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Abstract This research is focused on the condensation and phase transformation of NiO-TiO2, Co1-XO-NiO, and Co1-XO-MgO solid solution via dynamic laser ablation condensation and high temperature annealing. TiO2 rutile nanospheres with enhanced solid solution of NiO were synthesized via very energetic pulse laser ablation on clamped Ni/Ti target in oxygen for a very rapid heating/cooling, and hence pressure effect. Upon electron irradiation, the NiO-dissolved rutile (r) were partially transformed into 2(01 ) commensurate superstructure and Ni2(1+x)Ti1-xO4 spinel (s) following the crystallographic relationship [111]r//[012]s; (10 )r//(200)s. Alternatively, random NiTiO3 nanodomains were formed from amorphous regions in such a rapid decomposition process. In addition, the dense fluorite-type (f) derived TiO2 condensates dissolved up to 5 at% Ni2+ of the cations were synthesized via the same route. The nanocondensates less than 20 nm in size are nearly cubo-octahedral in shape and tended to transform martensitically to monoclinic (m) baddeleyite-type following the crystallographic relationship (100)f//(110)m; [001]f//[001]m. The condensates twice larger in size, with considerable matrix constraint, are nearly spherical in shape and consist of mosaic m-twin variants following complicated crystallographic relationships with each other and with the relic f-phase: (010)f//( 20)m; [001]f//[001]m. The charge and volume compensating oxygen vacancies due to NiO dissolution in the dense TiO2 condensates could facilitate the relaxation and amorphization process. Further more, pulse laser irradiation of Ni, Co, and Co-Ni (or Ni-Co) targets in an oxygen background gas produced nanocondensates with rock-salt type structure. Analytical electron microscopic observations indicated that such nanocrystals are cubic in shape for NiO and cubo-octahedral for Co1-xO and Ni1-xCoxO. The nanocrystals coalesced predominantly with {100} or {111} facets to form nano chain aggregates or closer packed manner. The Co1-xO was more or less oxidized as Co3-

The diffusional transformation kinetics of C-Mn steels during continuous cooling have been measured and predicted in this study for predicting the non-isothermal multi-stage cooling transformation kinetics. A suitable thermodynamic model is assessed for determining the driving force of austenite to ferrite transformation and the austenite/ferrite interface concentrations under various equilibrium constraints, which are essential to determine the diffusion-controlled transformation kinetics. The continuous cooling transformation (CCT) curves of C-Mn steels are determined using dilatometric method. Pham¡¦s empirical growth model is found most suitable for describing the start and finish transformation curve. The Avrami equation, common-used for isothermal transformation, is found to be applicable to the continuous cooling transformation. The Avrami exponents, nF and nP, for ferrite- and pearlite- dominant CCT, respectively, are close to the isothermal ones reported in the literature. The Avrami constant, b, increases with decreasing austenitizing temperature, indicating a fast progress of transformation. Combining Pham¡¦s empirical growth model with Avrami equation, the CCT kinetics of C-Mn steels can be predicated well. The examination on the microstructural evolution during CCT suggests that the transformation of austenite to grain boundary allotriomorphs of ferrite (GBAF) can be divided into (1) nucleation and growth (NG) stage, (2) growth only (site saturation, SS) stage, and (3) coalescence stage. In the NG stage, the oblate ellipsoid aspect ratio of GBAF remains 3:1 until all the nucleation sites are exhausted., i.e. the onset of SS stage, then gradually decreases in the SS stage. Once the aspect ratio approaches unity, the coalescence starts to operate. Based on this observation, a physical base model is developed for predicting the austenite to GBAF CCT. This model possesses the capability to predict the start and finish transformation temperatures, the fraction transformed, and the final ferrite grain size. Although such model failed to predict the whole range of CCT curve due to the fact that only the GBAF transformation is included at present stage, it is still highly recommended for microstructural control. In order to completely predict the whole CCT curves, a semi-empirical physical base model is adopted. In addition, the methodology to predict multi-stage cooling transformation from CCT curves is also derived based on additivity rule and the concept of ideal TTT diagram. Associated with the additivity rule and the concept of ideal TTT diagram, such empirical model is validated to be applicable for the prediction of CCT and step wise cooling transformation. The latent heat is calculated using thermodynamic software for the accurate control of cooling history of the medium carbon steels which usually releases an abundance of latent heat. Associated with the semi-empirical transformation model, the calculation of latent heat is integrated into a heat transfer model and successfully implemented in a mill operation.

