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Čermák, Jan. "Návrh automatizovaného procesu elektrolytického leštění vzorků pro elektronový mikroskop." Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2021. http://www.nusl.cz/ntk/nusl-444286.
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This diploma thesis deals with the automation of the electropolishing process, which is per-former as the last step in the preparation of metallographic samples intended for observation in an electron microscope. A complete hardware design of a single-purpose machine has been developed, which provides the automatic preperation of up to six samples per insertion. There was the design of a manipulator for sample handling together with chemically re-sistant sample holder suitable for automatic operation as a part of solution. The design of the whole machine was developed with regard to the safety of the operator. The thesis includes detailed 3D model of the device and the desing of an application for measurement in the LabVIEW. It describes the future working process of the machine, including a description of a software for controlling the machine and sending process data of each sample to the to the database in accordance with the principles of industry 4.0. In the conclusion, the achieved results and the proposal of further steps necessary for the realization of the machine are for-mulated.
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Schilling, Sibylle. "Liquid in situ analytical TEM : technique development and applications to austenitic stainless steel." Thesis, University of Manchester, 2017. https://www.research.manchester.ac.uk/portal/en/theses/liquid-in-situ-analytical-tem-technique-development-and-applications-to-austenitic-stainless-steel(fd490551-7d7a-4b2e-9b1f-917b5f8165b3).html.
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Environmentally-assisted cracking (EAC) phenomena affect the in-service behaviour of austenitic stainless steels in nuclear power plants. EAC includes such degradation phenomena as Stress Corrosion Cracking (SCC) and Corrosion Fatigue (CF). Factors affecting EAC include the material type, microstructure, environment, and stress. This is an important degradation issue for both current and Gen III+ light water reactors, particularly as nuclear power plant lifetimes are extended ( > 60 years). Thus, it is important to understand the behaviour of the alloys used in light water reactors, and phenomena such as SCC to avoid failures. Although there is no agreement on the mechanism(s) of SCC, the importance of localized electrochemical reactions at the material surface is widely recognised. Considerable research has been performed on SCC and CF crack growth, but the initiation phenomena are not fully understood. In this project, novel in situ analytical TEM techniques have been developed and applied to explore localised reactions in Type 304 austenitic stainless steel. In situ transmission electron microscopy has become an increasingly important and dynamic research area in materials science with the advent of unique microscope platforms and a range of specialized in situ specimen holders. In metals research, the ability to image and perform X-ray energy dispersive spectroscopy (XED) analyses of metals in liquids are particularly important for detailed study of the metal-environment interactions with specific microstructural features. To further facilitate such studies a special hybrid specimen preparation technique involving electropolishing and FIB extraction has been developed in this thesis to enable metal specimens to be examined in the liquid cell TEM specimen holder using both distilled H2O and H2SO4 solutions. Furthermore, a novel electrode configuration has been designed to permit the localized electrochemical measurement of electron-transparent specimens in the TEM. These novel approaches have been benchmarked by extensive ex situ experiments, including both conventional electrochemical measurements and microcell measurements. The results are discussed in terms of validation of in situ test data as well as the role of the electron beam in the experiments. In situ liquid cell TEM experiments have also explored the localized dissolution of MnS inclusions in H2O, and correlated the behaviour with ex situ experiments. Based on the research performed in this thesis, in situ liquid cell and in situ electrochemical cell experiments can be used to study nanoscale reactions pertaining to corrosion and localized dissolution leading to "precursor" events for subsequent EAC phenomena.
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Ryan, Keith Patrick. "Rapid cryogenic fixation of biological specimens for electron microscopy." Thesis, University of Plymouth, 1991. http://hdl.handle.net/10026.1/2504.
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This thesis describes investigations into cryofixation by the plunge-cooling technique, at ambient pressure. The objective was to characterise coolants which are commonly used for cryofixation, so that the structure and chemistry of biological specimens may be preserved in a more life-like state. The work began with the design of a suitable cooling device. This was developed further into a large test-bed apparatus which was used in both biological and methodological experiments. The large cooling apparatus demonstrated for the first time that ethane was a superior coolant under forced convection, compared to propane or Freon 22, for bare thermocouples, for exposed hydrated specimens and for metal-sandwiched hydrated specimens. Ice crystal formation was monitored in sandwiched specimens and found to correspond closely to modelling predictions. A biological application was the X-ray microanalysis of body fluids in "indicator" species of Chaetognaths, where results obtained from cryoscanning electron microscopy revealed ecophysiological differences. The use of low thermal mass supports demonstrated that good freezing can occur in the centre of specimens. A new cryomounting method was developed to load well-frozen specimens into the microscope. The effect of post-freeze processing temperature was investigated by monitoring ice crystals in red blood cells. Exposure to 213 K (-60°C) over a 48 hour period did not induce crystal growth and exposure to 233 K (-40°C) for 8 days showed minimal ice crystal damage. The progress of cryosubstitution was monitored over 48 h at 193 K ( -80°C), this showed that uranium ingressed to a depth of 320 µm which could be doubled when shrinkage was allowed for. The conclusion was that observed ice crystal damage originated during the initial freezing and not during subsequent cryoprocessing.
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Waterbury, Raymond. "The electron microscopy proteomic organellar preparation robot /." Thesis, McGill University, 2006. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=102768.
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An Electron Microscopy Proteomic Organellar Preparation (EMPOP) robot was developed as a tool for high-throughput preparation of subcellular fraction samples for electron microscopic identification. It will provide a means for validation of subcellular sample purity and confirmation of protein localization needed for organellar proteomics.The device automates all chemical and mechanical manipulations required to prepare organelles for electron microscopic examination. It has a modular, integrated design that supports automated filtration, chemical processing, delivery and embedding of up to 96 subcellular fraction samples in parallel. Subcellular fraction specimens are extremely fragile. Consequently, the system was designed as a single unit to minimize mechanical stress on the samples by integrating a core mechanism, composed of four modular plates, and seven support subsystems for: (1) cooling, (2-3) fluid handling, (4-7) positioning. Furthermore, control software was developed specifically for the system to provide standardized, reproducible sample processing while maintaining flexibility for adjustment and recall of operational parameters.
Development of the automated process progressed from initial validation experiments and process screening to define operational parameters for preservation of sample integrity and establish a basic starting point for successful sample preparation. A series of successive modifications to seal the local environment of the samples and minimize the effect of fluidic perturbations further increased process performance. Subsequent testing of the robot's full sample preparation capacity used these refinements to generate 96 samples in approximately 16 hours; reducing the time and labor requirement of equivalent manual preparation by up to 1,000 fold.
These results provide a basis for a structured approach toward process optimization and subsequent utilization the device for massive, parallel preparation of subcellular fraction samples for electron microscopic screening and quantitative analysis of subcellular and protein targets necessary for high-throughput proteomics.
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Frangakis, Achilleas S. "Noise reduction and segmentation techniques developed for multidimensional electron microscopy of biological specimens." [S.l. : s.n.], 2001. http://deposit.ddb.de/cgi-bin/dokserv?idn=962126888.
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Punwani, Karishma. "Automated control of the electron microscopy proteomic organellar preparation robot." Thesis, McGill University, 2005. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=99011.
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Electron microscopy (EM) is an important tool in organellar proteomics, where it is used to validate sample purity and to confirm protein presence. Current sample preparation techniques are manual, labor-intensive and time-consuming. To overcome these problems, an electron microscopy proteomic organellar preparation (EMPOP) robot is being developed for parallel preparation of up to 96 subcellular fraction samples in an efficient, repeatable and standardized manner. This thesis describes the development and validation of the software that controls the EMPOP robot. The software was organized in two coordinated levels consisting of a: (1) human-machine interface (HMI), and (2) low-level real-time control routines. The HMI was designed to be 'friendly and flexible', and to enable the operator to modify system parameters on-the-fly. Contrarily, the low-level control routines are responsible for controlling all EMPOP system processes. Pilot studies using the EMPOP system prove that the robot and software function predictably and consistently to generate high quality subcellular sample fractions.
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Knappett, Benjamin Richard. "Preparation of core@shell magnetic nanoparticles and their characterisation by electron microscopy." Thesis, University of Cambridge, 2015. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.709096.
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Harvey, Tyler. "Electron Orbital Angular Momentum| Preparation, Application and Measurement." Thesis, University of Oregon, 2017. http://pqdtopen.proquest.com/#viewpdf?dispub=10599464.
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The electron microscope is an ideal tool to prepare an electron into a specified quantum state, entangle that state with states in a specimen of interest, and measure the electron final state to indirectly gain information about the specimen. There currently exist excellent technologies to prepare both momentum eigenstates (transmission electron microscopy) and position eigenstates (scanning transmission electron microscopy) in a narrow band of energy eigenstates. Similarly, measurement of the momentum and position final states is straightforward with post-specimen lenses and pixelated detectors. Measurement of final energy eigenstates is possible with magnetic electron energy loss spectrometers. In 2010 and 2011, several groups independently showed that it was straightforward to prepare electrons into orbital angular momentum eigenstates. This disseratation represents my contributions to the toolset we have to control these eigenstates: preparation, application (interaction with specimen states), and measurement. My collaborators and I showed that phase diffraction gratings efficiently produce electron orbital angular momentum eigenstates; that control of orbital angular momentum can be used to probe chirality and local magnetic fields; and that there are several routes toward efficient measurement.
