This study reports on the synthesis of N-doped carbon spheres (N-CSs) by a simple synthetic procedure. A horizontal CVD type reactor was used to synthesize N-CSs from pyridine. Depending on the dilution of the pyridine with toluene, a nitrogen content of 0.13-5 mol % was obtained. The use of a vertical CVD reactor gave N-CSs with a N-content of 0.19-3 mol % when an ammonium solution and acetylene were used as reactants. The diameters of carbon spheres were found to be in the range of 40 nm to 1000 nm for both CVD reactors. The diameter can be controlled by varying the flow rate, temperature, time, concentration and the reactor type. The samples were characterized by TEM, HRTEM, elemental analysis, Raman spectroscopy, TGA, PXRD and ESR. We have demonstrated that unsubstituted thiophene can be polymerized by Fe3+-catalyzed oxidative polymerization. The average particle size was about 50 nm, within a narrow particlesize distribution. The undoped carbon spheres (CSs) were reacted with thiophene to give polymer/carbon composites containing polythiophene and carbon nanospheres via chemical oxidative polymerization reaction. Polythiophene molecules were either chemically bonded or physically adsorbed to the surface of carbon spheres. The microstructure and properties of the two types of composites were compared. The thermogravimetric analysis data confirmed that the presence of CSs in the polymer\carbon composites is responsible for the higher thermal stability of the composite material in comparison with pristine polythiophene. The FTIR analysis showed that covalent functionalized nanocomposites exhibit a high intensity of a C-S bond This study reports on the synthesis of N-doped carbon spheres (N-CSs) by a simple synthetic procedure. A horizontal CVD type reactor was used to synthesize N-CSs from pyridine. Depending on the dilution of the pyridine with toluene, a nitrogen content of 0.13-5 mol % was obtained. The use of a vertical CVD reactor gave N-CSs with a N-content of 0.19-3 mol % when an ammonium solution and acetylene were used as reactants. The diameters of carbon spheres were found to be in the range of 40 nm to 1000 nm for both CVD reactors. The diameter can be controlled by varying the flow rate, temperature, time, concentration and the reactor type. The samples were characterized by TEM, HRTEM, elemental analysis, Raman spectroscopy, TGA, PXRD and ESR. We have demonstrated that unsubstituted thiophene can be polymerized by Fe3+-catalyzed oxidative polymerization. The average particle size was about 50 nm, within a narrow particlesize distribution. The undoped carbon spheres (CSs) were reacted with thiophene to give polymer/carbon composites containing polythiophene and carbon nanospheres via chemical oxidative polymerization reaction. Polythiophene molecules were either chemically bonded or physically adsorbed to the surface of carbon spheres. The microstructure and properties of the two types of composites were compared. The thermogravimetric analysis data confirmed that the presence of CSs in the polymer\carbon composites is responsible for the higher thermal stability of the composite material in comparison with pristine polythiophene. The FTIR analysis showed that covalent functionalized nanocomposites exhibit a high intensity of a C-S bondThis study reports on the synthesis of N-doped carbon spheres (N-CSs) by a simple synthetic procedure. A horizontal CVD type reactor was used to synthesize N-CSs from pyridine. Depending on the dilution of the pyridine with toluene, a nitrogen content of 0.13-5 mol % was obtained. The use of a vertical CVD reactor gave N-CSs with a N-content of 0.19-3 mol % when an ammonium solution and acetylene were used as reactants. The diameters of carbon spheres were found to be in the range of 40 nm to 1000 nm for both CVD reactors. The diameter can be controlled by varying the flow rate, temperature, time, concentration and the reactor type. The samples were characterized by TEM, HRTEM, elemental analysis, Raman spectroscopy, TGA, PXRD and ESR. We have demonstrated that unsubstituted thiophene can be polymerized by Fe3+-catalyzed oxidative polymerization. The average particle size was about 50 nm, within a narrow particlesize distribution. The undoped carbon spheres (CSs) were reacted with thiophene to give polymer/carbon composites containing polythiophene and carbon nanospheres via chemical oxidative polymerization reaction. Polythiophene molecules were either chemically bonded or physically adsorbed to the surface of carbon spheres. The microstructure and properties of the two types of composites were compared. The thermogravimetric analysis data confirmed that the presence of CSs in the polymer\carbon composites is responsible for the higher thermal stability of the composite material in comparison with pristine polythiophene. The FTIR analysis showed that covalent functionalized nanocomposites exhibit a high intensity of a C-S bond at 695 cm-1 , which is not observed in the noncovalent functionalized nanocomposites

