mechanism, operative at large undercoolings.
Date: May 2011
Creator: Singh, Antariksh Rao Pratap

Phase Separation and Second Phase Precipitation in Beta Titanium Alloys

Description: The current understanding of the atomic scale phenomenon associated with the influence of beta phase instabilities on the evolution of microstructure in titanium alloys is limited due to their complex nature. Such beta phase instabilities include phase separation and precipitation of nano-scale omega and alpha phases in the beta matrix. The initial part of the present study focuses on omega precipitation within the beta matrix of model binary titanium molybdenum (Ti-Mo) alloys. Direct atomic scale observation of pre-transition omega-like embryos in quenched alloys, using aberration-corrected high resolution scanning transmission electron microscopy and atom probe tomography (APT) was compared and contrasted with the results of first principles computations performed using the Vienna ab initio simulation package (VASP) to present a novel mechanism of these special class of phase transformation. Thereafter the beta phase separation and subsequent alpha phase nucleation in a Ti-Mo-Al ternary alloy was investigated by coupling in-situ high energy synchrotron x-ray diffraction with ex-situ characterization studies performed using aberration corrected transmission electron microscopy and APT to develop a deeper understanding of the mechanism of transformation. Subsequently the formation of the omega phase in the presence of simultaneous development of compositional phase separation within the beta matrix phase of a Ti-10V-6Cu (wt%) alloy during continuous cooling has been investigated using a combination of transmission electron microscopy and atom probe tomography. The results of these investigations provided novel insights into the mechanisms of solid-state transformations in metallic systems by capturing the earliest stages of nucleation at atomic to near atomic spatial and compositional resolution.
Date: May 2011
Creator: Devaraj, Arun

Formation and Quantification of Corrosion Deposits in the Power Industry

Description: The presence of deposits on the secondary side of pressurized water reactor (PWR) steam generator systems is one of the main contributors to the high maintenance costs of these generators. Formation and transport of corrosion products formed due to the presence of impurities, metals and metallic oxides in the secondary side of the steam generator units result in formation of deposits. This research deals with understanding the deposit formation and characterization of deposits by studying the samples collected from different units in secondary side system at Comanche Peak Steam Electric Station (CPSES). Fourier transform infrared spectrophotometry (FTIR), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) have been used for studying the phases, morphologies and compositions of the iron oxides formed at Unit 1 and Unit 2 of secondary side of steamgenerator systems. Hematite and magnetite were found to be the dominant phases of iron oxides present in the units. Fe, Cr, O, Ni, Si, Cl and Cu were found in samples collected from both the units. A qualitative method was developed to differentiate iron oxides using laser induced breakdown spectroscopy (LIBS) based on temporal response of iron oxides to a high power laser beam. A quantitative FTIR technique was developed to identify and quantify iron oxides present in the different components of the secondary side of the steam generator of CPSES. Amines are used in water treatment to control corrosion and fouling in pressurized water reactors. CPSES presently uses an amine combination of dimethylamine (DMA), hydrazine and morpholine to control the water chemistry. Along with the abovementioned amines, this study also focuses on corrosion inhibition mechanismsof a new amine DBU (1, 8-diazabicyclo [5.4.0] undec-7-ene). Electrochemical impedance spectroscopy and polarization curves were used to study the interaction mechanism between DBU solution and inconel alloys 600 and 690 at steamgenerator operating ...
Date: May 2007
Creator: Namduri, Haritha

Surface Engineering and Characterization of Laser Deposited Metallic Biomaterials

Description: Novel net shaping technique Laser Engineered Net shaping™ (LENS) laser based manufacturing solution (Sandia Corp., Albuquerque, NM); Laser can be used to deposit orthopedic implant alloys. Ti-35Nb-7Zr-5Ta (TNZT) alloy system was deposited using LENS. The corrosion resistance being an important prerequisite was tested electrochemically and was found that the LENS deposited TNZT was better than conventionally used Ti-6Al-4V in 0.1N HCl and a simulated body solution. A detailed analysis of the corrosion product exhibited the presence of complex oxides which are responsible for the excellent corrosion resistance. In addition, the in vitro tests done on LENS deposited TNZT showed that they have excellent biocompatibility. In order to improve the wear resistance of the TNZT system boride reinforcements were carried out in the matrix using LENS processing. The tribological response of the metal matrix composites was studied under different conditions and compared with Ti-6Al-4V. Usage of Si3N4 balls as a counterpart in the wear studies showed that there is boride pullout resulting in third body abrasive wear with higher coefficient of friction (COF). Using 440C stainless steel balls drastically improved the COF of as deposited TNZT+2B and seemed to eliminate the effect of “three body abrasive wear,” and also exhibited superior wear resistance than Ti-6Al-4V.
Date: May 2007
Creator: Samuel, Sonia