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Tipping, Claudia, of Western Sydney Hawkesbury University, of Science Technology and Agriculture Faculty, and School of Horticulture. "Morphological and structural investigations into C3 C4 and C3/C4 members of the genus Panicum grown under elevated CO2 concentrations." THESIS_FSTA_HOR_Tipping_C.xml, 1996. http://handle.uws.edu.au:8081/1959.7/329.
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Three perennial tropical Panicum species were grown under ambient and elevated (900 ppm) carbon dioxide concentrations in especially designed microclimate chambers. The study aimed to investigate the influence of high carbon dioxide concentrations on morphology/anatomy with physiological change among three closely related species possessing distinctly different photosynthetic pathways. The anatomy of the leaf was investigated using light microscopy (LM), transmission electron microscopy (TEM), and graphics image analysis. A suitable schedule for fixation, dehydration and embedding of leaf specimens for both forms of microscopy was developed. The anatomy of the species investigated did not change qualitatively, but there were detectable changes in leaf thickness and tissue proportions of the epidermis, mesophyll and thickened tissues (sclerenchyma, bundle sheath, vascular elements) that differed with species. This study is also relevant to the investigation of the evolution of C4, although species, and the progression involved in plants with characteristics intermediate between those of C3 and C4 species. These intermediate species have been mainly characterized by CO2 exchange and biochemical analysis, but they also display anatomical characteristics in between those of C3 and C4 plants. The evolutionary progression of the C3 to C4 species remains unsolved, although current studies indicate that the evolutionary step was from the C3 plant to the C4. Thus the intermediate C3/C4 plants may not be intermediate in an evolutionary sense and they could be seen as a simple hybridization between a C3 plant and C4 plant. In most of the parameters measured the C3/C4 P. decipiens resembled either the C3 P. tricanthum or the C4 P. antidotale. It may therefore be likened to a physiological chimera rather than to a true intermediate formDoctor of Philosophy (PhD)
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Hrubanová, Kamila. "Scanning Electron Microscopy and its Applications for Sensitive Samples." Doctoral thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2019. http://www.nusl.cz/ntk/nusl-409082.
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Předložená dizertační práce s názvem “Rastrovací elektronová mikroskopie a její aplikace pro senzitivní vzorky” pojednává o problematice rastrovací elektronové mikroskopie v kontextu instrumentálního a metodologického vývoje vedoucího k inovativnímu řešení, které je dobře aplikovatelné zejména v mikrobiologickém výzkumu. Součástí práce je rozprava o historii a současném stavu elektronové mikroskopie (EM) jakožto vědecké zobrazovací a analytické techniky, tato část se nachází v úvodních kapitolách. Nepopiratelný přínos EM v biologických a lékařských oborech je dokazován mnoha citovanými vědeckými publikacemi. Předložená dizertační práce přináší novinky z oblasti přípravy preparátů a kryogenní rastrovací elektronové mikroskopie (cryo-SEM) vyvinuté na pracovišti Ústavu přístrojové techniky AV ČR, v.v.i. v Brně. Jedná se především o návrhy a výrobu speciálních držáků vzorků a vývoj nových metodik v oblasti přípravy mikrobiologických preparátů vedoucích k nalezení optimálních parametrů jednotlivých procesů. V experimentální části se nachází ověření metodologických postupů při studiu hydratovaných a na elektronový svazek senzitivních preparátů. Následné srovnání různých přístupů na definovaném biologickém systému z oblasti mikrobiologie přispívá k rozšíření interpretace doposud známých výsledků. Mezi zkoumanými mikrobiologickými kmeny byly biofilm-pozitivní bakterie Staphylococcus epidermidis a kvasinky jako Candida albicans a Candida parapsilosis, jež jsou považovány za klinicky významné, protože se podílejí na vzniku závažných infekcí zejména u imunokompromitovaných pacientů. Dále byl studován vliv růstu biofilmu bakterie Bacillus subtilis na biodeteriorizaci a biodegradaci poly--kaprolaktonových fólií. Vývoj v oblasti cryo-SEM byl aplikován ve výzkumu mikrobů s biotechnologickým potenciálem, jako jsou např. Cupriavidus necator a Sporobolomyces shibatanus.
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Necsulescu, Valerica. "An assessment on the use of tissue clear® versus xylene in deparaffinizing wax containing specimens for electron microscopy." Thesis, Bloemfontein : Central University of Technology, Free State, 2006. http://hdl.handle.net/11462/86.
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Thesis (M. Tech.) - Central University of Technology, Free State, 2006Electron microscopy plays an important role in diagnostic histopathology. When this investigation is anticipated, extra tissue is submitted directly for electron microscopy. However, often it is decided only later in a problematic case to perform this investigation and then the only tissue available is embedded in the routine laboratory’s paraffin block. This tissue has to be retrieved from the wax and this entails using a clearing agent before the rest of the electron microscopy method can be implemented. Traditionally xylene is the agent that is used but has the disadvantage of being extremely toxic. This study compared the morphological effects of a relatively new and non toxic clearing agent, Tissueclear®, with that of xylene. Exposure of tissue to clearing agents for 30 minutes and overnight was performed to assess whether Tissueclear® gave better results in the long term than xylene, in the hope that the laboratory turn around time could be improved and the amount of toxic reagents used in the EM laboratory will be reduced. A second part of the study involved a questionnaire submitted to laboratory staff to assess their knowledge of xylene toxicity. Of the 325 cases submitted for electron microscopy at Universitas Hospital between January 2004 and July 2005, 140 of these had to be retrieved from paraffin wax. Four specimens were prepared from each case. Two were processed in xylene for 30 minutes and overnight and two in Tissueclear® for 30 minutes and overnight. The specimens were evaluated for consistency and resin compaction as well as ultrastructural preservation of the cell membrane, cytoplasmic content and extracellular material. The results showed that Tissueclear® and xylene gave comparable results after 30 minutes and that Tissueclear® was superior after overnight processing. This meant that a specimen submitted for electron microscopy would be processed immediately without waiting for the following morning as was the case with xylene and that the processing time for such a specimen had been shortened from 3 to 2 days. It also meant that the laboratory staff was exposed to one less toxic reagent. The results on the questionnaire showed that there were large areas of ignorance regarding toxicity as well as appropriate safety procedures that need to be followed in the laboratory. It is hoped that this study will improve awareness in this regard and encourage the use of other newer less toxic reagents.
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Moore, Katharine. "Preparation and characterisation of mixed CeO2-Nb2O5-Bi2O3 nanoparticles." Thesis, University of Cambridge, 2015. https://www.repository.cam.ac.uk/handle/1810/252691.
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Mixed metal oxides are ionic compounds containing at least two metal ions within an oxide structure. The literature contains a plethora of examples of mixed metal oxides on the bulk scale, which have been well characterised, however, mixed metal oxides on the nanoscale are far less well understood. The work presented here investigates the Bi2O3-CeO2-Nb2O5 mixed oxide system and characterises the resulting nanoparticles and crystal structures. Although the parent oxides are well known and much work has previously been done in analysing their crystal structures, combinations of these oxides have not been well characterised, especially on the nanoscale. Using high resolution electron microscopy (HRTEM), powder X-ray diffraction (PXRD), electron dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) as analytical tools, the structures of the nanoparticles in this system have been explored. As each of the parent oxides possess useful properties, which have been utilised in industrial applications such as electrolyte components in solid oxide fuel cells and as catalysts in a range of chemical reactions, it was hypothesised that if all three metal ions could be contained in one particle they could show novel and interesting characteristics. It was proposed that due to the more relaxed crystal structure in nanoparticles, the solid solubility of the metal ions should be increased, and a solid solution of ions would form. This work presents results showing the synthesis of binary and ternary oxides in the nano-form within the Bi2O3-CeO2-Nb2O5 system, including quantitative analysis of these particles. Secondly, and most importantly, it presents the first successful synthesis of quaternary oxide nanoparticles containing bismuth, cerium and niobium using the low temperature resin-gel method. Finally, the work attempts to explain how and why the ions are ordered in a given arrangement, with bismuth showing a preference for surface site occupation, as shown by XPS data, and describes some preliminary computational results which corroborate the experimental data.
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Bouwer, James Christopher. "Preparation, theory, and biological applications of highly luminescent CdSe/ZnS quantum dots in optical and electron microscopy /." Diss., Connect to a 24 p. preview or request complete full text in PDF format. Access restricted to UC IP addresses, 2002. http://wwwlib.umi.com/cr/ucsd/fullcit?p3061628.
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Yang, Fan. "Structural analysis of gastric H+,K+-ATPase at E1 state using carbon sandwich preparation in cryo-electron microscopy." Master's thesis, 京都大学 (Kyoto University), 2014. http://hdl.handle.net/2433/188532.
