Diamond is widely known for its extraordinary properties, such as high hardness, thermal conductivity, electron mobility, energy bandgap and durability making it a very attractive material for many applications. Synthetic diamonds retain most of the attractive properties of natural diamond. Among the types of synthetic diamonds, nanocrystalline diamond (NCD) is being developed for electrical, tribological, optical, and biomedical applications. In this research work, NCD films were grown by the pulsed electron beam ablation (PEBA) method at different process conditions such as accelerating voltage, pulse repetition rate, substrate material and temperature. PEBA is a relatively novel deposition technique, which has been developed to provide researchers with a new means of producing films of equal or better quality than more conventional methods such as Pulsed Laser Deposition, Sputtering, and Cathodic Vacuum Arc. The deposition process parameters have been defined by estimating the temperature and pressure of the plasma particles upon impact with the substrates, and comparing the data with the carbon phase diagram. Film thickness was measured by visible reflectance spectroscopy technique and was in the range of 40 – 230 nm. The nature of chemical bonding, namely, the ratio (sp3/sp3+sp2) and nanocrystallinity percentage were estimated using visible Raman spectroscopy technique. The films prepared from the ablation of a highly ordered pyrolytic graphite (HOPG) target on different substrates consisted mainly of nanocrystalline diamond material in association with a diamond-like carbon phase. The micro-structural properties and surface morphology of the films were studied by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The mechanical properties of the NCD films were evaluated by nano-indentation.

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Nanocrystalline materials are polycrystalline solids with grain size in the nanometer range (< 100nm), which have been found to exhibit superior properties such as high magnetic permeability and corrosion resistance, as well as a considerably increase of strength when compared with their coarse grain counterparts. All those improved properties are attributed to the high volume fraction of grain boundaries (GBs). However, the high density of GBs brings a large amount of excess enthalpy to the whole system, making the nanostructures unstable and suffer from severe thermal or mechanical grain growth. In order to maintain the advantageous properties of nanocrystalline materials, it is necessary to stabilize GB and inhibit grain growth. While alloying has been found to be an effective way of achieving stabilized nanocrystalline metal alloys experimentally, the direct quantification of solute effects on GB motion still poses great challenge for investigating thermal stability of general nanocrystalline materials. In this research, impurity segregation and solute drag effects on GB motion were investigated by extending the interface random-walk method in direct molecular dynamics simulations. It was found that the GB motion was controlled by the solute diffusion perpendicular to the boundary plane. Based on the simulation results at different temperatures and impurity concentrations, the solute drag effects can be well modeled by the theory proposed by Cahn, Lücke and Stüwe (CLS model) more than fifty years ago. However, a correction to the original CLS model needs to be made in order to quantitatively predict the solute drag effects on a moving GB.

Made available in DSpace on 2014-06-11T19:23:29Z (GMT). No. of bitstreams: 0 Previous issue date: 2007-09-19Bitstream added on 2014-06-13T19:50:19Z : No. of bitstreams: 1 costa_wb_me_bauru.pdf: 1013500 bytes, checksum: af2a82e89ba237d24c1ff8441a9da739 (MD5) / Secretaria de Educação do Estado de São Paulo / Filmes nanocristalinos e amorfos de GaAs tem recentemente chamado a atenção de vários grupos de pesquisa devido as suas possíveis aplicações em novos dispositivos ópticos e eletrônicos. Igualmente atraentes são as novas propriedades físicas relacionadas com a estrutura nanocristalina e os efeitos da desordem na estrutura eletrônicas destes materiais. Entre as aplicações existentes, podemos citar o uso destes filmes como camadas anti-guia em lasers com emissão perpendicular à superfície, as camadas “buffer” em hetero-epitaxias de GaAs sobre Si, e os filtros interferométricos para a região do infravermelho. A preparação e a caracterização de filmes nanocristalinos de GaAs hidrogenados e não hidrogenados usando a técnica de RF magnetron sputtering foram focalizados neste trabalho. Um alvo de GaAs e uma atmosfera controlada contendo quantidades variáveis de argônio (Ar) e hidrogênio (H2) foram usadas na deposição do filme. Foi investigada a influência do fluxo de Ar e H2 na composição, estrutura e propriedades ópticas dos filmes. A influência da temperatura de substrato e potência de deposição também foi analisada. As técnicas de difração de raios-X e análise da energia de dispersão por emissão de raios-X (EDX), foram utilizadas na análise da estrutura e composição do filme, enquanto medidas ópticas de transmitância e refletância permitiram a determinação do coeficiente de absorção óptica e índice de refração dos filmes. A presença de ligações de hidrogênio nos filmes foi confirmada pelas bandas de absorção do Ga-H e As-H usando um espectrofotômetro de transformada de Fourier (FTIR). Os resultados mostram que a microestrutura, a composição e as propriedades ópticas do material são fortemente influenciadas por todos os parâmetros investigados, com destaque para o fluxo de hidrogênio utilizado nas deposições... / The nanocrystalline and amorphous GaAs films are recently attracting the attention of several research groups due to their possible application in new electronic and optical devices. Also attractive are the new physical properties related to the nanocrystalline structure and the effects of disorder in the electronic structure of these materials. Among the existing applications we can mention the use of these films as antiguide layers in surface emitting lasers, as buffer layers in the GaAs hetero-epitaxy onto Si substrates, and as infrared interferometric filters. The preparation and characterization of hydrogenated and non-hydrogenated nanocrystalline GaAs films using the RF magnetron sputtering technique were focused here. An electronic grade GaAs water target and an atmosphere composed of variable amounts of Ar and 'H IND.2' were used in the film depositions. We have investigated the influence of Ar and 'H IND.2' fluxes on composition, structure, and optical properties of the films. The influence of substrate temperature and deposition power were also analyzed. X-ray diffraction and energy dispersive electron analysis (EDX) were used in the analysis of the film structure and composition, while optical transmittance and reflectance measurements allowed the determination of the optical absorption coefficient and refractive index of the films. The presence of bonded hydrogen in the films was confirmed by the Ga-H and As-H absorption bands using Fourier transform infrared spectra (FTIR). The results show that the microstructure, the composition, and the optical properties of the material are strongly influenced by all the investigated parameters, in special the hydrogen flux used in the depositions. The hydrogenated films ('H IND.2' flux of 3.0 sccm / Ar flux of 20.0 sccm) produced at relatively low power (30W) and substrate temperature (60ºC), have presented the widest... (Complete abstract click electronic access below)

