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  Partner: UNT Libraries
 Department: Department of Materials Science and Engineering
 Decade: 2000-2009
 Collection: UNT Theses and Dissertations
Characterization of Cure Kinetics and Physical Properties of a High Performance, Glass Fiber-Reinforced Epoxy Prepreg and a Novel Fluorine-Modified, Amine-Cured Commercial Epoxy.

Characterization of Cure Kinetics and Physical Properties of a High Performance, Glass Fiber-Reinforced Epoxy Prepreg and a Novel Fluorine-Modified, Amine-Cured Commercial Epoxy.

Date: December 2003
Creator: Bilyeu, Bryan
Description: Kinetic equation parameters for the curing reaction of a commercial glass fiber reinforced high performance epoxy prepreg composed of the tetrafunctional epoxy tetraglycidyl 4,4-diaminodiphenyl methane (TGDDM), the tetrafunctional amine curing agent 4,4'-diaminodiphenylsulfone (DDS) and an ionic initiator/accelerator, are determined by various thermal analysis techniques and the results compared. The reaction is monitored by heat generated determined by differential scanning calorimetry (DSC) and by high speed DSC when the reaction rate is high. The changes in physical properties indicating increasing conversion are followed by shifts in glass transition temperature determined by DSC, temperature-modulated DSC (TMDSC), step scan DSC and high speed DSC, thermomechanical (TMA) and dynamic mechanical (DMA) analysis and thermally stimulated depolarization (TSD). Changes in viscosity, also indicative of degree of conversion, are monitored by DMA. Thermal stability as a function of degree of cure is monitored by thermogravimetric analysis (TGA). The parameters of the general kinetic equations, including activation energy and rate constant, are explained and used to compare results of various techniques. The utilities of the kinetic descriptions are demonstrated in the construction of a useful time-temperature-transformation (TTT) diagram and a continuous heating transformation (CHT) diagram for rapid determination of processing parameters in the processing of prepregs. Shrinkage ...
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Electrochemical synthesis of CeO2 and CeO2/montmorillonite nanocomposites.

Electrochemical synthesis of CeO2 and CeO2/montmorillonite nanocomposites.

Date: December 2003
Creator: Wang, Qi
Description: Nanocrystalline cerium oxide thin films on metal and semiconductor substrates have been fabricated with a novel electrodeposition approach - anodic oxidation. X-ray diffraction analysis indicated that as-produced cerium oxide films are characteristic face-centered cubic fluorite structure with 5 ~ 20 nm crystal sizes. X-ray photoelectron spectroscopy study probes the non-stoichiometry property of as-produced films. Raman spectroscopy and Scanning Electron Microscopy have been applied to analyze the films as well. Deposition mode, current density, reaction temperature and pH have also been investigated and the deposition condition has been optimized for preferred oriented film formation: galvanostatic deposition with current density of -0.06 mA/cm2, T > 50oC and 7 < pH < 10. Generally, potentiostatic deposition results in random structured cerium oxide films. Sintering of potentiostatic deposited cerium oxide films leads to crystal growth and reach nearly full density at 1100oC. It is demonstrated that in-air heating favors the 1:2 stoichiometry of CeO2. Nanocrystalline cerium oxide powders (4 ~ 10 nm) have been produced with anodic electrochemical synthesis. X-ray diffraction and Raman spectroscopy were employed to investigate lattice expansion phenomenon related to the nanoscale cerium oxide particles. The pH of reaction solution plays an important role in electrochemical synthesis of cerium oxide films ...
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Hydrophobic, fluorinated silica xerogel for low-k applications.

Hydrophobic, fluorinated silica xerogel for low-k applications.

Date: May 2004
Creator: Zhang, Zhengping
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. ...
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Study of Conductance Quantization by Cross-Wire Junction

Study of Conductance Quantization by Cross-Wire Junction

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Date: May 2004
Creator: Zheng, Tao
Description: The thesis studied quantized conductance in nanocontacts formed between two thin gold wires with one of the wires coated by alkainthiol self assembly monolayers (SAM), by using the cross-wire junction. Using the Lorenz force as the driving force, we can bring the two wires in contact in a controlled manner. We observed conductance with steps of 2e2 / h. The conductance plateaus last several seconds. The stability of the junction is attributed to the fact that the coating of SAM improves the stability and capability of the formed contact.
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Determination of Wear in Polymers Using Multiple Scratch Test.

Determination of Wear in Polymers Using Multiple Scratch Test.

