In this study we contribute towards establishing the process-microstructure relationships in thin films grown off-normally by ionized physical vapor deposition. High power impulse magnetron sputtering (HiPIMS) is used at various peak target powers and deposition rates to grow copper (Cu) and chromium (Cr) films from a cathode placed at an angle 90 degrees with respect to the substrate normal. Films are also deposited by direct current magnetron sputtering (DCMS), for reference. Scanning electron microscopy is employed to investigate column tilting and deposition rate while X-ray diffraction techniques are utilized to study crystal structure and grain tilting. It is demonstrated that the columnar structure of Cu tilts less with respect to the substrate normal as the peak target power increases, which has been shown to correspond to a higher ionization degree of the sputtered material [1]. One explanation for this is that the trajectories of the ions are deflected towards the substrate and therefore deposited closer to the normal, as has been suggested in the literature (see e.g. [2]). Energetic bombardment by ions might also increase surface mobility, which further raises the columns. It is also concluded that the change in tilting is not caused by a lower deposition rate obtained when employing HiPIMS. The same is not seen for Cr, where all deposited films exhibit the same tilting angle. When the column tilting of Cu and Cr is compared a large difference is observed, where the columns of Cr are closer to the substrate normal. The reasons for this difference are discussed in light of nucleation and growth characteristics in the two materials. X-ray diffraction analysis reveals that Cu films exhibit an (111) fiber texture. Comparison of films grown by DCMS and HiPIMS shows that in the HiPIMS cases the grains are closer to the surface normal and better oriented with each other. In the case of Cr both DCMS and HiPIMS grown films are (110) biaxially aligned.

In this study, samples of nanoscale structures of nickel (Ni) nanorods were prepared using the glancing angle deposition (GLAD) technique. Annealing was done using a split- top tube furnace at high vacuum chamber pressure. The pre-melting of the nanorods was maintained at 500 °C for 30 minutes in all the samples. Using the samples with 90 minutes of GLAD time, the annealing behavior of the nanorods was studied at 300 °C, 400 °C, 500 °C and 600 °C. The nanorods were then imaged using scanning electron microscopy. Using X-ray diffraction, the crystalline microstructures of the nanorods were studied. It was found that with increasing annealing temperatures, the intensity of peaks for both Ni (111) and Ni (200) increased, which indicates that better crystals were formed. The results indicate that re-crystallization occurs after annealing, leading to the formation of larger grain sizes compared to as-deposited grain sizes. Annealing substantially changed the structure of the nanorods, leading to different smoother, more connected crystal structures for the annealed nanorods compared to as-deposited ones.

Advanced optical technologies profoundly impact countless aspects of modern life. At the heart of these technologies is the manipulation of light using optical materials. Currently, optical technologies are created using naturally occurring materials. However, a new and exciting approach is to use nanomaterials for technology development. Nanomaterials are artificially constructed material systems with precisely engineered nanostructures. Many technological revolutions await the development of new nanoscale fabrication methods that must provide the ability to control, enhance, and engineer the optical properties of these artificial constructs. This thesis responds to the challenges of nanofabrication by examining glancing angle deposition (GLAD) and improving its optical-nanomaterial fabrication capabilities. GLAD is a bottom-up nanotechnology fabrication method, recognized for its flexibility and precision. The GLAD technique provides the ability to controllably fabricate high-surface-area porous materials, to create structurally induced optical-anisotropy in isotropic materials, and to tailor the refractive index of a single material. These three advantages allow GLAD to assemble optical nanomaterials into a range of complex one-dimensional photonic crystals (PCs). This thesis improves upon previous GLAD optical results in a number of important areas. Multiple optical measurement and modeling techniques were developed for GLAD-fabricated TiO2 nanomaterials. The successful characterization of these nanomaterials was extended to engineer PC structures with great precision and a superior degree of control. The high surface area of basic PC structures was exploited to fabricate an optimized colourimetric sensor with excellent performance. This colourimetric sensor required no power source and no read-out system other than the human eye, making it a highly attractive sensing approach. Incorporating engineered defects into GLAD-fabricated PCs established a new level of design sophistication. Several PC defect structures were examined in detail, including spacing layers and index profile phase-shifts. Remarkable control over defect properties was achieved and intriguing polarization-sensitive optical effects were investigated in anisotropic defect layers. The success of these results demonstrates the precision and flexibilty of the GLAD technique in fabricating optical nanomaterials and advanced photonic devices. / Micro-Electro-Mechanical Systems (MEMS) and Nanosystems