abstract: Silicon nanowires were grown epitaxially on Si (100) and (111) surfaces using the Vapor-Liquid-Solid (VLS) mechanism under both thermal and plasma enhanced growth conditions. Nanowire morphology was investigated as a function of temperature, time, disilane partial pressure and substrate preparation. Silicon nanowires synthesized in low temperature plasma typically curved compared to the linear nanowires grown under simple thermal conditions. The nanowires tended bend more with increasing disilane partial gas pressure up to 25 x10-3 mTorr. The nanowire curvature measured geometrically is correlated with the shift of the main silicon peak obtained in Raman spectroscopy. A mechanistic hypothesis was proposed to explain the bending during plasma activated growth. Additional driving forces related to electrostatic and Van der Waals forces were also discussed. Deduced from a systematic variation of a three-step experimental protocol, the mechanism for bending was associated with asymmetric deposition rate along the outer and inner wall of nanowire. The conditions leading to nanowire branching were also examined using a two-step growth process. Branching morphologies were examined as a function of plasma powers between 1.5 W and 3.5 W. Post-annealing thermal and plasma-assisted treatments in hydrogen were compared to understand the influences in the absence of an external silicon source (otherwise supplied by disilane). Longer and thicker nanowires were associated with longer annealing times due to an Ostwald-like ripening effect. The roles of surface diffusion, gas diffusion, etching and deposition rates were examined. / Dissertation/Thesis / Ph.D. Materials Science and Engineering 2011

abstract: Nanocrystalline (nc) thin films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. Furthermore, the mechanical behavior and microstructure of nc films is intimately related. Thus, precise control of the size, aspect ratio and spatial distribution of grains can enable the synthesis of thin films with exceptional mechanical properties. However, conventional bottom-up techniques for synthesizing thin films are incapable of achieving the microstructural control required to explicitly tune their properties. This dissertation focuses on developing a novel technique to synthesize metallic alloy thin films with precisely controlled microstructures and subsequently characterizing their mechanical properties using in situ transmission electron microscopy (TEM). Control over the grain size and distribution was achieved by controlling the recrystallization process of amorphous films by the use of thin crystalline seed layers. The novel technique was used to manipulate the microstructure of structural (TiAl) and functional (NiTi) thin films thereby exhibiting its capability and versatility. Following the synthesis of thin films with tailored microstructures, in situ TEM techniques were employed to probe their mechanical properties. Firstly, a novel technique was developed to measure local atomic level elastic strains in metallic glass thin films during in situ TEM straining. This technique was used to detect structural changes and anelastic deformation in metallic glass thin films. Finally, as the electron beam (e-beam) in TEMs is known to cause radiation damage to specimen, systematic experiments were carried out to quantify the effect of the e-beam on the stress-strain response of nc metals. Experiments conducted on Al and Au films revealed that the e-beam enhances dislocation activity leading to stress relaxation. / Dissertation/Thesis / Supplementary Video S1 / Supplementary Video S2 / Supplementary Video S3 / Doctoral Dissertation Materials Science and Engineering 2017