Metastable b-Ti alloys are titanium alloys with sufficient b stabilizer alloying additions such that it's possible to retain single b phase at room temperature. These alloys are of great advantage compared to a/b alloys since they are easily cold rolled, strip produced and can attain excellent mechanical properties upon age hardening. Beta 21S, a relatively new b titanium alloy in addition to these general advantages is known to possess excellent oxidation and corrosion resistance at elevated temperatures. A homogeneous distribution of fine sized a precipitates in the parent b matrix is known to provide good combination of strength, ductility and fracture toughness. The current work focuses on a study of different mechanisms to engineer homogeneously distributed fine sized a precipitates in the b matrix. The precipitation of metastable phases upon low temperature aging and their influence on a precipitation is studied in detail. The precipitation sequence on direct aging above the w solvus temperature is also assessed. The structural and compositional evolution of precipitate phase is determined using multiple characterization tools. The possibility of occurrence of other non-classical precipitation mechanisms that do not require heterogeneous nucleation sites are also analyzed. Lastly, the influence of interstitial element, oxygen on a precipitation during the oxidation of Beta 21S has been determined. The ingress of oxygen and its influence on microstructure have also been correlated to measured mechanical properties.

Hot-pressed BaTiO3 ceramics are prepared from commercial nano-size powder supplied by Cabot. Samples have been thoroughly analysed for the crystalline phases, microstructure, including stacking faults and dislocations, by X-ray diffractometry, scanning electron microscopy, and transmission electron microscopy. This research consists of three major endeavours: (a) the analysis of stacking faults, (b) the hexagonal

The use of plasma sprayed ceramic coats as thermal barrier coatings (TBCs) for the protection of metallic structures and equipment from severe thermal, abrasive and corrosive conditions has been documented extensively in the last two decades. The state-of-the-art TBCs consist of a double layer coat. a top ceramic layer and an intermediate bond coat (MCrAIY, M=Ni, Co, Fe) deposited on the alloy substrate. Zirconia, both stabilized and partially stabilized with different oxides has been used as the ceramic top coat due to its low thermal conductivity and low thermal expansion coefficient. Studies of the microstructure of the TBCs have shown aspects that can help the understanding of the properties of the coating. The ternary system ZrOz-Y203-TiCz is believed to offer improved properties when it is compared to Zr02-Y203. However, the use of &02-Y203-Ti02 as TBCs, a major part of this work, is not widely reported in the literature. The purpose of this thesis was to study the microstructure of a plasma sprayed ZrOrY203-TiO2 TBC using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), and Transmission Electron Microscopy (TEM). The evolution of the Zr41_phase distribution in the ceramic coat was followed by XRD after different heat treatments, with the finding that the cooling rate plays a decisive role in the final Zr42 phase composition. SEM studies allowed a description of the lamellae structure of the Zr02-Y203-TiOz coating. The evolution of the morphology, porosity and crack distribution in the coat after different thermal treatments were followed by SEM. Evidence of incipient sintering is observed in Zr02-Y203-Ti02 coats heated at temperatures higher than 1200 °C. This should lead to poor coating performance. EDS analysis revealed an heterogeneous distribution of titanium through the oating. A detailed microstructural characterization of the as-sprayed coating was done using TEM. Microstructural features such as micro-twins, antiphase-boundaries and mottled morphology associated with "non-transformable" tetragonal ZrO2 phase were identified. It is believed that these microstructural elements promote toughening and thermal stress relief mechanisms that provide the coating with the erosion and thermal shock resistance required for a TBC. The presence of TiO2 is linked to a higher proportion of tetragonal ZrO2 in the Zr02-Y203-Ti02 coating, therefore improved properties of the coating are expected. The addition of TiO2 promotes grain growth and decreases the final density in pressed and sintered Zr02-Y203-TiO2 powders. The results obtained are a contribution to the understanding of the microstructure of TBCs and to the sparse knowledge base of the ZrOrY2O3-TiO2 coatings. Further work should be done in the characterization of the ZrO2-Y2O3-Ti42 coatings and the study of its stability under different conditions in order to determine the real potential of this material offers as an alternative to the better known ZrOrY203 TBC.