Date: August 2004
Creator: Damarla, Gowrisankar
Description: Wear is an important phenomenon that occurs in all the polymer applications in one form or the other. However, important links between materials properties and wear remain illusive. Thus optimization of material properties requires proper understanding of polymer properties. Studies to date have typically lacked systematic approach to all polymers and wear test developed are specific to some polymer classes. In this thesis, different classes of polymers are selected and an attempt is made to use multiple scratch test to define wear and to create a universal test procedure that can be employed to most of the polymers. In each of the materials studied, the scratch penetration depth s reaches a constant value after certain number of scratches depending upon the polymer and its properties. Variations in test parameters like load and speed are also studied in detail to understand the behavior of polymers and under different conditions. Apart from polystyrene, all the other polymers studied under multiple scratch test reached asymptotes at different scratch numbers.
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Development of a Novel Grease Resistant Functional Coatings for Paper-based Packaging and Assessment of Application by Flexographic Press

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

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Date: August 2004
Creator: Brown, Robert W.
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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Investigation of growth kinetics of self-assembling monolayers by means of contact angle, optical ellipsometry, angle-resolved XPS and IR spectroscopy.

Investigation of growth kinetics of self-assembling monolayers by means of contact angle, optical ellipsometry, angle-resolved XPS and IR spectroscopy.

Date: August 2004
Creator: Jakubowicz, Agnieszka
Description: Absorption of octadecanethiol and p-nitrobenzenethiol onto gold surfaces from ethanol solutions has been studied by means of contact angle, optical ellipsometry, angle-resolved XPS (ARXPS), and with grazing angle total reflection FTIR. Growth of the monolayers from dilute solutions has been monitored and Langmuir isotherm adsorption curves were fitted to experimental data. A saturated film is formed within approximately 5h after immersion in solutions of concentrations ranging from 0.0005mM to 0.01mM. We found, that the final density of monolayer depends on the concentration of the solution.
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Barrier and Long Term Creep Properties of Polymer Nanocomposites.

Barrier and Long Term Creep Properties of Polymer Nanocomposites.

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Date: December 2004
Creator: Ranade, Ajit
Description: The barrier properties and long term strength retention of polymers are of significant importance in a number of applications. Enhanced lifetime food packaging, substrates for OLED based flexible displays and long duration scientific balloons are among them. Higher material requirements in these applications drive the need for an accurate measurement system. Therefore, a new system was engineered with enhanced sensitivity and accuracy. Permeability of polymers is affected by permeant solubility and diffusion. One effort to decrease diffusion rates is via increasing the transport path length. We explore this through dispersion of layered silicates into polymers. Layered silicates with effective aspect ratio of 1000:1 have shown promise in improving the barrier and mechanical properties of polymers. The surface of these inorganic silicates was modified with surfactants to improve the interaction with organic polymers. The micro and nanoscale dispersion of the layered silicates was probed using optical and transmission microscopy as well as x-ray diffraction. Thermal transitions were analyzed using differential scanning calorimetry. Mechanical and permeability measurements were correlated to the dispersion and increased density. The essential structure-property relationships were established by comparing semicrystalline and amorphous polymers. Semicrystalline polymers selected were nylon-6 and polyethylene terephthalate. The amorphous polymer was polyethylene terphthalate-glycol. Densification ...
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Synthesis and characterization of crystalline assembly of poly Nisopropylacry-lamide)-co-acrylic acid nanoparticles.

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

Date: December 2004
Creator: Zhou, Bo
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 ...
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Charge Interaction Effects in Epoxy with Cation Exchanged Montmorillonite Clay and Carbon Nanotubes.

Charge Interaction Effects in Epoxy with Cation Exchanged Montmorillonite Clay and Carbon Nanotubes.

Date: May 2005
Creator: Butzloff, Peter Robert
Description: The influence of charge heterogeneity in nanoparticles such as montmorillonite layered silicates (MLS) and hybrid systems of MLS + carbon nanotubes was investigated in cured and uncured epoxy. Epoxy nanocomposites made with cation-exchanged montmorillonite clay were found to form agglomerates near a critical concentration. Using differential scanning calorimetry it was determined that the mixing temperature of the epoxy + MLS mixture prior to the addition of the curing agent critically influenced the formation of the agglomerate. Cured epoxy samples showed evidence of the agglomerate being residual charge driven by maxima and minima in the concentration profiles of thermal conductivity and dielectric permittivity respectively. A hybrid nanocomposite of MLS and aniline functionalized multi walled nanotubes indicated no agglomerates. The influence of environmentally and process driven properties on the nanocomposites was investigated by examination of moisture, ultrasound, microwaves and mechanical fatigue on the properties of the hybrid systems. The results point to the importance of charge screening by adsorbed or reacted water and on nanoparticulates.
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Functionalization and characterization of porous low-κ dielectrics.

