Aluminum and Zinc oxide powder were blended by friction stir processing (FSP) with threaded pin of 6mm in diameter under conditions of traverse speed, 1mm/sec and rotation speed, 1500rpm. Different thermal analysis (DTA) was conducted to reveal that the melting point of the stir zone decreased to 592oC from 660oC of the green compact specimen containing 20wt%ZnO. X-ray diffraction (XRD) identified that Zn from ZnO dissolved into Al matrix, and did not resolve redox products, alomina. Scanning electron microscopy (SEM) with filed emission gun was employed with EDS analysis. It is interesting to note that many redoxed products with oxygen concentration higher than that of the matrix can be seen as dark and gray phases in BSE images. Evidently, a chemical reaction in Al/ZnO system is possible during FSP and results of the reduced Zn dissolving into the Al matrix and the expected but not detectable nanoscale alumina uniformly being dispersed into the matrix can be attributed to the excellent 22% elongation, and 350 MPa tensile strength in the stir zone from stirred Al-25wt% ZnO.

<p>The purpose of this work was to design and to develop a high performance catalyst for the production of hydrogen from reforming of crude ethanol and also, to develop the kinetics and reactor model of crude ethanol reforming process. Crude ethanol reforming is an endothermic reaction of ethanol and other oxygenated hydrocarbons such as (lactic acid, glycerol and maltose) with water present in fermentation broth to produce hydrogen (H2) and carbon dioxide (CO2). Ni/Al2O3 catalysts were prepared using different preparation methods such as coprecipitation, precipitation and impregnation methods with different Ni loadings of 10 25 wt.%, 10-20 wt.%, and 10-20 wt.% respectively.</p><p>All catalysts were characterised by thermogravimetric/differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), (including X-ray line broadening), temperature programmed reduction (TPR), BET surface area measurements, pore volume and pore size distribution analysis. TG/DSC analyses for the uncalcined catalysts showed the catalyst were stable up from 600oC. XRD analyses showed the presence of NiO, NiAl2O4 and Al2O3 species on the calcined catalysts whereas Ni, NiAl2O4, and Al2O3 were present on reduced catalysts. BET surface area decreased and average pore diameter reached a maximum and then decreased as the Ni loading increased. The temperature programmed reduction profiles showed peaks corresponding to the reduction of NiO between 400-600oC and reduction of NiAl2O4 between 700-800oC. Catalyst screening was performed in a micro reactor with calcination temperature, reaction temperature and the ratio of catalyst weight to crude ethanol flow rate (W/Fcrude-C2H5OH) of 600 oC, 400oC and 0.59 h respectively. Maximum crude-ethanol conversion of 85 mol% was observed for catalyst with 15wt% Ni loading prepared by precipitation method (PT15), while maximum hydrogen yield (= 4.33 moles H2 / mol crude-ethanol feed) was observed for catalyst with 15wt% Ni loading prepared by coprecipitation (CP15). </p><p>Performance tests were carried out on (CP15) in which variables such as space velocity (WHSV) 1.68h-1to 4.68h-1, reduction temperature 400 to 600oC and reaction temperature 320 to 520 oC, were changed for optimum performance evaluation of the selected catalyst. The catalyst deactivated over first three hours of 11 hours time-on-stream (TOS) before it stabilized, the reaction conditions resulted in a drop of ethanol conversion from 80 to 70mol%.</p><p>The compounds identified in the liqiud products in all cases were ethanoic acid, butanoic acid, butanal, propanone, propanoic acid, propylene glycol and butanedioic acid. The kinetic analysis was carried out for the rate data obtained for the reforming of crude ethanol reaction that produced only hydrogen and carbon dioxide. These data were fitted to the power law model and Eldey Rideal models for the entire temperature range of 320-520 oC. The activation energy found were 4405 and 4428 kJ/kmol respectively. Also the simulation of reactor model showed that irrespective of the operating temperature, the benefit of an increase in reactor length is limited. It also showed that by neglecting the axial dispersion term in the model the crude ethanol conversion is under predicted. In addition the beneficial effects of W/FAO start to diminish as its value increases (i.e. at lower flow rates).