The glancing angle deposition (GLAD) technique is now used by over one hundred research groups, each requiring a fundamental understanding of and new techniques for modulating the properties of GLAD in order to optimize their results. In this thesis, the structural characteristics of nanostructured columnar films were therefore investigated and quantified using gas adsorption porosimetry, focused ion beam tomography, optical methods, scanning electron microscopy (SEM) image analysis. Questions such as ``What is their surface area?'', ``How porous are they?'', ``How do the films evolve as they grow?'', and ``Can the structural characteristics be manipulated?'' were answered. Surface areas, determined from krypton gas adsorption, were found to be high, making GLAD promising for applications requiring large and rough surface interfaces. Specifically, peak specific surface areas of 700 +/- 150 m^2g^{-1}, 325 +/- 40 m^2g^{-1}, 50 +/- 6 m^2g^{-1} were measured for silica (SiO_2), titania (TiO_2) and indium tin oxide (ITO), respectively. Broad pore distributions, with peaks in the low mesoporous regime of 2 nm to 5 nm, were also determined. The internal surface area may also be up to three times as high as that of the externally exposed surface. As well, despite the fact that GLAD column broaden as they grow, the surface area increases linearly with film thickness. Focused ion beam milling, with concurrent SEM imaging, was then employed to investigate and reconstruct the three-dimensional structure of GLAD films in the tens of nanometers regime not measurable by krypton gas adsorption porosimetry. The measured growth scaling trends agreed with previous findings, but were determined using only one sample, instead of multiple samples of increasing thickness. Mean column diameters, center-to-center spacings, void spacings, and column densities were found to scale with thickness as w = (9.4 +/- 3.0) t^{0.35 +/- 0.09} nm, c = (24.8 +/- 5.2) t^{0.31 +/- 0.08} nm, v = (15.2 +/- 3.8) t^{0.25 +/- 0.06} nm, and d = (3400 +/- 2500) t^{-0.65 +/- 0.15} columns um^{-2}, respectively. Finally, spatially graded nanostructures were demonstrated by extending the GLAD technique to include macroscopic shadowing. Optically transparent, graded thickness and pitch helical films were fabricated with polarization selectivity over a spatial range of 30 mm, concurrent with 70 nm spectral tunability. These structures will be useful for tunable frequency photonic devices. / Micro-Electrical-Mechanical Systems (MEMS) and Nanosystems

This thesis investigates technologies directed towards developing photonic crystal display devices. A switching technology based on dye electrophoretic motion within a 1D porous photonic crystal was developed. Dissociated absorbing dye species were moved through the assembled device and reflectance was controllably altered by up to 0.4. Refinement of fabrication techniques yielded a slow switching device, whose time-resolved reflectance data was analyzed. A wavelength dependence of the device switching speed was observed. This phenomenon was described by modelling where bandgap effects match observation. These devices may be improved by employing a 3D photonic crystal. We developed a nanoimprint lithography technique for seeding films deposited by GLAD for the fabrication of 3D square spiral photonic crystals. Parameters for patterning a precisely defined mould pattern using electron beam lithography were established. A large area diamond:1 square spiral photonic crystal was fabricated on the nanoimprinted seeds, and it exhibited a visible wavelength bandgap. / Micro-Electro-Mechanical Systems (MEMS) and Nanosystems

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