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Particle contamination control is a critical issue for the semiconductor industry. In the near future, this industry will be concerned with the chemical identities of contaminant particles as small as 0.01 pm in size. Therefore, analytical techniques with both high chemical sensitivity and spatial resolution are required. Transmission electron microscopy (TEM) provides excellent spatial resolution and yields structural and compositional information. It is rarely used, however, due to the difficulty of sample preparation. The goals of this research are to promote the use of TEM as an ultrafine particle analysis tool by developing new sample preparation methods, and to exploit the new TEM techniques for analysis of particles in semiconductor processing fluids. A TEM methodology for the analysis of particulate contaminants in fluids with an elemental detectability limit as low as 0.1 part per trillion (ppt), and a particle concentration detectability limit as low as 1 particle/ml for particles greater than 0.2 pm was developed and successfully applied to the analysis of particles in HF, H202, de-ionized (DI) water, and on the surface of an electronic device. HF samples from three manufacturers were examined. For HF (B), the maximum particle concentration was 8.3 x 103 particles/ml. Both a viscous material and lath-shaped particles were observed. The Sb concentration was less than 0.6 part per billion (ppb). HF (C) was the cleanest. CaF2 and TiO2 particles were identified in HF (D). For H2 02, iron and tin oxides and hydroxides were identified. The maximum particle concentration was 990 particles/ml. The Sn and Fe concentrations were less than 0.3 ppb. Spherical and dendritic particles were observed. For DI water, spherical and dendritic particles (<2 particles/ml), and particles containing Fe or Si with concentrations less than 0.1 ppt were observed. Contaminants on an electronic device surface were also analyzed. Clusters of small particles were determined to be a mixture of aluminum oxides and aluminum silicates.

As características das células musculares e da junção miotendínea do músculo pterigóideo mediai de ratos adultos e com envelhecimento foram estudadas, empregando-se as técnicas de microscopia de luz e eletrônica de varredura e de transmissão. A microscopia de luz mostrou que as fibras musculares inserem-se na superfície óssea mandibular através de tecido colágeno composto por numerosos fibroblastos. Os cortes examinados sob luz polarizada revelaram a presença de fibras colágenas tipo\' e li\' nesta região. Além disso, puderam-se notar os capilares sangüíneos em grande número. Observações ao microscópio eletrônico de varredura ressaltaram as estriações presentes no músculo esquelético. O tecido conjuntivo que constitui o endomísio foi notado quando as amostras foram tratadas com solução de hidróxido de sódio e foi possível observar os diferentes diâmetros apresentados pelas fibras musculares. A microscopia eletrônica de transmissão evidenciou o alinhamento dos sarcômeros e as concentrações de mitocôndrias junto à lâmina basal na terminação da fibra muscular. O estudo da junção miotendínea dos ratos adultos e com envelhecimento identificou as fibras colágenas e os feixes de miofibrilas formando interdigitações que promovem o aumento da superfície de contato nesta região. Os aspectos observados nos músculos de ratos adultos mostraram-se bastante similares aos encontrados nos ratos com envelhecimento. / The mediai pterygoid muscle cells and myotendinous junction characteristics of adult and aging rats were studied, using light microscopy and scanning and transmission electron microscopy techniques. The Iight microscopy showed the muscle fibers inserting in the mandible surface through collagen tissue and numerous fibroblasts. The samples examined in polarized light revealed the presence of type I and 11I collagen fibers in this site. Furthermore, the numerous blood capillaries could be noticed. Observations at the scanning electron microscope evidenced strias present in the skeletal muscle. The connective tissue that constitutes the endomysium could be noticed when the samples were treated with sodium hydroxide solution and it was possible to observe the muscle fibers different diameters. The transmission electron microscopy revealed the sarcomeres alignment and the mitochondria concentration by the basal lamina in the muscle fiber termination. The adult and aging rats myotendinous junction study showed the collagen fibers and the myofibrils bundles developing finger-like processes that increases the contact areas in this site. The aspects seen in adult rats pterygoid muscles were very similar to the ones seen in the aging rats.