Amorphization and De-vitrification in Immiscible Copper-Niobium Alloy Thin Films

Description: While amorphous phases have been reported in immiscible alloy systems, there is still some controversy regarding the reason for the stabilization of these unusual amorphous phases. Direct evidence of nanoscale phase separation within the amorphous phase forming in immiscible Cu-Nb alloy thin films using 3D atom probe tomography has been presented. This evidence clearly indicates that the nanoscale phase separation is responsible for the stabilization of the amorphous phase in such immiscible systems since it substantially reduces the free energy of the undercooled liquid (or amorphous) phase, below that of the competing supersaturated crystalline phases. The devitrification of the immiscible Cu-Nb thin film of composition Cu-45% Nb has been studied in detail with the discussion on the mechanism of phase transformation. The initial phase separation in the amorphous condition seems to play a vital role in the crystallization of the thin film. Detailed analysis has been done using X-ray diffraction, transmission electron microscopy and 3D atom probe tomography.
Date: May 2007
Creator: Puthucode Balakrishnan, Anantharamakrishnan

Biocompatible Hybrid Nanomaterials Involving Polymers and Hydrogels Interfaced with Phosphorescent Complexes and Toxin-Free Metallic Nanoparticles for Biomedical Applications

Description: The major topics discussed are all relevant to interfacing brightly phosphorescent and non-luminescent coinage metal complexes of [Ag(I) and Au(I)] with biopolymers and thermoresponsive gels for making hybrid nanomaterials with an explanation on syntheses, characterization and their significance in biomedical fields. Experimental results and ongoing work on determining outreaching consequences of these hybrid nanomaterials for various biomedical applications like cancer therapy, bio-imaging and antibacterial abilities are described. In vitro and in vivo studies have been performed on majority of the discussed hybrid nanomaterials and determined that the cytotoxicity or antibacterial activity are comparatively superior when compared to analogues in literature. Consequential differences are noticed in photoluminescence enhancement from hybrid phosphorescent hydrogels, phosphorescent complex ability to physically crosslink, Au(I) sulfides tendency to form NIR (near-infrared) absorbing AuNPs compared to any similar work in literature. Syntheses of these hybrid nanomaterials has been thoroughly investigated and it is determined that either metallic nanoparticles syntheses or syntheses of phosphorescent hydrogels can be carried in single step without involving any hazardous reducing agents or crosslinkers or stabilizers that are commonly employed during multiple step syntheses protocols for syntheses of similar materials in literature. These astounding results that have been discovered within studies of hybrid nanomaterials are an asset to applications ranging from materials development to health science and will have striking effect on environmental and green chemistry approaches.
Date: August 2011
Creator: Marpu, Sreekar B.

Void Growth and Collapse in a Creeping Single Crystal

Description: Aircraft engine components can be subjected to a large number of thermo-mechanical loading cycles and to long dwell times at high temperatures. In particular, the understanding of creep in single crystal superalloy turbine blades is of importance for designing more reliable and fuel efficient aircraft engines. Creep tests on single crystal superalloy specimens have shown greater creep strain rates for thinner specimens than predicted by current theories. Therefore, it is necessary to develop a more predictive description of creep processes in these materials for them to be used effectively. Experimental observations have shown that the crystals have an initial porosity and that the progressive growth of these voids plays a major role in limiting creep life. In order to understand void growth under creep in single crystals, we have analyzed the creep response of three dimensional unit cells with a single spherical void under different types of isothermal creep loading. The growth behavior of the void is simulated using a three dimensional rate dependent crystal plasticity constitutive relation in a quasi-static finite element analysis. The aim of the present work is to analyze the effect of stress traixiality and Lode parameter on void growth under both constant true stress and constant engineering stress isothermal creep loading.
Date: August 2011
Creator: Srivastava, Ankit

Tribological Improvements of Carbon-Carbon Composites by Infiltration of Atomic Layer Deposited Lubricious Nanostructured Ceramic Oxides