Orientador: José Humberto Dias da Silva / Banca: Carlos Frederico de Oliveira Graeff / Banca: Antonio Ricardo Zanatta / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: A recente descoberta de propriedades ferromagnéticas em alguns semicondutores magnéticos diluídos (DMS) trouxe a esta classe de materiais um grande potencial para aplicações em dispositivos de controle de spin. Um DMS é basicamente formado por um semicondutor dopado por íons magnéticos, os quais têm o papel de criar um momento magnético local e também, em algumas situações, de introduzir portadores livres no material. Entre os DMSs conhecidos, o 'GA IND.1-x'MN IND.XN' surge como o mais forte candidato a aplicações práticas por apresentar até o momento a mais alta temperatura de transição ferromagnética ('T IND.C' 'DA ORDEM DE' 400 k). Até o presente, os filmes de 'GA IND.1-x'MN IND.XN' com propriedades ferromagnéticas relatados na literatura foram preparados por epitaxia por feixe molecular (MBE). Neste trabalho, descrevemos a preparação de filmes nanocristalinos de 'GA IND.1-x'MN IND.XN' com diferentes conteúdos de Mn (0,00 'MENOR' x 'MENOR' 0,18) pela técnica de RF-magnetron sputtering reativo. Analisamos os efeitos da incorporação de Mn na estrutura e nas propriedades ópticas destes filmes através de medidas de difração de raios-X e de absorção óptica entre o ultravioleta (6,5 eV) e infravermelho próximo (1,4 eV). Os resultados apontam um aumento do parâmetro de rede e do índice de refração, uma diminuição do gap ótico e um aumento da densidade de estados de defeitos no interior do gap conforme se aumenta o conteúdo de Mn nos filmes de 'GA IND.1-x'MN IND.XN' preparados por sputtering. Estes resultados são semelhantes aos reportados para a incorporação de Mn em filmes monocristalinos de 'GA IND.1-x'MN IND.XN' com propriedades ferromagnéticas preparados por MBE. / Abstract: The recent discoveries related to the ferromagnetic properties in some diluted magnetic semiconductors (DMS) have attracted considerable attention on this class of material due to their potential application on spin control devices. A DMS is basically formed by a semiconductor doped with magnetic ions with the purpose of creating local magnetic moments and, in some situations, to introduce free carriers in the material. Among the known DMSs, 'GA IND.1-x'MN IND.XN' is the one with the highest ferromagnetic transition temperature ('T IND.C' 'DA ORDEM DE' 400 k), and it is consequently on of the stronger candidates for practical applications. Until now, the 'GA IND.1-x'MN IND.XN' films with ferromagnetic properties described in the literature were prepared by molecular beam epitaxy (MBE). In this work, we report the preparation of nanocrystalline 'GA IND.1-x'MN IND.XN' films (0,00 'MENOR' x 'MENOR' 0,18) by reactive RF-magnetron sputtering technique. We analyzed the Mn incorporation effects on structure and optical properties of the films by X-ray diffraction measurements and optical absorption between UV (6,5 eV) and near infrared (1,4 eV). The results show the increase of the lattice parameters and of the refractive index, a decrease of the optical gap and a increase of defect states in the gap when Mn concentration is increased. These results are similar to those reported for Mn incorporation in monocrystalline 'GA IND.1-x'MN IND.XN' films prepared by MBE with ferromagnetic properties. / Mestre