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Johnson, Matthew C. "Identifying key factors in two-dimensional crystal production and sample preparation for structure-function studies of membrane proteins by cryo-EM." Diss., Georgia Institute of Technology, 2013. http://hdl.handle.net/1853/52974.
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Electron crystallography of two-dimensional crystals is a structure-determination method well suited to the study of membrane protein structure-function. Two-dimensional crystals consist of ordered arrays of protein within reconstituted lipid bilayers, an arrangement that mimics the natural membrane environment. In this work we describe our recent progress in the use of this method with three different proteins, each providing a window into a separate paradigm in the electron crystallographic pipeline. Specific crystallization conditions for human leukotriene C₄ synthase (LTC₄S) have previously been determined, but our continued refinement of purification and crystallization has identified a number of additional parameters that greatly affect crystal size and quality, and we have developed a protocol to rapidly and reproducibly grow large, non-mosaic crystals of LTC₄S. The human gamma-glutamyl carboxylase (GGCX) has also been crystallized, but is sensitive to cryo-EM sample preparation conditions and we present here the successful reproduction of crystallization and refinement of cryo-EM sample preparation conditions. Lastly, we describe our crystallization screens with the Vibrio cholerae sodium-pumping NADH:ubiquinone reductase complex (Na⁺-NQR), and identify the factors critical to membrane reconstitution of the complex, a necessary first step towards crystallization. We also describe a semi-quantitative crystal screening protocol we have developed that provides quick and accurate method to assess two- dimensional crystallization trials, and discuss some general observations in optimization of membrane protein purification and two-dimensional crystallization for electron crystallography.
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Schumann, Dirk. "High resolution structural investigation of synthetic and natural 2:1 clay-mineral assemblages using advanced sample preparation and electron microscopy imaging techniques." Thesis, McGill University, 2012. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=106372.
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In this study, X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), and conventional TEM (CTEM) of Pt-C replicas are used to characterize both synthetic and natural 2:1 clay minerals from a variety of geological environments. In manuscript 1, reference samples of illite and expandable 2:1 clay minerals (i.e., smectite-group minerals, vermiculite and rectorite) varying in interlayer charge were investigated to characterize their interlayer expansion after treatment with octadecylammonium (nC=18) cations. The results of this study show that the treatment of ultrathin sections of 2:1 clay minerals with nC=18 cations and their subsequent investigation under the HRTEM provide information on the distribution of layer charges and layer-charge heterogeneities that cannot be obtained with conventional techniques of sample preparation. The major objective of manuscript 2 is to test whether oxalate catalyzes the crystallization of saponite at low temperatures and pressures. Additionally, the experiments of this study allow the investigation of the expansion behaviour and the structure of newly formed saponite crystals after exchange with n-alkylammonium cations in HRTEM lattice-fringe images. As these clay minerals are interpreted to replicate by template-catalyzed polymerization and transmit the charge distribution from layer to layer, the formation of 2:1 layer silicates with a variable layer-charge has significant implications for the abiotic origin of life. The finding that polar organic molecules such as oxalic acid catalyze clay-mineral formation in the laboratory is of great relevance to what processes may have occurred on carbonaceous chondrites and on the primitive, outgassing Earth that finally led to the evolution of life. In manuscript 3, I investigated the role of oxalate in promoting the nucleation of 2:1 silicate layers of saponite within the low-charge, smectite-like interlayers of rectorite. This study was aimed to test the intercalating hypothesis of Weiss et al. (1969) and Weiss (1981), who claimed to have successfully proven the synthesis of new smectite layers from a solution within the low-charge interlayers of rectorite. Lattice-fringe images show that the oxalate-promoted formation of the new 2:1 layer silicates from the silica gel leads to the alteration and destruction of the rectorite structure. The saponite layers grow independently of any crystallographic orientation given by the rectorite layers. In manuscript 4, XRD, HRTEM and CTEM were used to characterize the clay-mineral separates (2.0-0.5, 0.5-0.1, and <0.1 μm) from argillaceous rocks taken at increasing depth from two wells, North Ben Nevis (NBN) P-93 (2025 m, 2730 m) and Adolphus (AD) D-50 (2035 m, 3135 m) in the Jeanne d'Arc Basin, offshore Newfoundland, in order to understand the diagenetic changes of the 2:1 clay minerals that constitute the smectite to illite (S→I) reaction during progressive burial. Lattice-fringe images of clay minerals in ultrathin sections treated with nC=18 cations show the multiphase nature of the clay-mineral assemblages (e.g., smectite-group minerals, expandable and non-expandable illite, vermiculite) in all size fractions. Conventional TEM images of Pt-C replicas show a change in particle morphology with increasing depth of burial. Irregular, flake-like particles dominate in NBN P-93 at 2025 m and AD D-50 at 2035 m, whereas at greater depths (NBN P-93 at 2730 m and AD D-50 at 3135 m), a larger proportion of lath-like or equidimensional particles are observed. The diagenetic evolution of S→I in the investigated depth interval of the Jeanne d'Arc Basin should be considered as a sequence of multiple discrete 2:1 clay-mineral phases that dissolve and crystallize from solution in overlapping zones of burial depth and not as a single, continuous and progressive reaction-series, as conventionally assumed.Des argiles naturelles et synthétiques provenant de divers milieux géologiques ont été caractérisées par diffraction X et par microscopie électronique en transmission conventionnelle sur répliques Pt-C, et par imagerie à haute résolution sur sections ultraminces.Dans le premier manuscrit, l'effet du traitement avec des cations octadécylammoniac (nC = 18) sur des échantillons d'illite et d'argiles gonflables de type 2:1 (smectites, vermiculite et rectorite) dont la charge des feuillets est variable a été étudié afin de mieux comprendre l'expansion de leur espace interfoliaire. L'imagerie haute résolution de section ultraminces d'argiles de type 2:1 démontre que ce traitement révèle des détails sur la distribution et l'hétérogénéité des charges de leurs feuillets qui échappent aux techniques conventionnelles de préparation de ces minéraux.Dans le deuxième manuscrit, l'effet catalytique de l'oxalate sur la cristallisation de la saponite à 60°C et à pression ambiante est évalué. L'expansion de la saponite néoformée, après son traitement avec les cations nC = 18, est également étudiée en microscopie électronique par transmission à haute résolution. Les feuillets de saponite se répliquent par polymérisation catalysée par une matrice bidimensionnelle et transmettent la distribution de leur charge d'un feuillet à l'autre, une observation aux répercussions importantes sur l'hypothèse d'une origine abiotique de la vie. L'effet catalytique de molécules organiques polaires sur la néoformation d'argiles aurait pu jouer un rôle chez les chondrites carbonées et lors du dégazage de l'atmosphère terrestre précoce, et ainsi contribuer à l'apparition de la vie sur Terre.Dans le troisième manuscrit, j'ai étudié le rôle de l'oxalate dans la nucléation de la saponite, une argile 2:1, à partir de smectite à faible charge interstratifiée dans la rectorite. Ceci fournit un test de l'hypothèse d'intercalation de Weiss et al. (1969) et de Weiss (1981). Ces auteurs ont dit avoir observé la synthèse de smectite à partir de solution au sein de l'espace interfoliaire à faible charge de la rectorite. L'imagerie de franges réticulaires indique toutefois que la néoformation de cristallites de saponite à partir d'un gel de silice, favorisée par la présence d'oxalate, détruit la structure de type 2:1 de la rectorite. Les couches de saponite croissent de façon indépendante de l'orientation cristallographique des couches de rectorite.Dans le quatrième manuscrit, la diffraction X et la microscopie électronique par transmission ont servi à caractériser les fractions concentrées de minéraux argileux (2.0-0.5, 0.5-0.1, et <0.1 μm) à diverses profondeur dans deux puits, North Ben Nevis (NBN) P–93 (2025 m, 2730 m) et Adolphus (AD) D–50 (2035 m, 3135 m), dans le but de mieux comprendre les modifications diagénétiques au cours de l'illitisation de la smectite (S→I) pendant l'enfouissement progressif du bassin Jeanne d'Arc, au large de Terre-Neuve. Les images à haute résolution de franges réticulaires d'argiles traitées avec des cations nC = 18 démontrent la présence de phases multiples (par exemple, smectites aux charges de feuillet faible à forte, illites gonflable ou non, vermiculite) dans toutes les fractions granulométriques. Les images conventionnelles de répliques Pt-C illustrent un changement morphologique progressif avec la profondeur d'enfouissement. Des particules irrégulières et en paillettes prédominent à 2025 m (puits NBN P-93) et à 2035 m (AD D-50), tandis qu'à plus grande profondeur (NBN P-93 à 2730 m, AD D-50 à 3135 m) la proportion de particules en lamelles ou équidimensionnelles augmente. L'évolution diagénétique S→I en fonction de la profondeur du bassin Jeanne d'Arc procède par la dissolution et la croissance en solution de phases minérales 2:1 multiples et distinctes sur des intervalles de profondeur qui se chevauchent, plutôt qu'en une série de réactions progressives et continues telle qu'on les conçoit habituellement.
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Harris, Peter John. "Preparation and characterisation of light emitting porous semiconductors." Thesis, De Montfort University, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.391080.