<p>The purpose of this work was to design and to develop a high performance catalyst for the production of hydrogen from reforming of crude ethanol and also, to develop the kinetics and reactor model of crude ethanol reforming process. Crude ethanol reforming is an endothermic reaction of ethanol and other oxygenated hydrocarbons such as (lactic acid, glycerol and maltose) with water present in fermentation broth to produce hydrogen (H2) and carbon dioxide (CO2). Ni/Al2O3 catalysts were prepared using different preparation methods such as coprecipitation, precipitation and impregnation methods with different Ni loadings of 10 25 wt.%, 10-20 wt.%, and 10-20 wt.% respectively.</p><p>All catalysts were characterised by thermogravimetric/differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), (including X-ray line broadening), temperature programmed reduction (TPR), BET surface area measurements, pore volume and pore size distribution analysis. TG/DSC analyses for the uncalcined catalysts showed the catalyst were stable up from 600oC. XRD analyses showed the presence of NiO, NiAl2O4 and Al2O3 species on the calcined catalysts whereas Ni, NiAl2O4, and Al2O3 were present on reduced catalysts. BET surface area decreased and average pore diameter reached a maximum and then decreased as the Ni loading increased. The temperature programmed reduction profiles showed peaks corresponding to the reduction of NiO between 400-600oC and reduction of NiAl2O4 between 700-800oC. Catalyst screening was performed in a micro reactor with calcination temperature, reaction temperature and the ratio of catalyst weight to crude ethanol flow rate (W/Fcrude-C2H5OH) of 600 oC, 400oC and 0.59 h respectively. Maximum crude-ethanol conversion of 85 mol% was observed for catalyst with 15wt% Ni loading prepared by precipitation method (PT15), while maximum hydrogen yield (= 4.33 moles H2 / mol crude-ethanol feed) was observed for catalyst with 15wt% Ni loading prepared by coprecipitation (CP15). </p><p>Performance tests were carried out on (CP15) in which variables such as space velocity (WHSV) 1.68h-1to 4.68h-1, reduction temperature 400 to 600oC and reaction temperature 320 to 520 oC, were changed for optimum performance evaluation of the selected catalyst. The catalyst deactivated over first three hours of 11 hours time-on-stream (TOS) before it stabilized, the reaction conditions resulted in a drop of ethanol conversion from 80 to 70mol%.</p><p>The compounds identified in the liqiud products in all cases were ethanoic acid, butanoic acid, butanal, propanone, propanoic acid, propylene glycol and butanedioic acid. The kinetic analysis was carried out for the rate data obtained for the reforming of crude ethanol reaction that produced only hydrogen and carbon dioxide. These data were fitted to the power law model and Eldey Rideal models for the entire temperature range of 320-520 oC. The activation energy found were 4405 and 4428 kJ/kmol respectively. Also the simulation of reactor model showed that irrespective of the operating temperature, the benefit of an increase in reactor length is limited. It also showed that by neglecting the axial dispersion term in the model the crude ethanol conversion is under predicted. In addition the beneficial effects of W/FAO start to diminish as its value increases (i.e. at lower flow rates).

