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 Department: Department of Materials Science and Engineering
 Collection: UNT Theses and Dissertations
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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Micro and nano composites composed of a polymer matrix and a metal disperse phase.

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

Date: December 2007
Creator: Olea Mejia, Oscar Fernando
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 ...
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Supercritical CO2 foamed biodegradable polymer blends of polycaprolactone and Mater-Bi.

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

Date: December 2007
Creator: Ogunsona, Emmanuel Olusegun
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.
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Trapping of hydrogen in Hf-based high κ dielectric thin films for advanced CMOS applications.

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

Date: December 2007
Creator: Ukirde, Vaishali
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 ...
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Advanced Technology for Source Drain Resistance Reduction in Nanoscale FinFETs

Advanced Technology for Source Drain Resistance Reduction in Nanoscale FinFETs

Date: May 2008
Creator: Smith, Casey Eben
Description: Dual gate MOSFET structures such as FinFETs are widely regarded as the most promising option for continued scaling of silicon based transistors after 2010. This work examines key process modules that enable reduction of both device area and fin width beyond requirements for the 16nm node. Because aggressively scaled FinFET structures suffer significantly degraded device performance due to large source/drain series resistance (RS/D), several methods to mitigate RS/D such as maximizing contact area, silicide engineering, and epitaxially raised S/D have been evaluated.
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Modifications of epoxy resins for improved mechanical and tribological performances and their effects on curing kinetics.

Modifications of epoxy resins for improved mechanical and tribological performances and their effects on curing kinetics.

Date: May 2008
Creator: Chonkaew, Wunpen
Description: A commercial epoxy, diglycidyl ether of bisphenol-A, was modified by two different routes. One was the addition of silica to produce epoxy composites. Three different silane coupling agents, glycidyloxypropyl trimethoxy silane (GPS), -methacryloxypropyl trimethoxy silane (MAMS) and 3-mercaptopropyltriethoxy silane (MPS), were used as silica-surface modifiers. The effects of silica content, together with the effects of chemical surface treatment of silica, were studied. The results indicate that epoxy composites with silica exhibit mechanical and tribological properties as well as curing kinetics different than the pure epoxy. The optimum silica content for improved mechanical and tribological properties (low friction coefficient and wear rate) was different for each type of silane coupling agent. An unequivocal correlation between good mechanical and improved tribological properties was not found. Activation energy of overall reactions was affected by the addition of silica modified with MAMS and MPS, but not with GPS. The second route was modification by fluorination. A new fluoro-epoxy oligomer was synthesized and incorporated into a commercial epoxy by a conventional blending method. The oligomer functioned as a catalyst in the curing of epoxy and polyamine. Thermal stability of the blends decreased slightly at a high oligomer content. Higher wear resistance, lower friction coefficient and ...
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Orientation, Microstructure and Pile-Up Effects on Nanoindentation Measurements of FCC and BCC Metals

Orientation, Microstructure and Pile-Up Effects on Nanoindentation Measurements of FCC and BCC Metals

Date: May 2008
Creator: Srivastava, Ashish Kumar
Description: This study deals with crystal orientation effect along with the effects of microstructure on the pile-ups which affect the nanoindentation measurements. Two metal classes, face centered cubic (FCC) and body centered cubic (BCC, are dealt with in the present study. The objective of this study was to find out the degree of inaccuracy induced in nanoindentation measurements by the inherent pile-ups and sink-ins. Also, it was the intention to find out how the formation of pile-ups is dependant upon the crystal structure and orientation of the plane of indentation. Nanoindentation, Nanovision, scanning electron microscopy, electron dispersive spectroscopy and electron backscattered diffraction techniques were used to determine the sample composition and crystal orientation. Surface topographical features like indentation pile-ups and sink-ins were measured and the effect of crystal orientation on them was studied. The results show that pile-up formation is not a random phenomenon, but is quite characteristic of the material. It depends on the type of stress imposed by a specific indenter, the depth of penetration, the microstructure and orientation of the plane of indentation. Pile-ups are formed along specific directions on a plane and this formation as well as the pile-up height and the contact radii with the indenter ...
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