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Brittin, Mark. "Analytical and morphological studies of polymer-stabilised liquid crystals." Thesis, University of Reading, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.297785.
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Bowers, Cynthia Thomason. "Transmission Electron Microscopy Analysis of Silicon-Doped Beta-Gallium Oxide Films Grown by Pulsed Laser Deposition." Wright State University / OhioLINK, 2019. http://rave.ohiolink.edu/etdc/view?acc_num=wright1580120635333744.
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Aborass, Marwa A. EL-Mehde. "Effect of diamond-like carbon coating on implant drill wear during implant site preparation." University of the Western Cape, 2017. http://hdl.handle.net/11394/6306.
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Magister Chirurgiae DentiumDental implants are artificial fixtures that are surgically inserted into the jaws to replace missing teeth. The success of dental implant treatment is dependent on achieving successful osseointegration (Branemark et al. 2001). Drills used for implant site preparation are made of different materials such as stainless steel (SS), zirconia and ceramic. Most of them do not have sufficient cutting efficiency and wear resistance (Oliveira et al. 2012). Recently diamond-like carbon coating (DLC) has been added as a drill coating to increase the cutting efficiency, increase wear resistance and drill hardness (Batista Mends et al. 2014).
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Ertan, Salih. "Preparation And Characterization Of Carbon Supported Platinum Nanocatalysts With Different Surfactants For C1 To C3 Alcohol Oxidations." Master's thesis, METU, 2011. http://etd.lib.metu.edu.tr/upload/12613623/index.pdf.
Full textAbstract:
In this thesis, carbon supported platinum nanoparticles have been prepared by using PtCl4 as a starting material and 1-octanethiol, 1-decanethiol, 1-dodecanethiol and 1-hexadecanethiol as surfactants for methanol, ethanol and 2-propanol oxidation reactions. The structure, particle sizes and surface morphologies of the platinum were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM) and transmission electron microscopy (TEM). XRD and TEM results indicate that all prepared catalysts have a face centered cubic structure and are homogeneously dispersed on the carbon support with a narrow size distribution (2.0 to 1.3 nm). X-ray photoelectron spectra of the catalysts were examined and it was found that platinum has two different oxidation state, Pt (0) and Pt (IV), oxygen and sulfur compounds are H2Oads and OHads, bounded and unbounded thiols. The electrochemical and electrocatalytic properties of those catalysts were investigated towards C1 to C3 alcohol oxidations by cyclic voltammetry (CV) and chronoamperometry (CA). The highest electrocatalytic activity was obtained from catalyst I which was prepared with 1-octanethiol. This may be attributed to decrease in the ratio of bounded to unbounded thiol species and increase in Pt (0)/Pt (IV), H2Oads/OHads ratios, electrochemical surface area, CO tolerance and percent platinum utility.
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Sen, Fatih. "The Preparation And Analysis Of New Carbon Supported Pt And Pt+second Metal Nanoparticles Catalysts For Direct Methanol Fuel Cells." Phd thesis, METU, 2012. http://etd.lib.metu.edu.tr/upload/12614728/index.pdf.
Full textAbstract:
In this thesis, firstly, carbon-supported platinum nanoparticle catalysts have been prepared by using PtCl4 and H2PtCl6 as starting materials and 1-hexanethiol, and tert-octanethiol, as surfactants for the first time. Secondly, these prepared catalysts were heated to 200 °C, 300 °
C, and 400 °
C for 4 h under argon gas. Lastly, PtRu/C catalysts, which have different atomic percent ratios of Pt and Ru (Pt/Ru: 0.8, 2.1 and 3.5), were prepared using PtCl4 and RuCl3 as starting materials and tert-octanethiol as a surfactant. Each was characterized by X-ray diffraction, transmission electron microscopy, energy dispersive analysis, X-ray photoelectron spectroscopy, cyclic voltammetry, and elemental analysis, and their activities were determined toward the methanol oxidation reaction. It has been found that all prepared catalysts are more active toward methanol oxidation reaction compared to the commercial catalysts. It was also found that increasing the temperature during the heat treatment process results in an enlargement of platinum particle size and a decrease in catalytic activity in the methanol oxidation reaction. Transmission electron microscopy shows that platinum nanoparticles are homogeneously dispersed on the carbon support and exhibited a narrow size distribution with an average particle size of about 2-3 nm in diameter. X-ray photoelectron spectra of all catalysts indicated that most of the platinum nanoparticles (>
70 %) have an oxidation state of zero and rest (<
30 %) have a +4 oxidation state with (Pt 4f7/2) binding energies of 71.2-72.2 and 74.3-75.5 eV, respectively.
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Williams, Shara Carol. "Patterning nanocrystals using DNA." Berkeley, Calif. : Oak Ridge, Tenn. : Lawrence Berkeley National Laboratory ; distributed by the Office of Scientific and Technical Information, U.S. Dept. of Energy, 2003. http://www.osti.gov/servlets/purl/825530-PLgXcs/native/.
Full textAbstract:
Thesis (Ph.D.); Submitted to the University of California at Berkeley, Berkeley, CA (US); 1 Sep 2003.Published through the Information Bridge: DOE Scientific and Technical Information. "LBNL--55024" Williams, Shara Carol. National Institutes of Health (US) 09/01/2003. Report is also available in paper and microfiche from NTIS.
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Fiedler, Holger. "Preparation and characterization of Carbon Nanotube based vertical interconnections for integrated circuits: Preparation and characterization of Carbon Nanotube based verticalinterconnections for integrated circuits." Doctoral thesis, Universitätsverlag der Technischen Universität Chemnitz, 2013. https://monarch.qucosa.de/id/qucosa%3A20091.
Full textAbstract:
(ULSI) causes an increase of the resistance of the wiring system by increased scattering of electrons at side walls and grain boundaries in the state of the art Cu technology, which increases the RC delay of the interconnect system and thus degrades the performance of the device. The outstanding properties of carbon nanotubes (CNT) such as a large mean free path, a high thermal conductance and a large resistance against electromigration make them an ideal candidate to replace Cu in future feature nodes. The present thesis contributes to the preparation and properties of CNT based vertical interconnections (vias). In addition, all processes applied during the fabrication are compatible to ULSI and an interface between CNT based vias and a Cu metallization is studied. The methodology for the evaluation of CNT based vias is improved; it is highlighted that by measuring the resistance of one multiwall CNT and taking into account the CNT density, the performance of the CNT based vias can be predicted accurately. This provides the means for a systematic evaluation of different integration procedures and materials. The lowest contact resistance is obtained for carbide forming metals, as long as oxidation during the integration is avoided. Even though metal-nitrides exhibit an enhanced contact resistance, they are recommended to be used at the bottom metallization in order to minimize the oxidation of the metal-CNT contact during subsequent processing steps. Overall a ranking for the materials from the lowest to the highest contact resistance is obtained: Ta < Ti < TaN < TiN « TiO2 « Ta2O5 Furthermore the impact of post CNT growth procedures as chemical mechanical planarization, HF treatment and annealing procedures after the CNT based via fabrication are evaluated. The conductance of the incorporated CNTs and the applicable electrical transport regime relative to the CNT quality and the CNT length is discussed. In addition, a strong correlation between the temperature coefficient of resistance and the initial resistance of the CNT based vias at room temperature has been observed.Die kontinuierliche Miniaturisierung der charakteristischen Abmessungen in hochintegrierten Schaltungen (ULSI) verursacht einen Anstieg des Widerstandes im Zuleitungssystem aufgrund der erhöhten Streuung von Elektronen an Seitenwänden und Korngrenzen in der Cu-Technologie, wodurch die Verzögerungszeit des Zuleitungssystems ansteigt. Die herausragenden Eigenschaften von Kohlenstoffnanoröhren (CNT), wie eine große mittlere freie Weglänge, hohe thermische Leitfähigkeit und eine starke Resistenz gegenüber Elektromigration machen diese zu einem idealen Kandidaten, um Cu in zukünftigen Technologiegenerationen zu ersetzen. Die vorliegende Arbeit beschreibt die Herstellung und daraus resultierenden Eigenschaften von Zwischenebenenkontakten (Vias) basierend auf CNTs. Alle verwendeten Prozessierungsschritte sind kompatibel mit der Herstellung von hochintegrierten Schaltkreisen und eine Schnittstelle zwischen den CNT Vias und einer Cu-Metallisierung ist vorhanden. Insbesondere das Verfahren zur Evaluierung von CNT Vias wurde durch den Einsatz verschiedener Methoden verbessert. Insbesondere soll hervorgehoben werden, dass durch die Messung des Widerstandes eines einzelnen CNTs, bei bekannter CNT Dichte, der Via Widerstand sehr genau vorausgesagt werden kann. Dies ermöglicht eine systematische Untersuchung des Einflusses der verschiedenen Prozessschritte und der darin verwendeten Materialien auf den Via Widerstand. Der niedrigste Kontaktwiderstand wird für Karbidformierende Metalle erreicht, solange Oxidationsprozesse ausgeschlossen werden können. Obwohl Metallnitride einen höheren Kontaktwiderstand aufweisen, sind diese für die Unterseitenmetallisierung zu empfehlen, da dadurch die Oxidation der leitfähigen Schicht minimiert wird. Insgesamt kann eine Reihenfolge beginnend mit dem niedrigsten zum höchsten Kontaktwiderstand aufgestellt werden: Ta < Ti < TaN < TiN « TiO2 « Ta2O5 Desweiteren wurde der Einfluss von Verfahren nach dem CNTWachstum wie die chemischmechanische Planarisierung, eine HF Behandlung und einer Temperaturbehandlung evaluiert, sowie deren Einfluss auf die elektrischen Parameter des Vias untersucht. Die Leitfähigkeit der integrierten CNTs und die daraus resultierenden elektrischen Transporteigenschaften in Abhängigkeit der CNT Qualität und Länge werden besprochen. Ebenso wird die starke Korrelation zwischen dem Temperaturkoeffizienten des elektrischen Widerstandes und des Ausgangswiderstandes der CNT basierten Vias bei Raumtemperatur diskutiert.