<p>In this dissertation core level electron spectroscopy has been employed to study various aspects of metal oxide films grown under ultra-high vacuum conditions. </p><p>Studies on <i>in situ</i> ion insertion of lithium into thin TiO₂ systems were performed. The electronic and geometric properties are investigated in detail, along with an estimation of charge transfer from Li to Ti. </p><p>A detailed study of chemical vapour deposition of ZrO₂ on Si(100)-(2x1) was performed. ZrO₂ is found to be an insulator, i.e. its electronic levels are decoupled from the substrate and the Zr levels are best referenced to the local vacuum level. The alignment of the valence and conduction band has been determined. </p><p>Combinatorial chemical vapour deposition of TiO₂ and ZrO₂ on Si(100)-(2x1) was realized. A film with graded stoichiometry consisting of pure TiO₂ and ZrO₂ on the opposing ends and mixed composition of both oxides in the middle was obtained. A detailed study of the electronic levels revealed that ZrO₂ remains an insulator in the monolayer regime and that modification of ZrO₂ with a small amount of TiO₂ leads to a more symmetric alignment of the bands relative to Si. </p><p>The influence of a core hole on the O 1s x-ray absorption spectrum in TiO₂ and ZrO₂ is elucidated. Supported by O 1s photoemission measurements and <i>ab initio</i> calculations it is concluded that the static final state picture as well as dynamical threshold effects must be considered in order to determine the location of the conduction band minimum within the XAS framework. </p><p>Finally a Co modified Co:ZnO film was shown to display ferromagnetic properties. It could be evidenced that Co with oxygen as nearest neighbours was responsible for the magnetism and not metallic Co.</p>

For an electronic device well-designed interfaces are critical for the performance. Studies of interfaces down to an atomic level are thus highly motivated both from a fundamental and technological point of view. In this thesis, a surface science approach has been employed to study the formation of interfaces in systems relevant for transistor and solar cell applications. Surface science methodology entails ultra high vacuum environment, single crystalline surfaces, submonolayer control of deposited material, surface sensitive spectroscopy and atomic resolution microscopy. The primary experimental method for characterization is electron spectroscopy. This is a family of very powerful experimental techniques capable of giving information on the atomic level. Additionally, studies have been performed using scanning tunnelling microscopy. Combined these two methods can provide an atomic level characterisation of the geometric and electronic properties of the surface. The emphasis of this work is placed on ultra thin TiO2 and ZrO2 films grown on silicon substrates by means of ultra-high vacuum metal-organic chemical vapour deposition. ZrO2 has also been grown on SiC and FeCrAl. Deposition has been performed with different process parameters. The interface region of each film has been characterised. The band alignment, a most important issue with regard to the development of new transistor devices, for the ZrO2/Si(100) system has been explored. Decomposition pathways of the metal organic precursors have been studied in detail. Changing process parameters is shown to alter both the precursor decomposition pathway and the nature of the interface region, thus opening the possibility to tailor the material function. The titanium dioxide films grown in situ have shown to be excellent models of nanostructured electrode materials. In this spirit, interfaces of model systems for the solid-state dye-sensitized solar cell have been studied. Links between device performance and interface structure have been elucidated.

In this study SBA-15 mesoporous silica template was synthesized and used as a sacrificial template in the preparation of ordered mesoporous carbon material. A chemical vapour deposition (CVD) technique using LPG or alternatively sucrose, pyrolyzed upon a mesoporous Si matrix were used to produce nanostructured ordered mesoporous carbon (OMC) with graphitic character after removing the Si template. The sucrose method was found to be a suitable route for preparing OMC. The OMC was used as a conductive three dimensional porous support for depositing catalytic nanophase Pt metal. Deposition of Pt nanoparticles on OMC was accomplished using a CVD method with Pt(acac)2 as a precursor. The synthesized nano-composite materials were characterized by several techniques such as, HRTEM, HRSEM, EDS, XRD, BET, TGA, FT-IR and CV.