Description: A number of investigators have reported enhancement in oxidation and wear resistant of carbon-carbon composites (CCC) in the presence of protective coating layers. However, application of a surface and subsurface coating system that can preserve its oxidation and wear resistance along with maintaining lubricity at high temperature remains unsolved. To this end, thermodynamically stable protective oxides (ZnO/Al2O3/ZrO2) have been deposited by atomic layer deposition (ALD) to infiltrate porous CCC and graphite foams in order to improve the thermal stability and wear resistance in low and high speed sliding contacts. Characterization of microstructural evolution was achieved by using energy dispersive x-ray spectroscopy (EDS) mapping in scanning electron microscope (SEM) coupled with focused ion beam (FIB), x-ray tomography, high resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and X-ray diffraction (XRD). Evaluation of the tribological properties of CCC coated with abovementioned ALD thin films were performed by employing low speed pure sliding tribometer and a high speed/frequency reciprocating rig to simulate the fretting wear behavior at ambient temperature and elevated temperatures of 400°C.It was determined with x-ray tomography imaging and EDS mapping that ALD ZnO/Al2O3/ZrO2 nanolaminates and baseline ZrO2 coatings exhibited excellent conformality and pore-filling capabilities down to ~100 μm and 1.5 mm in the porous CCC and graphite foam, respectively, which were dependent on the exposure time of the ALD precursors. XRD and HRTEM determined the crystalline phases of {0002} textured ZnO (wurtzite), amorphous Al2O3, and {101}-tetragonal ZrO2. Significant improvements up to ~65% in the sliding and fretting wear factors were determined for the nanolaminates in comparison to the uncoated CCC. A tribochemical sliding-induced mechanically mixed layer (MML) was found to be responsible for these improvements. HRTEM confirmed the presence of a high density of ZnO shear-induced basal stacking faults inside the wear tracks responsible for intrafilm shear velocity ...
Date: August 2011
Creator: Mohseni, Hamidreza

Processing, Structure, and Tribological Property Interrelationships in Sputtered Nanocrystalline ZnO Coatings

Description: Solid lubricant coatings with controlled microstructures are good candidates in providing lubricity in moving mechanical assembly applications, such as orthopedics and bearing steels. Nanocrystalline ZnO coatings with a layered wurtzite crystal structure have the potential to function as a lubricious material by its defective structure which is controlled by sputter deposition. The interrelationships between sputtered ZnO, its nanocrystalline structure and its lubricity will be discussed in this thesis. The nanocrystalline ZnO coatings were deposited on silicon substrates and Ti alloys by RF magnetron sputtering with different substrate adhesion layers, direct current biases, and temperatures. X-ray diffraction identified that the ZnO (0002) preferred orientation was necessary to achieve low sliding friction and wear along with substrate biasing. In addition, other analyses such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were utilized to study the solid lubrication mechanisms responsible for low friction and wear.
Date: August 2009
Creator: Tu, Wei-Lun

Development of a Novel Grease Resistant Functional Coatings for Paper-based Packaging and Assessment of Application by Flexographic Press

Description: Recent commercial developments have created a need for alternative materials and methods for imparting oil/grease resistance to paper and/or paperboard used in packaging. The performance of a novel grease resistant functional coating comprised of polyvinyl alcohol (PVA), sodium tetraborate pentahydrate (borate) and acetonedicarboxylic acid (ACDA) and the application of said coating by means of flexographic press is presented herein. Application criteria is developed, testing procedures described, and performance assessment of the developed coating materials are made. SEM images along with contact angle data suggest that coating performance is probably attributable to decreased mean pore size in conjunction with a slightly increased surface contact angle facilitated by crosslinking of PVA molecules by both borate ions and ACDA.
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Date: August 2004
Creator: Brown, Robert W.

Supercritical CO2 foamed biodegradable polymer blends of polycaprolactone and Mater-Bi.

Description: Supercritical CO2 foam processing of biopolymers represents a green processing route to environmentally friendly media and packaging foams. Mater-Bi, a multiconstituent biopolymer of polyester, starch and vegetable oils has shown much promise for biodegradation. The polymer, however, is not foamable with CO2 so blended with another polymer which is. Polycaprolactone is a biopolymer with potential of 4000% change in volume with CO2. Thus we investigate blends of Mater-Bi (MB) and polycaprolactone (PCL) foamed in supercritical CO2 using the batch process. Characterization of the foamed and unfoamed samples were done using X-ray diffraction (XRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Micrographs of the samples from the SEM revealed that the cell size of the foams reduced and increased with increase in MB concentration and increase in the foaming temperature respectively. Mechanical tests; tensile, compression, shear and impact were performed on the foamed samples. It was noted that between the 20-25% wt. MB, there was an improvement in the mechanical properties. This suggests that at these compositions, there is a high interaction between PCL and MB at the molecular level compared to other compositions. The results indicate that green processing of polymer blends is viable.
Date: December 2007
Creator: Ogunsona, Emmanuel Olusegun

Micro and nano composites composed of a polymer matrix and a metal disperse phase.

Description: Low density polyethylene (LDPE) and Hytrel (a thermoplastic elastomer) were used as polymeric matrices in polymer + metal composites. The concentration of micrometric (Al, Ag and Ni) as well as nanometric particles (Al and Ag) was varied from 0 to 10 %. Composites were prepared by blending followed by injection molding. The resulting samples were analyzed by scanning electron microscopy (SEM) and focused ion beam (FIB) in order to determine their microstructure. Certain mechanical properties of the composites were also determined. Static and dynamic friction was measured. The scratch resistance of the specimens was determined. A study of the wear mechanisms in the samples was performed. The Al micro- and nanoparticles as well as Ni microparticles are well dispersed throughout the material while Ag micro and nanoparticles tend to form agglomerates. Generally the presence of microcomposites affects negatively the mechanical properties. For the nanoparticles, composites with a higher elastic modulus than that of the neat materials are achievable. For both micro- and nanocomposites it is feasible to lower the friction values with respective to the neat polymers. The addition of metal particles to polymers also improves the scratch resistance of the composites, particularly so for microcomposites. The inclusion of Ag and Ni particles causes an increase in the wear loss volume while Al can reduce the wear for both polymeric matrices.
Date: December 2007
Creator: Olea Mejia, Oscar Fernando

Trapping of hydrogen in Hf-based high κ dielectric thin films for advanced CMOS applications.