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Fiedler, Holger. "Preparation and characterization of Carbon Nanotube based vertical interconnections for integrated circuits." Doctoral thesis, Universitätsbibliothek Chemnitz, 2014. http://nbn-resolving.de/urn:nbn:de:bsz:ch1-qucosa-149474.
Full textAbstract:
(ULSI) causes an increase of the resistance of the wiring system by increased scattering of electrons at side walls and grain boundaries in the state of the art Cu technology, which increases the RC delay of the interconnect system and thus degrades the performance of the device. The outstanding properties of carbon nanotubes (CNT) such as a large mean free path, a high thermal conductance and a large resistance against electromigration make them an ideal candidate to replace Cu in future feature nodes. The present thesis contributes to the preparation and properties of CNT based vertical interconnections (vias). In addition, all processes applied during the fabrication are compatible to ULSI and an interface between CNT based vias and a Cu metallization is studied. The methodology for the evaluation of CNT based vias is improved; it is highlighted that by measuring the resistance of one multiwall CNT and taking into account the CNT density, the performance of the CNT based vias can be predicted accurately. This provides the means for a systematic evaluation of different integration procedures and materials. The lowest contact resistance is obtained for carbide forming metals, as long as oxidation during the integration is avoided. Even though metal-nitrides exhibit an enhanced contact resistance, they are recommended to be used at the bottom metallization in order to minimize the oxidation of the metal-CNT contact during subsequent processing steps. Overall a ranking for the materials from the lowest to the highest contact resistance is obtained: Ta < Ti < TaN < TiN « TiO2 « Ta2O5 Furthermore the impact of post CNT growth procedures as chemical mechanical planarization, HF treatment and annealing procedures after the CNT based via fabrication are evaluated. The conductance of the incorporated CNTs and the applicable electrical transport regime relative to the CNT quality and the CNT length is discussed. In addition, a strong correlation between the temperature coefficient of resistance and the initial resistance of the CNT based vias at room temperature has been observedDie kontinuierliche Miniaturisierung der charakteristischen Abmessungen in hochintegrierten Schaltungen (ULSI) verursacht einen Anstieg des Widerstandes im Zuleitungssystem aufgrund der erhöhten Streuung von Elektronen an Seitenwänden und Korngrenzen in der Cu-Technologie, wodurch die Verzögerungszeit des Zuleitungssystems ansteigt. Die herausragenden Eigenschaften von Kohlenstoffnanoröhren (CNT), wie eine große mittlere freie Weglänge, hohe thermische Leitfähigkeit und eine starke Resistenz gegenüber Elektromigration machen diese zu einem idealen Kandidaten, um Cu in zukünftigen Technologiegenerationen zu ersetzen. Die vorliegende Arbeit beschreibt die Herstellung und daraus resultierenden Eigenschaften von Zwischenebenenkontakten (Vias) basierend auf CNTs. Alle verwendeten Prozessierungsschritte sind kompatibel mit der Herstellung von hochintegrierten Schaltkreisen und eine Schnittstelle zwischen den CNT Vias und einer Cu-Metallisierung ist vorhanden. Insbesondere das Verfahren zur Evaluierung von CNT Vias wurde durch den Einsatz verschiedener Methoden verbessert. Insbesondere soll hervorgehoben werden, dass durch die Messung des Widerstandes eines einzelnen CNTs, bei bekannter CNT Dichte, der Via Widerstand sehr genau vorausgesagt werden kann. Dies ermöglicht eine systematische Untersuchung des Einflusses der verschiedenen Prozessschritte und der darin verwendeten Materialien auf den Via Widerstand. Der niedrigste Kontaktwiderstand wird für Karbidformierende Metalle erreicht, solange Oxidationsprozesse ausgeschlossen werden können. Obwohl Metallnitride einen höheren Kontaktwiderstand aufweisen, sind diese für die Unterseitenmetallisierung zu empfehlen, da dadurch die Oxidation der leitfähigen Schicht minimiert wird. Insgesamt kann eine Reihenfolge beginnend mit dem niedrigsten zum höchsten Kontaktwiderstand aufgestellt werden: Ta < Ti < TaN < TiN « TiO2 « Ta2O5 Desweiteren wurde der Einfluss von Verfahren nach dem CNTWachstum wie die chemischmechanische Planarisierung, eine HF Behandlung und einer Temperaturbehandlung evaluiert, sowie deren Einfluss auf die elektrischen Parameter des Vias untersucht. Die Leitfähigkeit der integrierten CNTs und die daraus resultierenden elektrischen Transporteigenschaften in Abhängigkeit der CNT Qualität und Länge werden besprochen. Ebenso wird die starke Korrelation zwischen dem Temperaturkoeffizienten des elektrischen Widerstandes und des Ausgangswiderstandes der CNT basierten Vias bei Raumtemperatur diskutiert
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Orbegoso, Flores Victor Humberto [UNESP]. "Avaliação in vitro da microinfiltração marginal e análise da fenda marginal cervical através da microscopia eletrônica de varredura, em restaurações de classe V de resina composta. Efeito dos sistemas adesivos e técnica de preparo cavitário." Universidade Estadual Paulista (UNESP), 2001. http://hdl.handle.net/11449/101403.
Full textAbstract:
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orbegosoflores_vh_dr_arafo.pdf: 838219 bytes, checksum: 839e8fda83a571e900cce3e586d69abb (MD5)O objetivo deste trabalho foi avaliar a formação de fendas marginais cervicais através da microscopia eletrônica de varredura, assim como, a microinfiltração marginal em preparos de classe V. foram utilizadas duas técnicas de preparo: P1 utilizando fresa carbide no 245 e P2 que utilizou o jato de ar abrasivo Mach 4.0 (80psi de pressão, 27 æm de tamanho de partícula). O tamanho das cavidades foi padronizado com 1,5 mm de profundidade, 2,0 mm de altura e 3,0 mm de largura. Os materiais utilizados foram: G1 -Optibond solo Plus, G2 - Prime & BondNT e G3 - Scotchbond Multiuso Plus (grupo controle), a resina composta Point 4 utilizada para restaurar as cavidades foi padronizada para todas as restaurações. Foram utilizados 42 dentes molares hígidos divididos em 3 grupos de 14 cada, utilizando a face vestibular e lingual sendo que os preparos mostraram a margem oclusal em esmalte e a margem cervical em cemento/dentina. Após as restaurações serem confeccionadas foram armazenadas em água deionizada durante 24 horas, para posteriormente realizar os procedimentos de acabamento e polimento, a seguir os dentes foram isolados com araldite e esmalte para unha e submetidos a testes de ciclagem térmico (400 ciclos)e imediatamente imersos numa solução de nitrato de prata, durante 2 horas, removidos, lavados e colocados numa solução fotoreveladora durante 16 horas. Nessas condições os dentes foram limpos e seccionados no sentido mésio/distal obtendo duas metades as quais por sua vez foram seccionadas no sentido vestíbulo lingual dividindo as restaurações pela metade. Assim, uma metade da restauração foi avaliada através da lupa esteroscópica para observar a microinfiltração e a outra metade preparada e metalizada para ser avaliada através da microscopia eletrônica de varredura. A análise estatística aplicada aos resultados permite concluir que... .
The aim of this study was to evaluate the formation of cervical gap with SEM, and the marginal microleakage in cavities class V. There were used two techniques for the preparations: P1 using a carbide # 245 and P2 using abrasive air Mach 4.0 (80 psi of preasure, 27nm measurement of the particle). The measurements of the cavities were standardized in 1.5mm of deepness, 2,0mm of highness and 3,0mm of lengthiness. The materials used were: G1 Optibond Solo Plus, G2 Prime & Bond NT and G3 Scotchbond Multiuso Plus (control group), it was used the composite Point 4 as the restorative material for all cavities. Forty-two healthy molars, divided in three groups of 14 each one, were used. Cavities were prepared in the buccal and lingual faces, its occlusal margin was in enamel and its cervical margin was in dentin/cement. After that finishing and polishing was made. Teeth were isolated with analdite and nail varnish and thermocycled (400 times). The preparations were dyed with silver nitrate for two hours. Preparations were stored in a photo developing solution for 16 hours. After that time teeth were cleaned and cut (buccal/lingual) Half of the preparation was observed in a stereoscopic microscope and the other half in a SEM. Results: 1.Preparations with abrasive air had a bigger gap; 2.Adhesive systems do not eliminate the formation of gaps; 3.Best results were found in the group prepared with bur and the adhesive Optibond Solo Plus, with a cervical gap 0,84nm, and in the other hand Scotchbond Multiuso Plus showed marginal gaps of 6,36nm; 4.In the occlusal margin Optibond Solo Plus had more microleakage tha Scotchbond Multiuso Plus and Prime & Bond NT.; 5. In the cervical margin, Optibond Solo Plus had good behavior controlling the marginal microleakage, compared with Scotchbond Multiuso Plus and Prime & Bond that had similar leakage between... (Complete abstract, click electronic address below).