Functionalization and characterization of porous low-κ dielectrics.

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Date: May 2005
Creator: Orozco-Teran, Rosa Amelia
Description: The incorporation of fluorine into SiO2 has been shown to reduce the dielectric constant of the existing materials by reducing the electrical polarizability. However, the incorporation of fluorine has also been shown to decrease film stability. Therefore, new efforts have been made to find different ways to further decrease the relative dielectric constant value of the existing low-k materials. One way to reduce the dielectric constant is by decreasing its density. This reduces the amount of polarizable materials. A good approach is increasing porosity of the film. Recently, fluorinated silica xerogel films have been identified as potential candidates for applications such as interlayer dielectric materials in CMOS technology. In addition to their low dielectric constants, these films present properties such as low refractive indices, low thermal conductivities, and high surface areas. Another approach to lower k is incorporating lighter atoms such as hydrogen or carbon. Silsesquioxane based materials are among them. 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 triethoxyfluorosilane-based (TEFS) xerogel films when reacted with silylation agents. TEFS films were employed because they form robust silica ...
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A magnetorheological study of single-walled and multi-walled carbon nanotube dispersions in mineral oil and epoxy resin.

A magnetorheological study of single-walled and multi-walled carbon nanotube dispersions in mineral oil and epoxy resin.

Date: May 2005
Creator: Yang, Zhengtao
Description: Single wall carbon nanotubes (SWNTs) and multi-walled carbon nanotubes (MWNTs) were dispersed in mineral oil and epoxy resin. The magnetorheological properties of these dispersions were studied using a parallel plate rheometer. Strain sweeps, frequency sweeps, magneto sweeps and steady shear tests were conducted in various magnetic fields. G', G", h* and ty increased with increasing magnetic field, which was partially attributed to the increasing degree of the alignment of nanotubes in a stronger magnetic field. The SWNT/mo dispersions exhibited more pronounced magnetic field dependence than SWNT/ep and MWNT/mo counterparts due to their much lower viscosity. The alignment of SWNTs in mineral oil increased with rising nanotube concentration up to 2.5vol% but were significantly restricted at 6.41vol% due to nanotube flocculation.
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Saturation and foaming of thermoplastic nanocomposites using supercritical CO2.

Saturation and foaming of thermoplastic nanocomposites using supercritical CO2.

Date: May 2005
Creator: Strauss, William C.
Description: Polystyrene (PS) nanocomposite foams were prepared using supercritical fluid (SCF) CO2 as a solvent and blowing agent. PS was first in-situ polymerized with a range of concentrations of montmorillonite layered silicate (MLS). The polymerized samples were then compression molded into 1 to 2mm thick laminates. The laminates were foamed in a batch supercritical CO2 process at various temperatures and pressures from 60°-85°C and 7.6-12MPa. The resulting foams were analyzed by scanning electron microscopy to determine effect of MLS on cellular morphology. Differential scanning calorimetry was used to determine the impact of nanocomposite microstructure on glass transition of the foamed polymer. X-ray diffraction spectra suggested that the PS/MLS composite had an intercalated structure at both the 1% and 3% mixtures, and that the intercalation may be enhanced by the foaming process.
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Morphological properties of poly (ethylene terephthalate) (PET) nanocomposites in relation to fracture toughness.

Morphological properties of poly (ethylene terephthalate) (PET) nanocomposites in relation to fracture toughness.

Date: August 2005
Creator: Pendse, Siddhi
Description: The effect of incorporation of montmorillonite layered silicate (MLS) on poly (ethylene terephthalate) (PET) matrix was investigated. MLS was added in varying concentration of 1 to 5 weight percent in the PET matrix. DSC and polarized optical microscopy were used to determine the crystallization effects of MLS addition. Non isothermal crystallization kinetics showed that the melting temperature and crystallization temperature decrease as the MLS percent increases. This delayed crystallization along with the irregular spherulitic shape indicates hindered crystallization in the presence of MLS platelets. The influence of this morphology was related with the fracture toughness of PET nanocomposites using essential work of fracture coupled with the infra red (IR) thermography. Both the essential as well as non essential work of fracture decreased on addition of MLS with nanocomposite showing reduced toughness.
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Indentation induced deformation in metallic materials.

Indentation induced deformation in metallic materials.