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abstract: In this dissertation research, conventional and aberration-corrected (AC) transmission electron microscopy (TEM) techniques were used to evaluate the structural and compositional properties of thin-film semiconductor compounds/alloys grown by molecular beam epitaxy for infrared photo-detection. Imaging, diffraction and spectroscopy techniques were applied to TEM specimens in cross-section geometry to extract information about extended structural defects, chemical homogeneity and interface abruptness. The materials investigated included InAs1-xBix alloys grown on GaSb (001) substrates, InAs/InAs1-xSbx type-II superlattices grown on GaSb (001) substrates, and CdTe-based thin-film structures grown on InSb (001) substrates. The InAsBi dilute-bismide epitaxial films were grown on GaSb (001) substrates at relatively low growth temperatures. The films were mostly free of extended defects, as observed in diffraction-contrast images, but the incorporation of bismuth was not homogeneous, as manifested by the lateral Bi-composition modulation and Bi-rich surface droplets. Successful Bi incorporation into the InAs matrix was confirmed using lattice expansion measurements obtained from misfit strain analysis of high-resolution TEM (HREM) images. Analysis of averaged intensity line profiles in HREM and scanning TEM (STEM) images of the Ga-free InAs/InAs1-xSbx type-II strained superlattices indicated slight variations in layer thickness across the superlattice stack. The interface abruptness was evaluated using misfit strain analysis of AC-STEM images, electron energy-loss spectroscopy and 002 dark-field imaging. The compositional profiles of antimony across the superlattices were fitted to a segregation model and revealed a strong antimony segregation probability. The CdTe/MgxCd1-xTe double-heterostructures were grown with Cd overflux in a dual-chamber molecular beam epitaxy with an ultra-high vacuum transfer loadlock. Diffraction-contrast images showed that the growth temperature had a strong impact on the structural quality of the epilayers. Very abrupt CdTe/InSb interfaces were obtained for epilayers grown at the optimum temperature of 265 °C, and high-resolution imaging using AC-STEM revealed an interfacial transition region with a width of a few monolayers and smaller lattice spacing than either CdTe or InSb. / Dissertation/Thesis / Doctoral Dissertation Materials Science and Engineering 2017

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Made available in DSpace on 2014-10-09T12:27:25Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:06:52Z (GMT). No. of bitstreams: 0 / A realização do presente trabalho permitiu o estudo dos micromecanismos de deformação e fratura da liga de titânio Ti-6Al-4V, utilizada comercialmente para a fabricação de biomateriais metálicos. As técnicas empregadas para a análise do material em estudo foram: microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET) e a difração de raios X (DRX). Estudar a influência e comportamento das diversas fases existentes em ligas de titânio é importante para se avaliar o comportamento de trincas nas ligas de titânio com alta resistência mecânica, que possuem microestrutura fina, relacionando a presença das fases alfa (&alpha;), beta (&beta;) e alfa+beta (&alpha;+&beta;) com a resistência do material. A avaliação in situ dos micromecanismos de deformação e fratura foi realizada por MET e também foi feito o estudo das transformações de fase durante o resfriamento em ligas de titânio, por MET, utilizando-se as técnicas de campo claro, campo escuro e difração de elétrons (DEAS), em área selecionada. Após tratamento térmico foram observadas as diferenças entre a quantidade das fases &alpha; e &beta;, em relação à microestrutura original do material para diferentes condições utilizadas no tratamento térmico aplicado à liga metálica. Observou-se a presença da microestrutura lamelar, formada durante o resfriamento no campo &beta;, promovendo a transformação de parte da estrutura alfa secundária em beta, que se encontrava retida entre as lamelas de alfa. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