Orientador: José Humberto Dias da Silva / Banca: Américo Tabata / Banca: Johnny Vilcarromero Lopez / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: Filmes nanocristalinos e amorfos de GaAs tem recentemente chamado a atenção de vários grupos de pesquisa devido as suas possíveis aplicações em novos dispositivos ópticos e eletrônicos. Igualmente atraentes são as novas propriedades físicas relacionadas com a estrutura nanocristalina e os efeitos da desordem na estrutura eletrônicas destes materiais. Entre as aplicações existentes, podemos citar o uso destes filmes como camadas anti-guia em lasers com emissão perpendicular à superfície, as camadas "buffer" em hetero-epitaxias de GaAs sobre Si, e os filtros interferométricos para a região do infravermelho. A preparação e a caracterização de filmes nanocristalinos de GaAs hidrogenados e não hidrogenados usando a técnica de RF magnetron sputtering foram focalizados neste trabalho. Um alvo de GaAs e uma atmosfera controlada contendo quantidades variáveis de argônio (Ar) e hidrogênio (H2) foram usadas na deposição do filme. Foi investigada a influência do fluxo de Ar e H2 na composição, estrutura e propriedades ópticas dos filmes. A influência da temperatura de substrato e potência de deposição também foi analisada. As técnicas de difração de raios-X e análise da energia de dispersão por emissão de raios-X (EDX), foram utilizadas na análise da estrutura e composição do filme, enquanto medidas ópticas de transmitância e refletância permitiram a determinação do coeficiente de absorção óptica e índice de refração dos filmes. A presença de ligações de hidrogênio nos filmes foi confirmada pelas bandas de absorção do Ga-H e As-H usando um espectrofotômetro de transformada de Fourier (FTIR). Os resultados mostram que a microestrutura, a composição e as propriedades ópticas do material são fortemente influenciadas por todos os parâmetros investigados, com destaque para o fluxo de hidrogênio utilizado nas deposições... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The nanocrystalline and amorphous GaAs films are recently attracting the attention of several research groups due to their possible application in new electronic and optical devices. Also attractive are the new physical properties related to the nanocrystalline structure and the effects of disorder in the electronic structure of these materials. Among the existing applications we can mention the use of these films as antiguide layers in surface emitting lasers, as buffer layers in the GaAs hetero-epitaxy onto Si substrates, and as infrared interferometric filters. The preparation and characterization of hydrogenated and non-hydrogenated nanocrystalline GaAs films using the RF magnetron sputtering technique were focused here. An electronic grade GaAs water target and an atmosphere composed of variable amounts of Ar and 'H IND.2' were used in the film depositions. We have investigated the influence of Ar and 'H IND.2' fluxes on composition, structure, and optical properties of the films. The influence of substrate temperature and deposition power were also analyzed. X-ray diffraction and energy dispersive electron analysis (EDX) were used in the analysis of the film structure and composition, while optical transmittance and reflectance measurements allowed the determination of the optical absorption coefficient and refractive index of the films. The presence of bonded hydrogen in the films was confirmed by the Ga-H and As-H absorption bands using Fourier transform infrared spectra (FTIR). The results show that the microstructure, the composition, and the optical properties of the material are strongly influenced by all the investigated parameters, in special the hydrogen flux used in the depositions. The hydrogenated films ('H IND.2' flux of 3.0 sccm / Ar flux of 20.0 sccm) produced at relatively low power (30W) and substrate temperature (60ºC), have presented the widest... (Complete abstract click electronic access below) / Mestre

Increasing the power density of the DC-DC converters requires the size and weight of the magnetic components, such as inductors and transformers, to be reduced. In this thesis, the losses in nanocrystalline inductor cores are characterised and analysed, including the traditional core loss and the gap loss caused by the air gap fringing flux. The loss calculations will form a basis for the design and optimisation of high power inductors for DC-DC converters for EV applications. This thesis first characterises experimentally the core losses in four nanocrystalline cores over a range of operating conditions that are representative of those encontered in typical high power converter applications, including non-sinusoidal waveforms and DC bias conditions. The core losses are assessed by the measured B-H loops and are characterised as a function of DC flux density, showing that for a fixed AC induction level, the losses can vary by almost an order of magnitude as the DC bias increases and the duty ratio moves away from 0.5. The results provide a more complete picture of the core loss variations with both DC and AC magnetisations than is available in manufactures’ data sheets. An electromagnetic finite element (FE) model is used to examine the gap loss that occurs in finely laminated nanocrystalline cores under high frequency operation. The loss is significant in the design example, contributing to almost half of the total inductor loss, and the gap loss is highly concentrated in the region of the air gap. The dependence of the gap loss on key inductor design parameters and operating condtions is also explored. An empirical equation is derived to provide a design-oriented basis for estimating gap losses. Thermal finite element analysis is used to estimate the temperature rise and identify the hot spot in a nanocrystalline inductor encapsulated in an alumimium case. The temperature distribution in the core largely corresponds to the non-uniform distribution of the gap loss. The thermal FEA can also be used to evaluate different thermal management methods to optimise the design for a more compact component. The FE modelling of gap loss and the thermal predictions are validated experimentally on a foil-wound Finemet inductor, showing good agreement between the predictions and measurements under various operating conditions.

>Magister Scientiae - MSc / Without reverting to encapsulation, organic bulk - heterojunction solar cells can be protected from the oxidation of the highly reactive low work function cathode metal electrode, by the deposition of metal oxide buffer layers onto an indium-tin oxide (ITO) substrate. The zinc-oxide (ZnO) or titanium dioxide (TiO2) layer can serve as an electron collecting contact. In such a case the ordering of layer deposition is inverted from the traditional layer sequencing, using an additional effect of the metal oxide layer acting as a hole blocking contact