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Tchana, Nkonta Daniella Vashti. "Caractérisation de l'effet de traitement de nanocristallisation superficielle (SMAT) sur un alliage CoCrMo." Thesis, Troyes, 2017. http://www.theses.fr/2017TROY0005/document.
Full textAbstract:
Ce travail a pour objectif d’évaluer le comportement à l’usure de pièces en CoCrMo utilisé dans l’orthopédie. Le procédé de nanocristallisation superficielle SMAT (Surface Mechanical Attrition Treatment) couplé à un polissage biomédical a été mis en œuvre dans cette étude pour améliorer les propriétés mécaniques, tribocorrosives d’un alliage CoCrMo. Dans un premier temps, une optimisation des paramètres SMAT sur un alliage CoCrMo a été réalisée. Différentes techniques de finition de surface ont ensuite été étudiées afin d’obtenir un état de surface acceptable pour des implants orthopédiques. Des techniques de caractérisation microstructurale ont alors été mises en œuvre sur des échantillons SMATés et polis : microscopie électronique à balayage et transmission (MEB ; MET), diffraction des électrons rétrodiffusés (EBSD), diffraction de kikuchi en transmission (TKD) et diffraction des rayons X (DRX). Les résultats obtenus ont montré que le traitement SMAT peut créer un raffinement des grains en surface de l’alliage CoCrMo avec notamment la présence de nano-grains en extrême surface. Des mesures d’indentation ainsi que des essais par la méthode du trou incrémental ont été effectués. Une augmentation de plus de 30% de la dureté a ainsi été observée après SMAT ainsi que la génération de contraintes résiduelles superficielles de compression. Les propriétés tribocorrosives de l’alliage CoCrMo ont également été étudiées par des essais d’usure par pion disque, scratch tests et des essais électrochimiques avant et après SMATThis aims of this work is to evaluate the wear behavior of CoCrMo parts used in orthopedics. The Surface Mechanical Attrition Treatment (SMAT) method coupled with biomedical polishing has been used in this study to improve the mechanical and tribocorrosive properties of a CoCrMo alloy. In a first step, an optimization of the SMAT parameters on a CoCrMo alloy was carried out. Different surface finishing techniques were then studied to obtain an acceptable surface finish for orthopedic implants. Microstructural characterization techniques were then applied on SMATed and polished samples: scanning and transmission electron microscopy (SEM, MET), backscattered electron diffraction (EBSD), transmission kikuchi diffraction (TKD), and ray diffraction X (XRD). The results obtained showed that the SMAT treatment can create a refinement of the surface grains of the CoCrMo alloy with the presence of nano-grains in the extreme surface. Indentation measurements as well as incremental hole tests were performed. An increase of more than 30% of the hardness was observed after SMAT as well as the generation of residual surface compressive stresses. The tribocorrosive properties of the CoCrMo alloy were also studied by disk wear tests, scratch tests, and electrochemical tests before and after SMAT
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Vykydal, Václav. "Radiační poškození vzorků v nízkovoltové transmisní elektronové mikroskopii." Master's thesis, Vysoké učení technické v Brně. Fakulta elektrotechniky a komunikačních technologií, 2019. http://www.nusl.cz/ntk/nusl-400992.
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This thesis is focused on Radiation damage of samples in low-voltage transmission electron microscopy. In thesis is general description of transmission electron microscopy and their important parts. There is described how samples are damaged by primary electron beam and how samples for transmission electron microscopy are prepared and which degradation occurs from the point of view materials of sample and time dose of electrons from primary electron beam.
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Mühle, Uwe. "Spezielle Anwendungen der Transmissionselektronenmikroskopie in der Siliziumhalbleiterindustrie." Doctoral thesis, Technische Universitaet Bergakademie Freiberg Universitaetsbibliothek "Georgius Agricola", 2015. http://nbn-resolving.de/urn:nbn:de:bsz:105-qucosa-160699.
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Die außerordentlichen Steigerungen der Funktionalität und Produktivität in der Halbleiterindustrie sind zum wesentlichen Teil auf eine Verkleinerung der Strukturdetails auf einer logarithmischen Skala über die letzten Jahrzehnte zurückzuführen. Sowohl zur Kontrolle des Fertigungsergebnisses als auch zur Klärung von Fehlerursachen ist die Nutzung transmissionselektronenmikroskopischer Methoden unabdingbar. Für die Zielpräparation von Halbleiterstrukturen sind Techniken unter Nutzung der Focused Ion Beam Geräte etabliert, die je nach der konkreten Aufgabenstellung variiert werden. Die Abbildung von Strukturdetails mit Abmessungen von wenigen Nanometern erfordert die Anwendung unterschiedlicher Kontrastmechanismen. Die Ergänzung der Abbildung durch die analytischen Techniken der energiedispersiven Röntgenmikroanalyse und der Elektronenenergieverlustanalyse ist ein wertvolles Werkzeug bei der Klärung von Fehlerursachen oder bei prozesstechnischen Fragestellungen. Die Nutzung der Rastertransmissionselektronenmikroskopie erlaubt die unmittelbare Kombination von Abbildung und Elementanalyse. Die lokale Verteilung von Dotierstoffen als wesentliche Grundlage für die Funktion von Bauelementen in der Halbleiterindustrie ist nur über ihre Auswirkung auf die Phase der transmittierten Elektronenwelle nachweisbar. Mittels Elektronenholographie kann dieser Einfluss gemessen werden und das Prozessergebnis von Implantationen dargestellt werden. Für die Charakterisierung von Details, die kleiner als die Probendicken sind, die im TEM genutzt werden, ist die Anwendung der Elektronentomographie ein geeignetes Werkzeug. Dazu sind spezielle Präparations- und Abbildungsstrategien erforderlichThe strong improvements in functionality and productivity in the semiconductor industry are mostly a result of the decrease of structural details on a logarithmic scale during the last decades. The monitoring of the production process, as well as failure analyses, utilize methods of transmission electron microscopy. For targeted preparations of semiconductor structures, techniques based on focused ion beams are established, with adaptions to the current task. The imaging of structural details with dimensions of a few nanometers requires the application of different contrast techniques, depending on the detailed request. Different opportunities of elemental analysis, such as energy dispersive X-ray analysis or electron energy loss analysis, deliver additional information about the chemical composition and binding states on a nanoscale. The use of scanning transmission electron microscopy enables a direct combination of imaging and elemental analysis. The local distribution of dopants, as one of the major basics for the function of semiconductor devices, can be observed via the phase shift of the transmitted electron wave only. This influence requires the application of electron holography, a technique which enables the visualization of the process result of implantations or diffusion processes. The characterization of details which are smaller than the thickness of a TEM-sample is enabled through the use of electron tomography. This technique requires special strategies for preparation and imaging and delivers a 3D-dataset, describing the structure
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Oliveira, Helder Fernandes de. "Potencial de sanificação de instrumentos reciprocantes associados com hipoclorito de sódio 2,5% e vinagre de maçã em canais radiculares infectados." Universidade Federal de Goiás, 2016. http://repositorio.bc.ufg.br/tede/handle/tede/6527.
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Objetive: Evaluate the antibacterial effect of reciprocating systems associated with sodium hypochlorite 2.5% and apple vinegar in infected root canals. Methods: Fifty human anterior teeth uniradicular were prepared, inoculated with E. faecalis and examined after sixty days. The teeth were randomly assigned to five groups: (1. WaveOne® 40.08; 2. Reciproc® 40.06; 3. Unicorne® 40.06; 4 and 5 positive and negative controls. For each experimental group (n = 10), five specimens were irrigated with sodium hypochlorite 2.5%, and five with apple vinegar. Bacterial growth was analyzed using turbidity of culture medium followed by UV spectrophotometry. The cleaning of dentinal walls was analyzed by scanning electronic microscopy (SEM). Results: All groups showed a significant reduction of the optimal density of the culture medium after the root canal preparation (p<0,05). No sanitizing strategy promoted the complete elimination of E. faecalis. In the analysis of cleaning the root surface, it was found that in none of the groups showed complete removal of debris, not being verified significant differences indifferent to analyzed thirds (p> 0.05). Conclusion: The reciprocating instruments (WaveOne®, Reciproc® and Unicorne®) and irrigating sodium hypochlorite solution 2.5% and apple cider vinegar have not been effective in eliminating E. faecalis complete in infected root canals.
