Ngai Hau Wai. / Thesis (M.Phil.)--Chinese University of Hong Kong, 1998. / Includes bibliographical references. / Text in English; abstract also in Chinese. / Ngai Hau Wai. / Acknowledgements --- p.ii / Abstract --- p.iii / Chapter Chapter 1: --- Introduction --- p.1 / Chapter 1.1 --- History of nanomaterials --- p.1 / Chapter 1.2 --- Application and properties of nanomaterials --- p.2 / Chapter 1.3 --- Thermodynamic of a binary system --- p.4 / Chapter 1.4 --- Nucleation and growth --- p.5 / Chapter 1.5 --- Spinodal decomposition --- p.7 / References --- p.10 / Figures --- p.11 / Chapter Chapter 2: --- Experimental setup and techniques --- p.21 / Chapter 2.1 --- How to achieve high undercooling? --- p.21 / Chapter 2.2 --- Preliminary steps --- p.22 / Chapter 2.2.1 --- Preparation of dehydrated B203 --- p.22 / Chapter 2.2.2 --- Preparation of the apparatus --- p.23 / Chapter 2.2.3 --- Preparation of Ni2P --- p.23 / Chapter 2.2.4 --- Alloying --- p.23 / Chapter 2.3 --- Experiment --- p.24 / Chapter 2.3.1 --- Preparation of pure glass --- p.24 / Chapter 2.3.2 --- Anneal the glass pieces at different temperature for 30 minutes… --- p.24 / Chapter 2.4 --- Investigation --- p.25 / Chapter 2.4.1 --- Thermal Properties --- p.25 / Chapter 2.4.2 --- TEM observation --- p.25 / References --- p.27 / Figures --- p.28 / Chapter Chapter 3: --- Crystallization kinetics of amorphous nanostructured materials --- p.32 / Abstract --- p.32 / Chapter 3.1 --- Introduction --- p.33 / Chapter 3.2 --- Experimental --- p.34 / Chapter 3.3 --- Results and Discussion --- p.35 / References --- p.41 / Figures --- p.42

by Leung Ching Chuen. / Thesis (M.Phil.)--Chinese University of Hong Kong, 1998. / Includes bibliographical references (leaf 47). / Text in English; abstract also in Chinese. / by Leung Ching Chuen. / Acknowledgments --- p.ii / Abstract --- p.iii / Chapter Chapter 1 --- Introduction --- p.1 / Chapter 1.1 --- Expansion of the Mesoscopic World --- p.2 / Chapter 1.2 --- Nanostructured Materials --- p.3 / Chapter 1.3 --- A New Age --- p.4 / Chapter 1.4 --- """Flaws"" of the New Age" --- p.5 / Chapter 1.5 --- Phase Transformation --- p.7 / Chapter 1.6 --- Nucleation and Growth --- p.8 / Chapter 1.7 --- Spinodal Decomposition --- p.11 / Chapter 1.8 --- Morphology Change during Spinodal Decomposition --- p.13 / References --- p.16 / Figures --- p.17 / Chapter Chapter 2 --- Experiment --- p.25 / Chapter 2.1 --- Experimental Preparations --- p.27 / Chapter 2.1.1 --- Fused Silica Tube Preparation --- p.27 / Chapter 2.1.2 --- Alloying --- p.27 / Chapter 2.2 --- Experimental Procedures --- p.28 / Chapter 2.2.1 --- Fluxing --- p.28 / Chapter 2.2.2 --- Undercooling --- p.29 / Chapter 2.3 --- Sample Analysis --- p.30 / Chapter 2.3.1 --- Surface Analysis --- p.30 / Chapter 2.3.2 --- Differential Scanning Calorimetry (DSC) --- p.30 / Chapter 2.3.3 --- Hardness Testing --- p.31 / Chapter 2.3.4 --- Optical Microscopy --- p.32 / Chapter 2.3.5 --- Scanning Electron Microscopy (SEM) --- p.32 / Chapter 2.3.6 --- Transmission Electron Microscopy (TEM) --- p.32 / Chapter 2.3.7 --- X-ray Powder Diffraction (XPD) --- p.33 / References --- p.34 / Figures --- p.35 / Chapter Chapter 3 --- Mechanism of Bulk Nanostructured Material Formation by Metastable Liquid State Spinodal Decomposition --- p.38 / Abstract --- p.39 / References --- p.47 / Figures --- p.48 / Chapter Chapter 4 --- Formation of Amorphous Nanostructured Material --- p.57 / Abstract --- p.58 / References --- p.66 / Figures --- p.67 / Chapter Chapter 5 --- Crystallization Kinetics of Amorphoous Nanostructured Alloy --- p.75 / Abstract --- p.76 / References --- p.85 / Figures --- p.86 / Chapter Chapter 6 --- Conclusion --- p.101