In science and technology there is a steadily increased demand of new materials and new materials production processes since they create new application areas as well as improved production technology and economy. This thesis includes development and studies of a chemical vapour deposition (CVD) process for growth of thin films of the metastable material copper nitride, Cu3N, which is a semiconductor and decomposes at around 300 oC. The combination of these properties opens for a variety of applications ranging from solar cells to sensor and information technology. The CVD process developed is based on a metal-organic compound copper hexafluoroacetylacetonate, Cu(hfac)2 , ammonia and water and was working at about 300 oC and  5 Torr. It was found that a small amount of water in the vapour increased the growth rate considerably and that the phase content, film texture, chemical composition and morphology were strongly dependent on the deposition conditions. In-situ oxygen doping during the CVD of Cu3N to an amount of 9 atomic % could also be accomplished by increasing the water concentration in the vapour. Oxygen doping increases the band gap of the material as well as the electrical resistivity and changes the stability. The crystal structure of Cu3N is very open and contains several sites which can be used for doping. Different spectroscopic techniques like X-ray photoelectron spectroscopy, Raman spectroscopy and near edge X-ray absorption fine structure spectroscopy were used to identify the oxygen doping site(s) in Cu3N. Besides the properties, the oxygen doping also affected the morphology and texture of the films. By combining thin layers of different materials several properties can be optimized at the same time. It has been demonstrated in this thesis that multilayers, composed of alternating Cu3N and Cu2O layers, i.e. a metastable and a stable material, could be grown by CVD technique. However, the stacking sequence affected the texture, morphology and chemical composition. The interfaces between the different layers were sharp and no signs of decomposition of the initially deposited metastable Cu3N layer could be detected.

In this dissertation core level electron spectroscopy has been employed to study various aspects of metal oxide films grown under ultra-high vacuum conditions. Studies on in situ ion insertion of lithium into thin TiO2 systems were performed. The electronic and geometric properties are investigated in detail, along with an estimation of charge transfer from Li to Ti. A detailed study of chemical vapour deposition of ZrO2 on Si(100)-(2x1) was performed. ZrO2 is found to be an insulator, i.e. its electronic levels are decoupled from the substrate and the Zr levels are best referenced to the local vacuum level. The alignment of the valence and conduction band has been determined. Combinatorial chemical vapour deposition of TiO2 and ZrO2 on Si(100)-(2x1) was realized. A film with graded stoichiometry consisting of pure TiO2 and ZrO2 on the opposing ends and mixed composition of both oxides in the middle was obtained. A detailed study of the electronic levels revealed that ZrO2 remains an insulator in the monolayer regime and that modification of ZrO2 with a small amount of TiO2 leads to a more symmetric alignment of the bands relative to Si. The influence of a core hole on the O 1s x-ray absorption spectrum in TiO2 and ZrO2 is elucidated. Supported by O 1s photoemission measurements and ab initio calculations it is concluded that the static final state picture as well as dynamical threshold effects must be considered in order to determine the location of the conduction band minimum within the XAS framework. Finally a Co modified Co:ZnO film was shown to display ferromagnetic properties. It could be evidenced that Co with oxygen as nearest neighbours was responsible for the magnetism and not metallic Co.

<p>When the amorphous silicon (a-Si) dangling bonds are bonded to hydrogen the concentration of the dangling bond is decreased. The resulting film is called hydrogenated amorphous silicon (a-Si:H). The reduction in the dangling bonds concentration improves the optoelectrical properties of the film. The improved properties of a-Si:H makes it possible to manufacture electronic devices including a solar cell. A solar cell device based on the hydrogenated amorphous silicon (a-Si:H) was fabricated using the Hot-Wire Chemical Vapour Deposition (HWCVD). When an n-i-p solar cell configuration is grown, the norm is that the p-doped layer is deposited from a mixture of silane (SiH4) gas with diborane (B2H6). The boron atoms from diborane bonds to the silicon atoms and because of the number of the valance electrons, the grown film becomes a p-type film. Aluminium is a group 3B element and has the same valence electrons as boron, hence it will also produce a p-type film when it bonds with silicon. In this study the p-doped layer is grown from the co-deposition of a-Si:H from SiH4 with aluminium evaporation resulting in a crystallized, p-doped thin film. When this thin film is used in the n-i-p cell configuration, the device shows photo-voltaic activity. The intrinsic layer and the n-type layers for the solar cell were grown from SiH4 gas and Phosphine (PH3) gas diluted in SiH4 respectively. The individual layers of the solar cell device were characterized for both their optical and electrical properties. This was done using a variety of experimental techniques. The analyzed results from the characterization techniques showed the films to be of device quality standard. The analysed results of the ptype layer grown from aluminium showed the film to be successfully crystallized and doped. A fully functional solar cell was fabricated from these layers and the cell showed photovoltaic activity.<br /> &nbsp / </p>