Mono-dispersed supported Ni catalysts were synthesized using the water-CTAB-hexanol reverse micellar system. The core of the reverse micelles contained an aqueous solution of NiCl2. Dynamic light scattering measurements showed that microemulsions having a water-to-surfactant molar ratio, Wo, of 10 lead to reverse micelles with lowest polydispersity, longest stability, and size range of interest. At an oil-to-aqueous phase ratio of 2, the diameter of the reverse micelles was found to increase with Wo in a linear fashion. At higher values of Wo (i.e. 25-30), the polydispersity was found to increase when lowering the amount of surfactant in the system. Ultimately, O/A = 2 and Wo = 10 were chosen as optimal conditions for microemulsion preparation. The aqueous NiCl2 concentration within the micelles was varied between 0.1 and 0.001 M. DLS results showed that although the average micelle diameter was between 70-83 nm throughout the range of metal salt concentrations, the crystallite size estimate based upon the reported micelle diameter and known aqueous NiCl2 concentration ranged between 2 to 7 nm. Therefore, the Ni crystallite size was varied by changing the aqueous NiCl2 concentration due to instability issues arising when changing the value of Wo. After deposition onto an alumina mesh support, the particles were dried, calcined, and reduced to produce Ni clusters. SEM and EDS analysis was used to confirm the presence of Ni compounds after the calcination stage. By the varying the aqueous NiCl2 concentration within the micelles, .0039, .0013, and .00039 wt. % Ni catalysts were produced and characterized using SEM. Particles in the size range of 10-14 nm were noticed for the .0039 wt. % Ni catalysts after reduction, 7-11 nm for .0013 wt. % Ni, and 5-9 nm for .00039 wt. % Ni. The lower-end of these particle size ranges was comparable to the crystallite size estimates. Ethane hydrogenolysis and ethylene hydrogenation reactions were conducted over the emulsion-prepared catalysts in order to determine particle size effects on catalytic activity. Results showed that the catalytic activity, defined in terms of per unit metal surface atom (or TON, turnover number), decreases with increasing particle size for the hydrogenolysis reaction. This trend may be due to an intrinsic size effect in which smaller particles exhibit the chemical or structural properties necessary for achieving a higher reaction rate. The results for ethylene hydrogenation showed that the reaction rate did not significantly change with crystallite size, confirming that the reaction is facile or structure-insensitive.

Advancement in biotechnology has successfully converted the conventional bearing couples into artificial joints. Materials used today, however, have not been satisfactory. Problems such as osteolysis and aseptic loosening lead to failure of artificial joints and also the lifespan of these joints is to be further improved. This research targets two issues related to the problem: coatings and design of new generation biofluids. Superior to metals and polymers, ceramics are hard and biocompatible and exhibit low wear and friction. The ceramic-on-ceramic bearing pair could last for a long time which could be beneficial to younger and active patients who need a bearing pair which would last for more than 15 years to avoid the possibility of a revision surgery. The first part of this thesis deals with studying the microstructure-property relationship of new ceramic-based materials and coatings. Specifically, alumina (ceramic) coatings at different current intensities were tested in order to determine their feasibility as a biomaterial for artificial joints. In order to find a new avenue for developing biofluids, the second part of this thesis focuses on the failure of artificial joints under inadequate lubrication. Also due to osteoarthritis, synthetic biofluid is injected into joints to help relieve pain but it works for only 6-9 months. We propose a new method using noble gold nanoparticles to modify fluids. This was accomplished by mixing different concentration of nanoparticles with biofluid. This thesis consists of 6 sections. The first section is an introduction to tribology, biotribology and artificial joints which is followed by the second section which discusses the objectives of the research. The third section describes the materials and methods used in the research. The tribological characterization of MAO alumina coatings is discussed in the fourth section and the fifth section discusses the effect of nanoparticles on fluid lubrication. The last section is the conclusion.

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In thin film fabrication, growth of high quality thin films with reproducibile properties is one of the main challenges. In order to achieve this goal, the influnce of the deposition system control parameters on film properties must be studied. This can be a complex process since many parameters may need to be considered. In this thesis, the electron beam evaporation of thin aluminum oxide films was investigated. Films were deposited with and without oxygen supply in the chamber, and at various ebeam source settings. A Varialble Angle Spectroscopic Ellipsometry system was used to characterize the films. Refractive index, which depends on material density and stoichiometry, was used as the figure of merit. It was observed that refractive index increases with deposition rate. Refractive index also changes with oxygen pressure and upon exposure to air. Various models to explain this behaviour are proposed and discussed. / Materials Engineering

