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Thesis (M.Phil.)--Hong Kong University of Science and Technology, 2005. / Includes bibliographical references (leaves 58-60). Also available in electronic version.

Thesis (M.S.)--Montana State University--Bozeman, 2004. / Typescript. Chairperson, Graduate Committee: Aleksandra Vinogradov. Includes bibliographical references (leaves 83-90).

Thesis (Ph. D.)--Colorado State University, 2004. / Includes bibliographical references.

The elastic properties of a solid are of considerable interest to both science and technology. Not only do they contain fundamental information about the nature of the inter-atomic bonding in the material, but they also determine the mechanical behavior of solids. In the past few years, considerable effort has been devoted to the study of elastic properties of bulk metallic glasses (BMGs), a relatively new class of metallic materials that display a unique combination of mechanical and physical properties. Our research has focused on Zr-based, Cu-based and Ca-based metallic glasses. Zr-based BMGs are known to have superior glass forming ability and high strength, but their ductility is too low for wide-spread practical applications. Cu-based BMGs recently received wide interest because of their low cost and good mechanical properties. Ca-based BMGs have low glass transition temperature Tg, around 390 K, which make them very attractive to be studied near Tg. In this work, resonant ultrasound spectroscopy (RUS) has been applied to study the elastic properties of above mentioned BMGs from 5 K to their glass transition temperature Tg. RUS is a novel technique for determining the elastic moduli of solids, based on the measurement of the resonances of a freely vibrating body. In an RUS experiment, the mechanical resonances of a freely vibrating solid of known shape are measured, and an iteration procedure is used to “match” the measured lines with the calculated spectrum. This allows determination of all elastic constant of the solid from a single frequency scan. Below Tg, the elastic constants of the BMGs under investigation show “normal” behavior, i.e. with increasing temperature, all moduli decrease and Poisson ratio increases. Above Tg changes in the trends occur due to structural relaxation and crystallization. We confirmed the suggested link between ductility and Poisson ratio: BMGs showing good ductility display high Poisson ratio. By increasing palladium content in Zr50Cu40-xAl10Pdx alloys, BMGs with high Poisson ratio and thus good ductility have been obtained. In addition, we developed a simple model to provide fast and good estimate of the temperature dependence of elastic constants of BMGs from room temperature measurements. Keywords: Elastic properties; Bulk metallic glasses (BMGs); Resonant ultrasound spectroscopy (RUS); Internal friction.

The elastic properties of novel transition metal oxides have been investigated, using a powerful technique known as Resonant Ultrasound Spectroscopy (RUS). Two sets of transition metal oxides have been studied. One is the ruthenate Ca2-xSrxRuO4 series with a layered perovskite structure, a Mott transition system that connects the Mott insulator Ca2RuO4 with the unconventional superconductor Sr2RuO4. The other set contains geometrically frustrated materials, including vanadium spinels AV2O4 (A = Zn, Mn and Fe) and titanate pyrochlores A2Ti2O7 (A= Y, Tb, Yb, Ho and Dy). The elastic response of five Ca2-xSrxRuO4 single crystals (x = 2.0, 1.9, 0.5, 0.3 and 0.2) has been measured. For 2.0 ≥ x ≥ 0.5, a dramatic softening over a wide temperature range is observed upon cooling, caused by the rotational instability of RuO6 octahedra (for x = 2.0 and 1.9) or the static rotation of the octahedra (for x = 0.5). For the Ca-rich samples (x = 0.3 and 0.2), the softening occurs in a very narrow temperature range, corresponding to the structural phase transition from high-temperature-tetragonal to low-temperature-orthorhombic symmetry. Elastic softening in ZnV2O4 is observed near the cubic-to-tetragonal structural phase transition at 50 K. The elastic response of MnV2O4 is quite unusual, displaying a softening over a wide temperature range with decreasing temperature. Upon cooling, C’ of FeV2O4 becomes so soft that it drops to almost zero around 140 K, where the cubic-to-tetragonal structural transition occurs. For Y2Ti2O7, all three elastic constants show normal “Varshni” behavior. For spin liquid Tb2Ti2O7, all three elastic constants show a pronounced softening below 50 K, indicative of a possible Jahn-Teller, cubic-to-tetragonal transition at very low temperatures. It is also found that the application of a magnetic field suppresses the elastic softening in this compound. Another spin liquid Yb2Ti2O7 shows no elastic softening. The elastic moduli of the spin-ice compounds, Ho2Ti2O7 and Dy2Ti2O7, show a broad “dip” around 100 K, which is believed to be caused by the strong crystal field effect in those two compounds.