Survey work has resolved certain reported anomalies in this system. In particular, TiNi was found to undergo two displacive phase transformations at temperatures near room temperature. Below 50°C the pseudo body-centered cubic compound undergoes a gradual distortion in an unusual second order phase transformation producing the "transition phase”, the existence of which is terminated by a typical martensitic burst transfor­mation at 20°C which produces the "martensitic phase". The crystal structures of the parent phase and transformation products, and the trans­formation characteristics have been studied with X-ray and electron diffrac­tion, electron microscopy, electrical resistance and density measurements. / Thesis / Master of Science (MS)

The aim of this study is to investigate the effects of coformers and polymers on the phase transformation and release profiles of cocrystals. Pharmaceutical cocrystals of Carbamazepine (CBZ) (namely 1:1 carbamazepine-nicotinamide (CBZ-NIC), 1:1 carbamazepine-saccharin (CBZ-SAC) and 1:1 carbamazepine-cinnamic acid (CBZ-CIN) cocrystals, were synthesized. A Quality by Design (QbD) approach was used to construct the formulation. Dissolution and solubility were studied using UV imaging and High Performance Liquid Chromatography (HPLC). The polymorphic transitions of cocrystals and crystalline properties were examined using Differential Scanning Calorimetry (DSC), X-Ray Powder Diffraction (XRPD), Raman spectroscopy (Raman) and Scanning Electron Microscopy (SEM). JMP 11 software was used to design the formulation. It has been found that Hydroxupropyl methylcellulose (HPMC) cannot inhibit the transformation of CBZ-NIC cocrystals to Carbamazepine Dihydrate (CBZ DH) in solution or in the gel layer of the matrix, as opposed to its ability to inhibit CBZ Form III (CBZ III) phase transition to CBZ DH. The selection of different coformers of SAC and CIN can affect the stability of CBZ in solution, resulting in significant differences in the apparent solubility of CBZ. The dissolution advantage of the CBZ-SAC cocrystal can only be shown for 20 minutes during dissolution because of the conversion to its dihydrate form (CBZ DH). In contrast, the improved CBZ dissolution rate of the CBZ-CIN cocrystal can be realised in both solution and formulation because of its stability. The polymer of Hypromellose Acetate Succinate (HPMCAS) seemed to best augment the extent of CBZ-SAC and CBZ-CIN cocrystal supersaturation in solution. At 2 mg/ml of HPMCAS concentration, the apparent CBZ solubility of CBZ-SAC and CBZ-CIN cocrystals can increase the solubility of CBZ III in pH 6.8 phosphate buffer solutions (PBS) by 3.0 and 2.7 times respectively. All pre-dissolved polymers in pH 6.8 PBS can increase the dissolution rates of CBZ cocrystals. In the presence of a 2 mg/ml HPMCAS in pH 6.8 PBS, the cocrystals of CBZ-NIC and CBZ-CIN can dissolve by about 80% within five minutes in comparison with 10% of CBZ III in the same dissolution period. Finally, CBZ-NIC cocrystal formulation was designed using the QbD principle. The potential risk factors were determined by fish-bone risk assessment in the initial design, after which Box-Behnken design was used to optimize and evaluate the main interaction effects on formulation quality. The results indicate that in the Design Space (DS), CBZ sustained release tablets meeting the required Quality Target Product Profile (QTPP) were produced. The tablets’ dissolution performance could also be predicted using the established mathematical model.

Wang, Xiaohui. / "November 1999." / Thesis (Ph.D.)--Chinese University of Hong Kong, 1999. / Includes bibliographical references. / Electronic reproduction. Hong Kong : Chinese University of Hong Kong, [2012] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Mode of access: World Wide Web. / Abstracts in English and Chinese.