The fabrication and mechanical properties of Ti2AlC composites reinforced with the alumina oxide fibers, such as NextelTM 720 and ALBF1, were described in this thesis. Alumina fibers and Ti2AlC powders were dispersed in the water and slip cast in the molds to form green bodies. Sedimentation test were carried out to optimize pH of the slurry. It was found that suspensions prepared with PAA as a dispersant and has an excellent stability in the pH range of 4 ~ 5. Composite green bodies were densified by pressureless sintering or hot isotatic pressing (HIP) at different temperatures. The microstructure of fabricated samples was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS), and porosimetry. It was found out that HIPing at 1300 oC for 4 hrs at 100 MPa results in almost fully dense composites with majority phases being alumina fibers and Ti2AlC. However, fully dense Ti2AlC composites could not be obtained by the pressurless sintering, even at temperature as high as 1400 oC at which reaction between Ti2AlC and NextelTM 720 was observed. The double torsion (DT) tests were carried out at room temperature to measure the fracture toughness of the HIPed pure and 5vol% alumina fiber reinforced Ti2AlC. DT results showed increase in the fracture toughness of Ti2AlC reinforcing with NextelTM 720 alumina fibers. However, fracture toughness of the samples reinforced with ALBF1 was lower than that of pure Ti2AlC because of the low relative densities of those composites. SEM study of the fracture surfaces after DT tests showed that toughening mechanisms by crack bridging and fiber pull outs at the crack tip are operative in all reinforced samples. In addition, elastic moduli of HIPed Ti2AlC measured by Resonant Ultrasound Spectroscopy (RUS) do not show significant change due to reinforcement with alumina fibers, while the Vickers hardness of composites was found to be larger for Ti2AlC reinforced with NextelTM 720 and lower for the samples reinforced with ALBF1.

Nonlinearities exist in all process control systems. The use of linear control techniques is valid only in a narrow range of operation. Therefore, in this thesis, multivariable nonlinear control techniques are considered. The target process is the single effect evaporative process of the liquor burning unit in Alcoa's alumina refinery in Kwinana and the proposed triple effects unit in the Wagerup refinery. Two types of nonlinear control strategies using differential geometry were studied, namely, the input output linearization (Kravaris and Soroush, 1990) and the input state linearization (Hunt et al, 1983a). The research has successfully demonstrated the superiority and simplicity of the nonlinear controller through simulations and plant implementations. An integrated software package using MAPLE V.3 as the computing environment was developed to automate the solution algorithms and to graphically simulate the closed loop dynamics of different processes using the two nonlinear control strategies.The issue of robustness of the nonlinear controller was addressed by developing a procedure called uncertainty vector adjustment. The effectiveness of the new strategy was successfully demonstrated on the simulated liquor burning process. Furthermore, the stability of the adjustment technique was proved and its theoretical bounds were established using Lyapunov function analysis.A comparative study of geometric nonlinear filter and extended Kalman filter was conducted to reduce the requirement of full state feedback necessary for nonlinear control using either input output linearization or input state linearization. The simulation of the single effect evaporation unit of the liquor burning process showed that the geometric nonlinear filter is superior to the extended Kalman filter in terms of nonlinear tracking performances.The plant trials of the input output linearization ++ / in Alcoa's Kwinana alumina refinery demonstrated the practicability and feasibility of implementing nonlinear control in an industrial setting and also fostered a closer gap between academia and industry. The trials established guidelines for implementing a global linearizing controller on site, including conversion of the relevant constraints and the output of an industrial proportional and integral controller to the equivalent proportional and integral action required by the nonlinear controller. The results showed that the performance of the nonlinear controller was better than the current linear controller on site in terms of responsiveness and resistance to disturbances. Hence, the nonlinear control strategy enables the process to settle faster.All in all, efforts have been made in this thesis to minimise the use of abstract mathematical language and, in some cases, simplify the language so that nonlinear control theory can be understood by a wider range of audience, especially industrial practitioners. It is hoped that the insights provided in the dissertation will encourage more industrial implementations of nonlinear controllers and forge more interaction to close the widening gap between academic and industrial practice in process control.Keywords: nonlinear control, differential geometry, symbolic algebra, evaporator process, uncertainty vector adjustment, geometric nonlinear filter.