>Magister Scientiae - MSc / In this thesis we report on the deposition of silicon nanostructures using a 3-zone thermal chemical vapour deposition process at atmospheric pressure. Nickel and gold thin films, deposited by DC sputtering on crystalline silicon substrates, were used as the catalyst material required for vapour-solid-liquid growth mechanism of the Si nanostructures. The core of this work is centred around the effect of catalyst type, substrate temperature and the source-to-substrate distance on the structural and optical properties of the resultant Si nanostructures, using argon as the carrier gas and Si powder as the source. The morphology and internal structure of the Si nanostructures was probed by using high resolution scanning and transmission electron microscopy, respectively. The crystallinity was measured by x-ray diffraction and the high resolution transmission electron microscopy. For composition and elemental analysis, Fourier transform infrared spectroscopy was used to quantify the bonding configuration, while electron energy-loss spectroscopy in conjunction with electron dispersion spectroscopy reveals the composition. Photoluminescence and UV-visible spectroscopy was used to extract the emission and reflection properties of the synthesized nanostructures.