The work in this thesis falls roughly into three parts, which I characterise loosely as a developmental stage, an exploratory stage, and an attempt to contribute to understanding of the field. In the developmental stage, I have worked to design a variety of methods to create high-quality samples of various Iron Pnictide superconductors, to dope them with various chemicals and to characterise the resulting crystalline samples. I discuss in depth the signature of good quality crystals and the various experiments that they have been used in by myself and my collaborators. These processes are ongoing and will hopefully continue to contribute to my research group's capabilities. My exploratory work involves a detailed survey of one particular family, Sr(Fe1-xCox)2As2, as the level of Cobalt is varied, and the mapping of the phase diagram for the system. I have also made a comparison to the better-measured Barium analogue, and discuss the reasons for the differences in character between the two, most notably the lack of a splitting of the structural and magnetic transitions in the first species. I also discuss the effect of pressure, which can lead to superconductivity in lightly doped samples for very modest pressures; and annealing, which increases transition temperatures within samples, on a limited quantity of crystals. Finally, I attempt to contribute to the understanding of the field via a series of Resonant Ultrasound Spectroscopic experiments conducted by a collaborator on my crystals and analysed by me. I see distinct first-order transitions in the parent compounds, characterisable above the high-T structural transition within a Ginzburg-Landau pseudoproper ferroelastic scheme for a transition coupling weakly to strain but driven by another order parameter. My observations allow several statements about the symmetry of the order parameter and are suggestive of a non-magnetically driven structural transition. In the case of doped samples a much richer behavior is seen, with a broad transition and simultaneous relaxation of all elastic peaks and a broad temperature range of significant dispersion. The effect of the softening is seen far above TN and lends strong support to the family of models predicting such high-T fluctuations.

Residual stress measurement methods have commonly been used to characterize states of stress in various elastic isotropic materials. In order to investigate the effects of elastic anisotropy on residual stress measurements, commercially pure grade 2 titanium (CP Ti Gr 2) was selected to study a strong texture, or preferred grain orientation. Warm rolled and air-cooled CP titanium is well known to have a texture from the factory. This texture and resulting elastic anisotropy were confirmed using two material characterization methods, resonant ultrasound spectroscopy (RUS) and electron backscatter diffraction (EBSD). The texture was further developed using a rolling mill to cold roll the titanium. A vacuum furnace set to a temperature of 550 C for one hour was used to stress relieve the titanium without reducing the texture. RUS and EBSD methods were used again to confirm the texture achieved by cold rolling. Well-characterized residual stresses were introduced with a shrink-fit ring and plug. The residual stress hole drilling method was used to characterize stresses in the rolling and transverse directions of the ring and plug assemblies. Stress profiles from hole drilling indicated some possible elastic anisotropic effects in two assemblies and are presented. However, more assemblies are needed to confirm the results. A stress determination technique with higher sensitivity may be necessary to substantiate assembly stress profile results.

