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  Partner: UNT Libraries
 Department: Department of Materials Science and Engineering
 Degree Level: Doctoral
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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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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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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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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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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