WC-Co cutting tools are widely used in the machining industry. The application of diamond coatings on the surfaces of the tools would prolong the cutting lifetime and improves the manufacturing efficiency. However, direct chemical vapor deposition (CVD) of diamond coatings on WC-Co suffer from severe premature adhesion failure due to interfacial graphitization induced by the binder phase Co. In this research, a combination of hydrochloric acid (HCl) and hydrogen (H2) plasma pretreatments and a novel double interlayer of carbide forming element (CFE)/Al were developed to enhance diamond nucleation and adhesion. The results showed that both the pretreatments and interlayers were effective in forming continuous and adhesive nanocrystalline diamond coatings. The method is a promising replacement of the hazardous Murakami's regent currently used in WC-Co pretreatment with a more environmental friendly approach.<p> Apart from coatings, diamond can be fabricated into other forms of nanostructures, such as nanotips. In this work, it was demonstrated that oriented diamond nanotip arrays can be fabricated by ion beam etching of as-grown CVD diamond. The orientation of diamond nanotips can be controlled by adjusting the direction of incident ion beam. This method overcomes the limits of other techniques in producing nanotip arrays on large areas with controlled orientation. Oriented diamond nano-tip arrays have been used to produce anisotropic frictional surface, which is successfully used in ultra-precision positioning systems.<p> Diamond-like carbon (DLC) has many properties comparable to diamond. In this thesis, the preparation of á-C:H thin films by end-Hall (EH) ion source and the effects of ion energy and nitrogen doping on the microstructure and mechanical properties of the as-deposited thin films were investigated. The results have demonstrated that smooth and uniform á-C:H and á-C:H:N films with large area and reasonably high hardness and Youngs modulus can be synthesized by EH ion source with a low ion energy. The EH ion beam deposition of carbon-based thin films have potential applications such as protective coatings on high capacity magnetic memory disk, for which coating uniformity and smoothness cannot be achieved by the traditional sputtering methods.

WC-Co cutting tools are widely used in the machining industry. The application of diamond coatings on the surfaces of the tools would prolong the cutting lifetime and improves the manufacturing efficiency. However, direct chemical vapor deposition (CVD) of diamond coatings on WC-Co suffer from severe premature adhesion failure due to interfacial graphitization induced by the binder phase Co. In this research, a combination of hydrochloric acid (HCl) and hydrogen (H2) plasma pretreatments and a novel double interlayer of carbide forming element (CFE)/Al were developed to enhance diamond nucleation and adhesion. The results showed that both the pretreatments and interlayers were effective in forming continuous and adhesive nanocrystalline diamond coatings. The method is a promising replacement of the hazardous Murakami's regent currently used in WC-Co pretreatment with a more environmental friendly approach.<p> Apart from coatings, diamond can be fabricated into other forms of nanostructures, such as nanotips. In this work, it was demonstrated that oriented diamond nanotip arrays can be fabricated by ion beam etching of as-grown CVD diamond. The orientation of diamond nanotips can be controlled by adjusting the direction of incident ion beam. This method overcomes the limits of other techniques in producing nanotip arrays on large areas with controlled orientation. Oriented diamond nano-tip arrays have been used to produce anisotropic frictional surface, which is successfully used in ultra-precision positioning systems.<p> Diamond-like carbon (DLC) has many properties comparable to diamond. In this thesis, the preparation of á-C:H thin films by end-Hall (EH) ion source and the effects of ion energy and nitrogen doping on the microstructure and mechanical properties of the as-deposited thin films were investigated. The results have demonstrated that smooth and uniform á-C:H and á-C:H:N films with large area and reasonably high hardness and Youngs modulus can be synthesized by EH ion source with a low ion energy. The EH ion beam deposition of carbon-based thin films have potential applications such as protective coatings on high capacity magnetic memory disk, for which coating uniformity and smoothness cannot be achieved by the traditional sputtering methods.

In this study SBA-15 mesoporous silica template was synthesized and used as a sacrificial template in the preparation of ordered mesoporous carbon material. A chemical vapour deposition (CVD) technique using LPG or alternatively sucrose, pyrolyzed upon a mesoporous Si matrix were used to produce nanostructured ordered mesoporous carbon (OMC) with graphitic character after removing the Si template. The sucrose method was found to be a suitable route for preparing OMC. The OMC was used as a conductive three dimensional porous support for depositing catalytic nanophase Pt metal. Deposition of Pt nanoparticles on OMC was accomplished using a CVD method with Pt(acac)2 as a precursor. The synthesized nano-composite materials were characterized by several techniques such as, HRTEM, HRSEM, EDS, XRD, BET, TGA, FT-IR and CV.