The preliminary goal of this study is to determine the effects of processing conditions, compositions and microstructural morphologies of the constituents on the physical and thermo-mechanical properties of alumina (Al_2O_3) reinforced aluminum (Al) composites. Composites with 0, 5, 10, 20 and 25 vol% Al_2O_3 were manufactured using powder metallurgy method. The elastic properties (Young's and shear modulus) and the coefficient of thermal expansion (CTE) of the composites were determined using Resonant Ultrasound Spectroscopy (RUS) and Thermo Mechanical Analyzer (TMA) respectively at various temperatures. Increasing compacting pressure improved relative density (or lowered porosity) of the composites. Furthermore, increasing the Al_2O_3 vol% in the composite increased the elastic moduli and reduced the CTE of the composites. Increasing the testing temperature from 25 to 450 oC, significantly reduced the elastic moduli of the composites, while the CTE of the composites changed only slightly with temperatures. Secondly, the goal of this study is to determine the effect of microstructures on the effective thermo-mechanical properties of the manufactured Al-Al_2O_3 composites using finite element (FE) method. Software OOF was used to convert the SEM micrographs of the manufactured composites to FE meshed models, which were then used to determine the effective elastic modulus and CTE. It was observed that, effective modulus dropped by 19.7% when porosity increased by 2.3%; while the effective CTE was mildly affected by the porosity. Additionally, the effect of residual stress on the effective thermo-mechanical properties was studied, and the stress free temperature of the composites was determined. Another objective of this study is to examine the stress-strain response of Al-Al_2O_3 composites due to compressive loads at various temperatures. Elastic modulus, yield stress and strain hardening parameters were determined from the stress-strain curves and their dependency on temperature, porosity and volume fraction were studied. The experimental results were compared with the numerical results. It was observed that high-localized stresses were present near the pores and at the interfaces between Al and Al_2O_3 constituents. Finally, functionally graded materials (FGMs) with varying Al_2O_3 concentration (0, 5and 10 vol%) in Al were manufactured; and their stress-strain response and CTE were determined at various temperatures.

Une meilleure compréhension des relations entre la structure complexe de l'os cortical et ses propriétés mécaniques est nécessaire à l'évaluation de la qualité osseuse. Les méthodes conventionnelles ex vivo de mesure de l'élasticité à l'échelle du millimètre ont des limitations liées à l'anisotropie du tissu, à son inhomogénéité et à la petite taille des échantillons. Au contraire, la spectroscopie par résonance ultrasonore (RUS) est bien adaptée à la mesure de petits échantillons anisotropes. Cette méthode estime l'élasticité à partir des fréquences de résonance de l'échantillon, et l'amortissement à partir de la largeur des pics de résonance. Son application à l'os était considérée difficile, du fait de l'amortissement important des modes de vibration, qui induit un recouvrement des pics de résonance et complique la mesure des fréquences. Pour surmonter cette difficulté, des adaptions de la méthode - dans la mesure, le traitement du signal et l'estimation des propriétés du matériau - ont été proposées. Elles ont été validées sur de l'os cortical et sur des échantillons de polymère et de matériau composite imitant l'os. La précision de la méthode a été démontrée, ainsi que sa capacité à mesurer tous les termes du tenseur d'élasticité à partir d'un seul échantillon. De plus, une nouvelle formulation Bayésienne de l'inversion apporte une solution automatique à un problème qui nécessitait une stratégie fastidieuse d'essai-erreur ou de complexes modifications du dispositif expérimental. Finalement, l'application à une grande collection d'échantillons de tibias humains démontre que la méthode RUS pourrait être utilisée en routine pour la mesure de la viscoélasticité de l'os. / Deep understanding of the structure-function relationships of cortical bone in the context of bone quality assessment is still missing. Currently available methods to measure millimeter-scale elasticity ex vivo have limitations arising from theanisotropy of the tissue, its heterogeneity, and the small size of the specimens.Resonant ultrasound spectroscopy is particularly suitable for the measurement of small anisotropic specimens. This method estimates elasticity from the free resonant frequencies of a specimen, and damping from the width of the resonant peaks. Its application to cortical bone was considered challenging because of the high damping of the vibrations modes, which causes overlapping of the resonant peaks and prevents a direct measurement of the resonant frequencies. To overcome the difficulty,adaptations of all the steps of RUS – measurement, signal processing and inverse estimation of the material properties – have been introduced. Validation of each step of the procedure has been achieved by application to several test samples, including a cortical bone specimen and bone-mimicking composite and polymer specimens.RUS was shown to be precise and accurate, with the advantage of providing the complete stiffness tensor from the measurement of a single specimen. Additionally, an original Bayesian formulation of the inversion provides an automated solution toa problem that was previously solved by tedious trial-and-error procedures or complex additions to the basic experimental setup. Finally, the application to a large collection of human tibiae specimens demonstrates that RUS can be considered a routine method to characterize the viscoelasticity of bone.