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>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.

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This dissertation summarises the study of different aspects of the aerosol-assisted chemical vapour deposition (AACVD) technique for the production of multi-wall carbon nanotubes (MWCNTs). Upscaling the synthesis while retaining the quality of MWCNTs has been a prime objective throughout the work. A key aspect of this work was the study of different growth parameters and their influence on the homogeneity of the products across the reactor. The effect of the precursor composition on the yield and quality of MWCNTs were also investigated. It was shown that the synthesis rate can be significantly (60 – 80 %) increased by tuning the composition of the precursor. Moreover, by optimising the synthesis recipe and using a larger reactor, the synthesis rate and efficiency of the precursor were increased fivefold (up to 14 g/hr) and twice (up to 88 %) respectively. Large area (up to 90 cm²), mm-thick carpets of MWCNTs which were both free-standing and on substrate were produced. The carpets could withstand normal handlings without tearing apart, making them suitable for macroscopic characterisations and applications. By in-situ qualitative and quantitative gas analysis of the atmosphere of the reactor, the thermocatalytic cracking behaviour of 25 precursors was investigated and a mechanism for successive formation of different hydrocarbon fragments inside the reactor was proposed. A number of dedicated gas analysis methods and apparatuses such as a probe for zone-by-zone gas analysis of reactor and a heated chamber for preparation of standard gas analysis samples were developed to explore some of the least investigated aspects of the thermocatalytic cracking of precursors. Mapping the reactor revealed that some single-wall and double-wall carbon nanotubes (SWCNTs and DWCNTs) were also produced near the exhaust of the reactor. The SWCNTs were partly covered by fullerene-like species and resembled different forms of carbon nanobuds. In addition, the effect of the electron beam on the interaction of the SWCNTs and the fullerene-like species was studied in situ using high-resolution transmission electron microscopy (HRTEM).

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The morphology evolution of high-temperature grown AlN nucleation layers on (111) silicon has been studied using atomic force microscopy (AFM). The structure and morphology of subsequently grown GaN film were characterized by optical microscopy, scanning electron microscopy, x-ray diffraction, and photoluminescence measurement. It was found that a thicker AlN buffer layer resulted in a higher crystalline quality of subsequently grown GaN films. The GaN with a thicker buffer layer has a narrower PL peak. Cracks were found in the GaN film which might be due to the formation of amorphous SiNx at the AlN and Si interface. / Singapore-MIT Alliance (SMA)

AlN nucleation layers are being investigated for growth of GaN on Si. The microstructures of high-temperature AlN nucleation layers grown by MOCVD on Si (111) substrates with trimethylaluminium pre-treatments have been studied using atomic force microscopy (AFM) and transmission electron microscopy (TEM). The AFM results show that with TMA pre-treatments, AlN grows in a pseudo-2-dimensional mode because the lateral growth rate of AlN is increased, and the wetting property of the AlN on silicon is improved. Also, no amorphous SiNx layer was observed at the interface with TMA pre-treatments and AlN films with good epitaxial crystalline quality were obtained. Transmission electron diffraction patterns revealed that the AlN and Si have the crystallographic orientation relationship AlN [0001]║Si[111] and AlN[11 2 0] ║Si[110]. High resolution transmission electron microscopy indicates a 5:4 lattice matching relationship for AlN and Si along the Si [110] direction. Based on this observation, a lattice matching model is proposed. / Singapore-MIT Alliance (SMA)

The periodic silane burst technique was employed during metalorganic chemical vapor deposition of epitaxial GaN on AlN buffer layers grown on Si (111). Periodic silicon delta doping during growth of both the AlN and GaN layers led to growth of GaN films with decreased tensile stresses and decreased threading dislocation densities, as well as films with improved quality as indicated by x-ray diffraction, micro-Raman spectroscopy, atomic force microscopy, and transmission electron microscopy. The possible mechanism of the reduction of tensile stress and the dislocation density is discussed in the paper. / Singapore-MIT Alliance (SMA)

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