As características das células musculares e da junção miotendínea do músculo pterigóideo mediai de ratos adultos e com envelhecimento foram estudadas, empregando-se as técnicas de microscopia de luz e eletrônica de varredura e de transmissão. A microscopia de luz mostrou que as fibras musculares inserem-se na superfície óssea mandibular através de tecido colágeno composto por numerosos fibroblastos. Os cortes examinados sob luz polarizada revelaram a presença de fibras colágenas tipo\' e li\' nesta região. Além disso, puderam-se notar os capilares sangüíneos em grande número. Observações ao microscópio eletrônico de varredura ressaltaram as estriações presentes no músculo esquelético. O tecido conjuntivo que constitui o endomísio foi notado quando as amostras foram tratadas com solução de hidróxido de sódio e foi possível observar os diferentes diâmetros apresentados pelas fibras musculares. A microscopia eletrônica de transmissão evidenciou o alinhamento dos sarcômeros e as concentrações de mitocôndrias junto à lâmina basal na terminação da fibra muscular. O estudo da junção miotendínea dos ratos adultos e com envelhecimento identificou as fibras colágenas e os feixes de miofibrilas formando interdigitações que promovem o aumento da superfície de contato nesta região. Os aspectos observados nos músculos de ratos adultos mostraram-se bastante similares aos encontrados nos ratos com envelhecimento. / The mediai pterygoid muscle cells and myotendinous junction characteristics of adult and aging rats were studied, using light microscopy and scanning and transmission electron microscopy techniques. The Iight microscopy showed the muscle fibers inserting in the mandible surface through collagen tissue and numerous fibroblasts. The samples examined in polarized light revealed the presence of type I and 11I collagen fibers in this site. Furthermore, the numerous blood capillaries could be noticed. Observations at the scanning electron microscope evidenced strias present in the skeletal muscle. The connective tissue that constitutes the endomysium could be noticed when the samples were treated with sodium hydroxide solution and it was possible to observe the muscle fibers different diameters. The transmission electron microscopy revealed the sarcomeres alignment and the mitochondria concentration by the basal lamina in the muscle fiber termination. The adult and aging rats myotendinous junction study showed the collagen fibers and the myofibrils bundles developing finger-like processes that increases the contact areas in this site. The aspects seen in adult rats pterygoid muscles were very similar to the ones seen in the aging rats.

Lithium-ion batteries(LIBs) have dominated the energy storage market in the past two decades. The high specific energy, low self-discharge, relatively high power and low maintenance of LIBs enabled the revolution of electronic devices and electric vehicle industry, changed the communication and transportation styles of the modern world. Although the specific energy of LIBs has increased significantly since first commercialized in 1991, it has reached a bottleneck with current electrode materials. To meet the increasing market demand, it is necessary to develop high capacity electrode materials.<div><br></div><div>Current commercial anode material for LIB is graphite which has a specific capacity of 372 mAh g-1. Other group IV elements (silicon (Si), germanium (Ge), tin (Sn)) have much higher capacities. However, group IV elements have large volume change during lithiation/delithiation, leading to pulverization of active materials and disconnection between electrode particles and current collector, resulting in fast capacity fading. To address this issue, it is essential to understand the microstructural evolution of Si, Ge and Sn during cycling.<br></div><div><br></div><div>This dissertation is mainly focused on the morphological and structural evolution of Sn and Ge based materials. In this dissertation, anin situ focused ion beam-scanning electron microscopy (FIB-SEM) method is developed to investigate the microstructuralevolution of a single electrode particle and correlate with its electrochemical performance. This method is applied toall projects. The first project is to investigate the microstructural evolution of a Sn particle during cycling. Surface structures of Sn particles are monitored and correlated with different states of charge. The second project is to investigate the morphological evolution of Ge particles at different conditions. Different structures (nanopores, cracks, intact surface) appear at different cycling rates. The third project is to study selenium doped Ge (GeSe) anodes. GeSe and Ge particles are tested at the same condition. Se doping forms Li-Ge-Se network, provides fast Li transport and buffers volume change. The fourth project is to study the reaction front of Ge particle during lithiation. Micron-sized Ge particles have two reaction fronts and a wedge shape reaction interface, which is different from the well-known core-shell mode. The fifth project is to investigate antimony (Sb)-coated porous Ge particles. The Sb coating suppresses electrolyte decomposition and porous structure alleviates volume change. The results in this dissertation reveal fundamental information about the reaction mechanism of Sn and Ge anode. The results also show the effects of doping, porous structuring and surface coating of anode materials.</div>