Description: In recent years, advanced high κ gate dielectrics are under serious consideration to replace SiO2 and SiON in semiconductor industry. Hafnium-based dielectrics such as hafnium oxides, oxynitrides and Hf-based silicates/nitrided silicates are emerging as some of the most promising alternatives to SiO2/SiON gate dielectrics in complementary metal oxide semiconductor (CMOS) devices. Extensive efforts have been taken to understand the effects of hydrogen impurities in semiconductors and its behavior such as incorporation, diffusion, trapping and release with the aim of controlling and using it to optimize the performance of electronic device structures. In this dissertation, a systematic study of hydrogen trapping and the role of carbon impurities in various alternate gate dielectric candidates, HfO2/Si, HfxSi1-xO2/Si, HfON/Si and HfON(C)/Si is presented. It has been shown that processing of high κ dielectrics may lead to some crystallization issues. Rutherford backscattering spectroscopy (RBS) for measuring oxygen deficiencies, elastic recoil detection analysis (ERDA) for quantifying hydrogen and nuclear reaction analysis (NRA) for quantifying carbon, X-ray diffraction (XRD) for measuring degree of crystallinity and X-ray photoelectron spectroscopy (XPS) were used to characterize these thin dielectric materials. ERDA data are used to characterize the evolution of hydrogen during annealing in hydrogen ambient in combination with preprocessing in oxygen and nitrogen.
Date: December 2007
Creator: Ukirde, Vaishali

Stimuli-responsive microgels for self-assembled crystalline structures and controlled drug release.

Description: Tissue response to PNIPAM and HPC nanoparticles has been studied by implantation method. The results suggest that both PNIAPM and HPC nanoparticles possess good biocompatibility and they may serve as a good carrier for the applications of controlled delivery. Rheological properties of dispersions of IPN microgels composed of PNIPAM and PAAc have been studied. It is found that the IPN microgel dispersion can undergo a sol-gel transition at temperature above 33°C. In vivo drug release experiments suggest that the gelation procedure creates a diffusion barrier and thus leads to slow release. An emulsion method has been used to grow columnar crystals by mixing PNIPAM microgel dispersions with organic solvents. Effect of both temperature and microgel concentration on formation of columnar crystals has been studied. PNIPAM-co-NMA microgels have been used for the fabrication of crystalline hydrogel films by self-crosslinking microgels. The hydrogel film exhibits an iridescent. The thermally responsive properties and mechanical properties of this film have been studied. Melting temperature (Tm) of colloidal crystals self-assembled with PNIPAM-co-AAc microgels has been investigated as a function of pH, salt concentration and microgel concentration. It is revealed that Tm increases as pH value increases; Tm decreases with increase of salt concentration; Tm increases as microgel concentration increases. Phase behavior of PNIPAM-co-HEAc microgel dispersions has been investigated. It is observed that these microgel dispersions exhibit liquid, crystal, and glass phase. As microgel size increases, crystal phase shifts to low concentration range. As temperature increases, crystal phase shifts to high concentration ranges. These colloidal crystals can be stabilized by NaOH-induced gelation. Effect of NaOH concentration on formation of physical gelation has been investigated.
Date: August 2009
Creator: Zhou, Jun

Maleic anhydride grafted polypropylene coatings on steel: Adhesion and wear.

Description: Polymeric coatings are being used in a growing number of applications, contributing to protection against weather conditions and localized corrosion, reducing the friction and erosion wear on the substrate. In this study, various polypropylene (PP) coatings were applied onto steel substrates by compression molding. Chemical modification of PP has been performed to increase its adhesion to metallic surfaces by grafting of maleic anhydride (MAH) onto PP in the presence of dicumyl peroxide (DCP). Influence of different concentrations of MAH and DCP on the properties of resulting materials have been examined. The coated steel samples are characterized by scanning electron microscopy (SEM), shear adhesion testing, FTIR and tribometry. The coatings with 3 wt. % MAH have shown the maximum adhesion strength due to maximum amount of grafting. The wear rates increased with increasing the amount of MAH due to simultaneous increase in un-reacted MAH.
Date: May 2010
Creator: Mahendrakar, Sridhar