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The application of gold and silver nanoparticles to areas such as medical research is based on unique optical properties exhibited by some metals. These properties are a direct consequence of localised excitations occurring at visible frequencies known as Surface Plasmon Resonances (SPRs). The exact frequency of an SPR induced in a nanoparticle can be 'tuned' in the optical range by, for example, changing the size of gold and silver nanoparticles, or by varying the relative concentrations of gold and silver within an alloy nanoparticle. Whatever the desired frequency, it is critical that the majority of nanoparticles exhibit the frequency within the resolution limit of the imaging system. The research presented here utilises the high resolution imaging and spectroscopy techniques of (Scanning) Transmission Electron Microscopy ((S)TEM) and Electron Energy Loss Spectroscopy (EELS). It is common practice to analyse the optical properties of alloy nanoparticles using techniques that acquire a single spectrum averaged over multiple particles such as Ultraviolet-Visible (UV-Vis) spectroscopy. However, this technique cannot detect any optical variation between the nanoparticles resulting from compositional change. In this research the author demonstrates through the use of EELS that the SPR can be determined for individual gold/silver alloy nanoparticles, for the purpose of determining the extent of their homogeneity. Importantly, the data presented here suggest dramatic variation in SPR frequency between particles and even within the same particle, indicative of large variations in alloy composition. This puts the assumption that alloying can be scaled down to the nanometre-scale to the test. In order to resolve and extract the SPR in both the pure gold and gold and silver alloy nanoparticles, the author has successfully applied multiple post acquisition techniques such as Richardson-Lucy deconvolution and Principle Component Analysis (PCA) to the EELS Spectrum Imaging (SI) acquisition method. Additionally, the valence band EELS data are supported by complementary electron microscopy techniques; Core loss EELS, Energy Dispersive X-Ray Spectroscopy (EDX) and High Angle Annular Dark Field (HAADF) imaging.

Structural material fatigue is a leading cause of failure and has motivated fatigue-resistant design to eliminate risks to human lives. Intrinsic microstructural features alter fatigue deformation mechanisms so profoundly that, essentially, fatigue properties of structural materials become deviant. With this in mind, we initiated this project to investigate the microstructural effect on fatigue behavior of potential structural high entropy alloys. With a better understanding of the effect of microstructure features on fatigue properties, the ultimate goal was to engineer the microstructure to enhance the fatigue life of structural materials. The effects of two major deformation mechanisms presented here are twinning-induced fatigue crack retardation, and transformation-induced fatigue crack retardation. The fundamental principle of both mechanisms is to delay the fatigue crack propagation rate by altering the work hardening ability locally within the crack plastic zone. In ultrafine grained triplex Al0.3CoCrFeNi, nano-sized deformation twins were observed during cyclic loading in FCC matrix due to low stacking fault energy (SFE). The work-hardening ability of the material near the crack was sustained with the formation of twins according to Considere's criteria. Further, due to the ultrafine-grained (UFG) nature of the material, fatigue runout stress was enhanced. In a coarse-grained, dual-phase high entropy alloy, persistent slip bands formed in FCC matrix during cyclic loading due mainly to the slight composition change that affects the SFE in the FCC matrix and eventually alters the deformation mechanism. Another way known to alter an alloy's work hardening (WH) ability is transformation-induced plasticity (TRIP). In some alloys, phase transformation happens due to strain localization, which alters the work-hardening ability. iii In a fine-grained, dual-phase metastable high entropy alloy, gamma (f.c.c.) to epsilon (h.c.p.) transformation occurred in the plastic zone that was induced from cracks. Thus, we designed a Cu-containing FeMnCoCrSi high entropy alloy that exhibited a normalized fatigue ratio of ~ 0.62 UTS (ultimate tensile strength). Our design approach was based on (a) engineering the gamma phase stability to attain sustained work hardening through delayed gamma (f.c.c.) to epsilon (h.c.p.) transformation to hinder fatigue crack propagation, (b) incorporating an ultrafine-grained microstructure to delay crack initiation, and (c) forming deformation twins to reduce the crack propagation rate. We verified that a UFG gamma dominant microstructure could provide opportunities for exceptional fatigue resistance, as sustained WH activity strengthened the material locally in the crack plastic zone, thereby validating our expectation that the combination of UFG and TRIP is a path to design the next generation of fatigue-resistant alloys.

Shear spinning of Haynes 282, Alloy 718, Alloy 600 and AISI 316L was done using several tool feeds and mandrel clearances. Multi passing of the materials was limited due to strain hardening and circumferential cracking except for AISI 316L. The effect of the tool feed and the mandrel clearance on the successful forming of the materials was established. The successfully spun samples were solution heat treated at varying temperatures and holding times to establish a range of grain sizes and hardness levels. An aging heat treatment process was performed for Haynes 282 and Alloy 718 to achieve precipitation strengthening. The micro hardness measurements were conducted for the materials prior to spinning and after spinning. The same was also done after the various heat treatment processes. Grain size mapping was conducted by the use of lineal intercept methods. Comparison of the results in terms of grain sizes and hardness values was done. The temperature ranges suitable for full recrystallization of the materials after the shear spinning were identified and the effect of the holding times on the grain growth established. Comparison with unspun samples showed that the heat treatment times required to achieve comparative hardness and grain sizes were distinctively different.

<p>Aluminum-Silicon (Al-Si) alloys are often preferred in the die casting industry due to excellent castability, high strength, corrosion resistance and low cost. Commonly, iron (Fe) is alloyed with the alloys to prevent die soldering. However, the addition of Fe in most of Al-Si alloys leads to formation of the intermetallic β-AlFeSi. The β-AlFeSi is harmful to the alloy structural integrity due to its needle-like morphology that creates stress concentration at the microscopic level. The phase presence is unfavorable to the mechanical properties and significantly reduces the elongation of the alloys. This research attempted to find viable way to control the morphology and formation of the β-AlFeSi phase.</p> <p>Thermodynamic simulations were done to investigate the sequence of intermetallic formation and other phases at different alloy compositions. The analysis of solidification paths of different alloys provided the correlation between the phase formation sequence and the fraction of the β-AlFeSi phase. The analysis also identified the feasible region of alloy design for minimizing the β-AlFeSi formation. Based on the thermodynamics simulation analysis, five alloys of different compositions were designed to validate the finding of the simulation. </p> <p>The tensile test results of the alloys indicated that lowering the Fe content increases the elongation of the alloy. The results also showed that elongation was reduced with the increase of Si level due to the formation of eutectic Silicon. The change of both Fe and Mn did not significantly affect the mechanical property of the alloy when the ratio of Fe to Mn was constant. Microscopic analysis showed that lowering the Fe level had effectively altered the morphology of the β-AlFeSi needle like structure. The β-AlFeSi was found to be smaller in terms of size when Fe is lower, subsequently reducing the probability of β-AlFeSi phase to be stress riser and crack initiation. </p> <p>The influence of heat treatment to the mechanical property of the alloys was also studied. The mechanical result on the heat-treated samples indicated that heat treatment is a viable method to improve the elongation property of the alloy. Microscopic observations showed that the β-AlFeSi phase was broken into shorter structures over the solution heat treatment process, resulting in better elongation. </p>

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