The amorphous state is becoming increasingly important in the pharmaceutical setting. Formulation of poorly water soluble drugs in the amorphous form enhances physicochemical properties of the drug, such as solubility and dissolution rate, which in turn may lead to an increased bioavailability. However, despite these advantages, many properties of the amorphous state are not yet understood and amorphous materials pose a challenge for structural analysis since they lack three dimensional long range order. Hence, compared to crystalline materials often little structural information can be gained using standard characterisation techniques. In this thesis, a range of analytical techniques and data analysis tools were used to characterise as well as quantify amorphous drugs and compare them to their crystalline counterparts. Apart from established characterisation techniques such as X-ray powder diffraction, microscopy, and differential scanning calorimetry, molecular-level characterisation was carried out using vibrational spectroscopies including infrared, near infrared, and Raman spectroscopy combined with multivariate analysis methods. To obtain deeper understanding of the structure of amorphous drugs and their corresponding crystalline forms novel approaches such as pair distribution function analysis of X-ray diffraction data and computational chemistry were employed. Three model drugs namely indomethacin, saquinavir, and fenofibrate were investigated in the scope of this thesis. For indomethacin differences between amorphous forms of indomethacin prepared by ball milling, spray drying, as well as melting and subsequent cooling were analysed using infrared, near infrared, and Raman spectroscopy in combination with principal component analysis. While all spectroscopic techniques were able to differentiate between the differently prepared samples, Raman spectroscopy proved to be most sensitive to small differences in the solid state of different samples. Consistent with the study of indomethacin, Raman spectroscopy combined with principal component analysis was the most sensitive analytical technique to detect structural changes induced by milling or heating saquinavir. In addition, pair distribution function transforms of the X-ray powder diffraction data significantly contributed to the understanding of differences in short-range and long-range order between differently treated saquinavir samples. A combination of vibrational spectroscopy, quantum mechanical calculations, and multivariate analysis proved suitable for physicochemical analysis of amorphous fenofibrate. The results of the study support the idea that non hydrogen bonded molecules such as fenofibrate are likely to exhibit random molecular orientations and conformations in the amorphous phase since the weak intermolecular interactions that occur between such molecules can easily be disrupted. A study of ternary mixtures of crystalline and amorphous forms of indomethacin showed that Raman and near-infrared spectroscopy in conjunction with PLS regression are well suited for quantification of the different solid-state forms simultaneously. It was found that near-infrared spectroscopy can be used to more accurately quantify the mixtures compared to Raman spectroscopy when fluorescing components, such as amorphous indomethacin, are present. Nevertheless quantification with Raman spectroscopy was still possible. Overall, the analytical methods used in this thesis were successfully employed for qualitative and quantitative analysis of amorphous drugs and their crystalline counterparts. It could be shown that it is beneficial to use a combination of different analytical techniques and data analysis tools since results are complementary and allow a more comprehensive description of the solid state.

Thesis (Ph. D.)--University of Texas at Austin, 2003. / Vita. Includes bibliographical references. Available also from UMI Company.

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Thesis (M.Sc.)--City University of Hong Kong, 2005. / At head of title: City University of Hong Kong, Department of Physics and Materials Science, Master of Science in materials engineering & nanotechnology dissertation. Title from title screen (viewed on Sept. 1, 2006) Includes bibliographical references.

Thesis (Ph. D.)--University of Texas at Austin, 2006. / Vita. Includes bibliographical references.

Thesis (Ph. D.)--Rutgers University, 2008. / "Graduate Program in Food Science." Includes bibliographical references.

Thesis--M. Phil., University of Hong Kong.