Objetivo: Avaliar o efeito antibacteriano de sistemas reciprocantes associados ao hipoclorito de sódio 2,5% e ao vinagre de maça em canais radiculares infectados. Materiais e métodos: Cinquenta dentes humanos unirradiculares extraídos foram preparados, inoculados com Enterococcus faecalis e incubados a 37°C por sessenta dias. Os espécimes foram aleatoriamente divididos em 05 grupos sendo três experimentais e dois controles (1. WaveOne® 40.08; 2. Reciproc® 40.06; 3. Unicone® 40.06; 4. Controle positivo; Controle negativo). Para cada grupo experimental, cinco espécimes foram irrigados com hipoclorito de sódio 2,5% e cinco com vinagre de maçã. O crescimento bacteriano foi analisado pela turbidez do meio de cultura e espectrofotometria UV. A limpeza das paredes dentinárias foi analisada por microscopia eletrônica de varredura. Resultados: Todos os grupos mostraram redução significativa da densidade óptica do meio de cultura após o preparo do canal radicular (p<0,05). Nenhuma estratégia de sanificação promoveu a eliminação completa do E. faecalis. Na análise da limpeza da superfície radicular, foi verificado que, em nenhum dos grupos houve a remoção completa dos debris, não sendo verificadas diferenças significativas indiferente aos terços analisados (p>0,05). Conclusão: Os instrumentos reciprocantes (WaveOne®, Reciproc® e Unicorne®) e as soluções irrigadoras hipoclorito de sódio 2,5% e vinagre de maça não foram efetivos na completa eliminação do E. faecalis em canais radiculares infectados.
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Orbegoso, Flores Victor Humberto. "Avaliação "in vitro" da microinfiltração marginal e análise da fenda marginal cervical através da microscopia eletrônica de varredura, em restaurações de classe V de resina composta. Efeito dos sistemas adesivos e técnica de preparo cavitário /." Araraquara : [s.n.], 2001. http://hdl.handle.net/11449/101403.
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Orientador: Marcelo Ferrarezi de AndradeBanca: Marcos Ribeiro Moysés
Banca: Alberto Magno Gonçalves
Banca: Sillas Luiz Lordelo Duarte Júnior
Banca: Sizenando de Toledo Porto Neto
Resumo: O objetivo deste trabalho foi avaliar a formação de fendas marginais cervicais através da microscopia eletrônica de varredura, assim como, a microinfiltração marginal em preparos de classe V. foram utilizadas duas técnicas de preparo: P1 utilizando fresa carbide no 245 e P2 que utilizou o jato de ar abrasivo Mach 4.0 (80psi de pressão, 27 æm de tamanho de partícula). O tamanho das cavidades foi padronizado com 1,5 mm de profundidade, 2,0 mm de altura e 3,0 mm de largura. Os materiais utilizados foram: G1 -Optibond solo Plus, G2 - Prime & BondNT e G3 - Scotchbond Multiuso Plus (grupo controle), a resina composta Point 4 utilizada para restaurar as cavidades foi padronizada para todas as restaurações. Foram utilizados 42 dentes molares hígidos divididos em 3 grupos de 14 cada, utilizando a face vestibular e lingual sendo que os preparos mostraram a margem oclusal em esmalte e a margem cervical em cemento/dentina. Após as restaurações serem confeccionadas foram armazenadas em água deionizada durante 24 horas, para posteriormente realizar os procedimentos de acabamento e polimento, a seguir os dentes foram isolados com araldite e esmalte para unha e submetidos a testes de ciclagem térmico (400 ciclos)e imediatamente imersos numa solução de nitrato de prata, durante 2 horas, removidos, lavados e colocados numa solução fotoreveladora durante 16 horas. Nessas condições os dentes foram limpos e seccionados no sentido mésio/distal obtendo duas metades as quais por sua vez foram seccionadas no sentido vestíbulo lingual dividindo as restaurações pela metade. Assim, uma metade da restauração foi avaliada através da lupa esteroscópica para observar a microinfiltração e a outra metade preparada e metalizada para ser avaliada através da microscopia eletrônica de varredura. A análise estatística aplicada aos resultados permite concluir que... (Resumo completo, clicar acesso eletrônico abaixo).
Abstract: The aim of this study was to evaluate the formation of cervical gap with SEM, and the marginal microleakage in cavities class V. There were used two techniques for the preparations: P1 using a carbide # 245 and P2 using abrasive air Mach 4.0 (80 psi of preasure, 27nm measurement of the particle). The measurements of the cavities were standardized in 1.5mm of deepness, 2,0mm of highness and 3,0mm of lengthiness. The materials used were: G1 Optibond Solo Plus, G2 Prime & Bond NT and G3 Scotchbond Multiuso Plus (control group), it was used the composite Point 4 as the restorative material for all cavities. Forty-two healthy molars, divided in three groups of 14 each one, were used. Cavities were prepared in the buccal and lingual faces, its occlusal margin was in enamel and its cervical margin was in dentin/cement. After that finishing and polishing was made. Teeth were isolated with analdite and nail varnish and thermocycled (400 times). The preparations were dyed with "silver nitrate" for two hours. Preparations were stored in a photo developing solution for 16 hours. After that time teeth were cleaned and cut (buccal/lingual) Half of the preparation was observed in a stereoscopic microscope and the other half in a SEM. Results: 1.Preparations with abrasive air had a bigger gap; 2.Adhesive systems do not eliminate the formation of gaps; 3.Best results were found in the group prepared with bur and the adhesive Optibond Solo Plus, with a cervical gap 0,84nm, and in the other hand Scotchbond Multiuso Plus showed marginal gaps of 6,36nm; 4.In the occlusal margin Optibond Solo Plus had more microleakage tha Scotchbond Multiuso Plus and Prime & Bond NT.; 5. In the cervical margin, Optibond Solo Plus had good behavior controlling the marginal microleakage, compared with Scotchbond Multiuso Plus and Prime & Bond that had similar leakage between... (Complete abstract, click electronic address below).
Doutor
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Trevelin, Lívia Tosi. "Análise morfológica da dentina irradiada pelo laser de Er:YAG (SSP) com diferentes larguras de pulso." Universidade de São Paulo, 2015. http://www.teses.usp.br/teses/disponiveis/23/23134/tde-15042015-120955/.
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Este estudo se propôs a analisar as características morfológicas da dentina humana irradiada com laser de Er:YAG utilizando diferentes larguras temporal de pulso nos protocolos de preparo cavitário e pré-tratamento da dentina. Foram utilizados 18 molares humanos que foram seccionados no sentido mésio-distal e amelocementário obtendo-se um disco plano de dentina. Em seguida foram lixados com uma sequência decrescentes de lixas para padronizar os espécimes em 2mm de espessura. Os grupos experimentais foram compostos a partir de 2 fatores de variação: 1) indicação clínica - preparo cavitário (E=200mJ/20Hz), e pré-tratamento (E=80mJ/2Hz); e 2) largura temporal de pulso - 50, 300 e 600µs. Assim formaram-se 6 grupos experimentais com (n=3): G1(E=200mJ/20Hz/50µs); G2(E=200mJ/20Hz/300µs); G3(E=200mJ/20Hz/600µs); G4(E=80mJ/2Hz/50µs); G5(E=80mJ/2Hz/300µs); G6(E=80mJ/2Hz/600µs). Os espécimes foram irradiados com o laser de Er:YAG com comprimento de onda de 2,94µm, de modo não contato, com um distância de 7mm do feixe de saída, sob irrigação de 60ml/min de água e 40ml/min de ar. Após a irradiação, os espécimes foram processados e destinados à avaliação descritiva das imagens obtidas em Microscopia Eletrônica de Varredura (MEV), nos diferentes grupos experimentais. A análise morfológica dos grupos irradiados revelou uma superfície irregular, ausência de smear layer que expõe a abertura dos túbulos dentinários, dentina peritubular evidente e, sem indícios de carbonização e derretimento para todos os protocolos utilizados. Os resultados deste estudo in vitro mostraram que a irradiação com o laser de Er:YAG promoveram um padrão morfológico microrretentivo característico de ablação para todos os grupos testados e os grupos G1 e G4, que utilizaram a menor largura temporal de pulso (50 ?s), apresentaram uma superfície mais rugosa quando comparados aos demais grupos. Por fim, podemos concluir que a largura temporal de pulso influência nas características morfológicas da dentina irradiada nas diferentes indicações clínicas testadas, preparo cavitário e pré-tratamento. A menor largura de pulso (50 µs) produz uma morfologia mais irregular quando comparada as maiores larguras de pulsos (300 e 600 µs).This study evaluated the morphological characteristics of Er:YAG laser irradiated dentin using different temporal pulses width on the protocols of cavity preparation and dentin pretreatment. Eighteen human molars were cut longitudinally in a mesiodistal direction and amelocemental junction providing dentin disks. Samples were polished in a decreasing silicon carbide paper to obtain standard 2mm thick disks. The experimental groups were divided by two variables: 1) clinical protocol - cavity preparation (E=200mJ/20Hz) and pretreatment (E=80mJ/2Hz); and 2) temporal pulse width - 50, 300 and 600µs. Therefore, six experimental groups were (n=3): G1(E=200mJ/20Hz/50µs); G2(E=200mJ/20Hz/300µs); G3(E=200mJ/20Hz/600µs); G4(E=80mJ/2Hz/50µs); G5(E=80mJ/2Hz/300µs); and G6(E=80mJ/2Hz/600µs). The samples were irradiated with the Er.YAG laser using wave-length of 2.94µm, in a non contact mode at a focal distance of 7mm from the target point under continuous water spray of 60-40ml/min. After the irradiation, the samples were processed and evaluated by scanning electron microscopic evaluation (SEM). The morphological analysis on the irradiated groups showed an irregular dentin surface, without smear layer, exposed dentinal tubules apertures, evidenced peritubular dentin, without carbonization and melting signs for all groups. A microretentive morphological pattern, characteristic of the ablation process could be observed in all groups. However, groups G1 and G4, that used 50?s of temporal pulse width, presented a greater irregularity when compared to other groups. In conclusion, the temporal pulse width interfere on the morphological characteristic of the irradiated dentin, regardless of clinical protocol, cavity preparation and pretreatment. The shorter the pulse width (50µs), the greater the surface irregularity.