Date: December 2005
Creator: Vadlakonda, Suman
Description: Nanoindentation has brought in many features of research over the past decade. This novel technique is capable of producing insights into the small ranges of deformation. This special point has brought a lot of focus in understanding the deformation behavior under the indenter. Nickel, iron, tungsten and copper-niobium alloy system were considered for a surface deformation study. All the samples exhibited a spectrum of residual deformation. The change in behavior with indentation and the materials responses to deformation at low and high loads is addressed in this study. A study on indenter geometry, which has a huge influence on the contact area and subsequently the hardness and modulus value, has been attempted. Deformation mechanisms that govern the plastic flow in materials at low loads of indentation and their sensitivity to the rate of strain imparted has been studied. A transition to elastic, plastic kind of a tendency to an elasto-plastic tendency was seen with an increase in the strain rate. All samples exhibited the same kind of behavior and a special focus is drawn in comparing the FCC nickel with BCC tungsten and iron where the persistence of the elastic, plastic response was addressed. However there is no absolute reason ...
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Synthesis and Characterization of Crystalline Assemblies of Functionalized Hydrogel Nanoparticles

Synthesis and Characterization of Crystalline Assemblies of Functionalized Hydrogel Nanoparticles

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Date: December 2005
Creator: Cai, Tong
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 ...
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Supercritical Silylation and Stability of Silyl Groups

Supercritical Silylation and Stability of Silyl Groups

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Date: May 2006
Creator: Nerusu, Pawan Kumar
Description: Methylsilsesquioxane (MSQ) and organosilicate glass (OSG) are the materials under this study because they exhibit the dielectric constant values necessary for future IC technology requirements. Obtaining a low-k dielectric value is critical for the IC industry in order to cope time delay and cross talking issues. These materials exhibit attractive dielectric value, but there are problems replacing conventional SiO2, because of their chemical, mechanical and electrical instability after plasma processing. Several techniques have been suggested to mitigate process damage but supercritical silylation offers a rapid single repair step solution to this problem. Different ash and etch damaged samples were employed in this study to optimize an effective method to repair the low-k dielectric material and seal the surface pores via supercritical fluid processing with various trialkylchlorosilanes. Fourier transform infrared spectroscopy (FTIR), contact angle, capacitance- voltage measurements, and x-ray photoemission spectroscopy, dynamic secondary ion mass spectroscopy (DSIMS), characterized the films. The hydrophobicity and dielectric constant after exposure to elevated temperatures and ambient conditions were monitored and shown to be stable. The samples were treated with a series of silylating agents of the form R3-Si-Cl where R is an alkyl groups (e.g. ethyl, propyl, isopropyl). Reactivity with the surface hydroxyls was inversely ...
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Evaluation of hydrogen trapping in HfO2 high-κ dielectric thin films.

Evaluation of hydrogen trapping in HfO2 high-κ dielectric thin films.

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Date: August 2006
Creator: Ukirde, Vaishali
Description: Hafnium based high-κ dielectrics are considered potential candidates to replace SiO2 or SiON as the gate dielectric in complementary metal oxide semiconductor (CMOS) devices. Hydrogen is one of the most significant elements in semiconductor technology because of its pervasiveness in various deposition and optimization processes of electronic structures. Therefore, it is important to understand the properties and behavior of hydrogen in semiconductors with the final aim of controlling and using hydrogen to improve electronic performance of electronic structures. Trap transformations under annealing treatments in hydrogen ambient normally involve passivation of traps at thermal SiO2/Si interfaces by hydrogen. High-κ dielectric films are believed to exhibit significantly higher charge trapping affinity than SiO2. In this thesis, study of hydrogen trapping in alternate gate dielectric candidates such as HfO2 during annealing in hydrogen ambient is presented. Rutherford backscattering spectroscopy (RBS), elastic recoil detection analysis (ERDA) and nuclear reaction analysis (NRA) were used to characterize these thin dielectric materials. It was demonstrated that hydrogen trapping in bulk HfO2 is significantly reduced for pre-oxidized HfO2 prior to forming gas anneals. This strong dependence on oxygen pre-processing is believed to be due to oxygen vacancies/deficiencies and hydrogen-carbon impurity complexes that originate from organic precursors used in ...
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Low Temperature Polymeric Precursor Derived Zinc Oxide Thin Films

Low Temperature Polymeric Precursor Derived Zinc Oxide Thin Films

Date: December 2006
Creator: Choppali, Uma
Description: Zinc oxide (ZnO) is a versatile environmentally benign II-VI direct wide band gap semiconductor with several technologically plausible applications such as transparent conducting oxide in flat panel and flexible displays. Hence, ZnO thin films have to be processed below the glass transition temperatures of polymeric substrates used in flexible displays. ZnO thin films were synthesized via aqueous polymeric precursor process by different metallic salt routes using ethylene glycol, glycerol, citric acid, and ethylene diamine tetraacetic acid (EDTA) as chelating agents. ZnO thin films, derived from ethylene glycol based polymeric precursor, exhibit flower-like morphology whereas thin films derived of other precursors illustrate crack free nanocrystalline films. ZnO thin films on sapphire substrates show an increase in preferential orientation along the (002) plane with increase in annealing temperature. The polymeric precursors have also been used in fabricating maskless patterned ZnO thin films in a single step using the commercial Maskless Mesoscale Materials Deposition system.
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Study of lead sorption on magnetite at high temperatures.

Study of lead sorption on magnetite at high temperatures.

Date: December 2006
Creator: Paliwal, Vaishali
Description: Lead's uptake on magnetite has been quantitatively evaluated in the present study at a temperature of 200°C and pH of 8.5 with lead concentrations ranging from 5 ppm to175 ppm by equilibrium adsorption isotherms. The pH independent sorption behavior suggested lead sorption due to pH independent permanent charge through weak electrostatic, non-specific attraction where cations are sorbed on the cation exchange sites. The permanent negative charge could be a consequence of lead substitution which is supported by increase in the lattice parameter values from the X-ray diffraction (XRD) results. Differential scanning calorimetry (DSC/TGA) results showed an increase of exothermic (magnetite to maghemite transformation) peak indicating substitution of lead ions due to which there is retardation in the phase transformation. Presence of outer sphere complexes and physical sorption is further supported by Fourier transformed infrared spectroscopy (FTIR). None of the results suggested chemisorption of lead on magnetite.
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Amorphization and De-vitrification in Immiscible Copper-Niobium Alloy Thin Films

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

Date: May 2007
Creator: Puthucode Balakrishnan, Anantharamakrishnan
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.
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Bulk and Interfacial Effects on Density in Polymer Nanocomposites

Bulk and Interfacial Effects on Density in Polymer Nanocomposites

Date: May 2007
Creator: Sahu, Laxmi Kumari
Description: The barrier properties of polymers are a significant factor in determining the shelf or device lifetime in polymer packaging. Nanocomposites developed from the dispersion of nanometer thick platelets into a host polymer matrix have shown much promise. The magnitude of the benefit on permeability has been different depending on the polymer investigated or the degree of dispersion of the platelet in the polymer. In this dissertation, the effect of density changes in the bulk and at the polymer-platelet interface on permeability of polymer nanocomposites is investigated. Nanocomposites of nylon, PET, and PEN were processed by extrusion. Montmorillonite layered silicate (MLS) in a range of concentrations from 1 to 5% was blended with all three resins. Dispersion of the MLS in the matrix was investigated by using one or a combination of X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Variation in bulk density via crystallization was analyzed using differential scanning calorimetry (DSC) and polarized optical microscopy. Interfacial densification was investigated using force modulation atomic force microscopy (AFM) and ellipsometry. Mechanical properties are reported. Permeability of all films was measured in an in-house built permeability measurement system. The effect of polymer orientation and induced defects on permeability ...
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Surface Engineering and Characterization of Laser Deposited Metallic Biomaterials

Surface Engineering and Characterization of Laser Deposited Metallic Biomaterials

Date: May 2007
Creator: Samuel, Sonia
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 ...
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Measurement of Lattice Strain and Relaxation Effects in Strained Silicon Using X-ray Diffraction and Convergent Beam Electron Diffraction

Measurement of Lattice Strain and Relaxation Effects in Strained Silicon Using X-ray Diffraction and Convergent Beam Electron Diffraction

Date: August 2007
Creator: Diercks, David Robert
Description: The semiconductor industry has decreased silicon-based device feature sizes dramatically over the last two decades for improved performance. However, current technology has approached the limit of achievable enhancement via this method. Therefore, other techniques, including introducing stress into the silicon structure, are being used to further advance device performance. While these methods produce successful results, there is not a proven reliable method for stress and strain measurements on the nanometer scale characteristic of these devices. The ability to correlate local strain values with processing parameters and device performance would allow for more rapid improvements and better process control. In this research, x-ray diffraction and convergent beam electron diffraction have been utilized to quantify the strain behavior of simple and complex strained silicon-based systems. While the stress relaxation caused by thinning of the strained structures to electron transparency complicates these measurements, it has been quantified and shows reasonable agreement with expected values. The relaxation values have been incorporated into the strain determination from relative shifts in the higher order Laue zone lines visible in convergent beam electron diffraction patterns. The local strain values determined using three incident electron beam directions with different degrees of tilt relative to the device structure have ...
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