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USSUI, VALTER. "Preparacao e caracterizacao de ceramicas de ZrOsub(2)-Ysub(2)Osub(3)-TiOsub(2) para aplicacoes em celulas a combustivel do tipo oxido solido." reponame:Repositório Institucional do IPEN, 2003. http://repositorio.ipen.br:8080/xmlui/handle/123456789/11081.
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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
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Kili, Koffi Ani. "Preparation, activation, et caracterisation des catalyseurs de metaux de transition associes aux terres rares." Université Louis Pasteur (Strasbourg) (1971-2008), 1988. http://www.theses.fr/1988STR13030.
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Etude de l'interaction entre les terres rares et les metaux de transition en jouant sur le mode d'impregnation, la nature des sels precurseurs des metaux de transition et des lanthanides et traitement thermique d'activation. Etude sur la dispersion et sur l'etat d'oxydation
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Sokol, Norbert. "Segmentace biologických vzorků v obrazech z kryo-elektronového mikroskopu s využitím metod strojového učení." Master's thesis, Vysoké učení technické v Brně. Fakulta elektrotechniky a komunikačních technologií, 2021. http://www.nusl.cz/ntk/nusl-442577.
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Zobrazovanie pomocou kryo-elektrónovej mikroskopie má svoje nezastúpiteľné miesto v analýze viacerých biologických štruktúr. Lokalizácia buniek kultivovaných na mriežke a ich segmentácia voči pozadiu alebo kontaminácii je základom. Spolu s vývojom viacerých metód hlbokého učenia sa podstatne zvýšila úspešnosť úloh sémantickej segmentácie. V tejto práci vyvinieme hlbokú konvolučnú neurónovú sieť pre úlohu sémantickej segmentácie buniek kultivovaných na mriežke. Dátový súbor pre túto prácu bol vytvorený pomocou dual-beam kryo-elektónového mikroskopu vyvinutého spoločnosťou Thermo Fisher Scientific Brno.
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SCHELL, JULIANA. "Investigação de parâmetros hiperfinos dos óxidos semicondutores SnOsub(2) e TiOsub(2) puros e dopados com metais de transição 3d pela espectroscopia de correlação angular gama-gama perturbada." reponame:Repositório Institucional do IPEN, 2015. http://repositorio.ipen.br:8080/xmlui/handle/123456789/23699.
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Tese (Doutorado em Tecnologia Nuclear)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP
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Pariot, Christine. "Implication des ions inorganiques dans la différenciation des fibres chez le lin : approche par microscopie ionique analytique." Rouen, 1994. http://www.theses.fr/1994ROUES021.
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Ce travail est une approche par imagerie ionique analytique de l'implication des ions inorganiques dans la différenciation des fibres chez le lin. Le modèle expérimental est l'hypocotyle de lin. La cartographie semi-quantitative des ions Na+, Ca2+, K+ et Mg2+ a été réalisée par microscopie ionique analytique (MIA). Cette technique a été combinée aux techniques de microscopie photonique et électronique. Ce travail comporte une mise au point méthodologique de la préparation des échantillons végétaux en vue de l'immobilisation des ions diffusibles. Il est réalisé une approche critique des possibilités et des limites des deux méthodes de préparation que nous avons utilisées: la méthode par précipitation au pyroantimoniate et la méthode par cryosubstitution. Ce travail comporte également une analyse critique des images, par microscopie ionique à balayage, des distributions ioniques dans l'hypocotyle de lin et propose quelques améliorations instrumentales. La mise en évidence d'une augmentation du rapport des concentrations Na/Ca, d'une structuration dans la distribution du sodium au sein de la paroi secondaire des fibres ainsi que les effets marqués sur le développement des fibres, d'une carence en sodium suggèrent que cet ion pourrait être impliqué dans la différenciation des fibres chez le lin. L'étude, par radiographie par capture neutronique, de la microlocalisation du bore dans les différents tissus de l'hypocotyle suggère aussi un rôle possible de cet élément dans la cohésion du tissu fibreux
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Bernardi, Cécile. "Analyse haute résolution spatiale par spectrométrie des pertes d'énergie d'électrons transmis : application en microélectronique à la caractérisation de couches minces (inférieur à 8NM) d'oxydes nitrurés." Grenoble 1, 1996. http://www.theses.fr/1996GRE10027.
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Ce travail evalue la potentialite de la microanalyse par spectrometrie de perte d'energie, couplee a un microscope electronique en transmission dote d'un canon a effet de champ, pour caracteriser chimiquement des structures de la microelectronique. Cette etude est principalement axee sur la caracterisation d'oxydes nitrures (e#o#x>8 nm). Apres avoir presente la methode experimentale que nous avons etablie pour obtenir des profils de concentration, nous montrons qu'avec cet outil de caracterisation, il est possible de: detecter l'azote dans une matrice de silice, avec une limite de detection de 4 10#2#0at/cm#3, d'atteindre une resolution spatiale de 0,8 nm 0,04 nm (pour une taille de sonde de 0,6 nm), d'etablir sans difficulte des profils de concentrations dans des couches minces (inferieures a 4 nm). Nous presentons et commentons ensuite les profils de concentration d'azote que nous avons etablis sur des oxydes nitrures soit sous nh#3, soit nous no. Pour situer et apprecier les resultats, nous les comparons avec les mesures donnees par deux techniques de surface: l'auger ou le sims. Nous montrons en particulier que si la spectroscopie auger permet d'atteindre une limite de detection en concentration equivalente a celle obtenue par spectrometrie de perte d'energie, elle conduit a etablir des profils moins precis en profondeur, donnant une information plus globale sur la repartition de l'azote dans les couches. Le sims est une methode plus sensible que la notre pour la detection de l'azote ; cependant, la spectrometrie de perte d'energie permet de rendre compte avec une bonne precision de fluctuations locales de composition. En conclusion, la configuration experimentale que nous avons etudiee est a l'heure actuelle l'unique methode permettant une analyse chimique locale des elements legers sur un circuit electronique, avec une resolution spatiale inferieure au nanometre
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Latroche, Michel. "Caracterisations physico-chimiques des bronzes de titane en relation avec leur stoechiometrie." Nantes, 1988. http://www.theses.fr/1988NANT2019.
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Ces bronzes de titane de type hollandite sont des composes a vfalence mixte de formule generale a::(x)tio::(2), avec a=k, rb, cs et 0,125
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Forano, Claude. "Les conducteurs protoniques : HSbO3.nH2O ET SnO2.nH2O : caracterisation, etude rmn et applications." Clermont-Ferrand 2, 1987. http://www.theses.fr/1987CLF21069.
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Preparation par une methode sol-gel permettant d'obtenir des materiaux de grande purete; mise en evidence de differences structurales importantes, d'une tres grande homogeneite morphologique et d'une difference importante de la taille des cristallites. Confirmation par rmn de l'existence de plusieurs especes protonees. Etude des variations de la conductivite en fonction de la temperature; influence de la teneur en eau. Mise en evidence de la relation entre la conductivite electrique et la mobilite protonique a partir de mesures des temps de relaxation et proposition d'un mecanisme de type grotthus. Elaboration de couches epaisses par serigraphie; possibilites d'application dans des dispositifs microioniques. Essais d'utilisation pour la detection de h::(2)
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Lepinay, Kevin. "Développement et applications de la tomographie chimique par spectroscopie EDX." Thesis, Lyon, INSA, 2013. http://www.theses.fr/2013ISAL0124/document.
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Cette thèse porte sur l’évaluation des techniques pour la tomographie chimique par STEM EDX : mise au point des procédures expérimentales, traitement des données, reconstruction des volumes, analyse de la qualité des résultats obtenus et évaluation de la complexité globale. Les performances très limitées de l’analyse STEM EDX font que peu d’études, jusqu’à aujourd’hui, se sont portées sur cette technique. Cependant, les avancées très notables procurées par les nouveaux détecteurs ‘SDD’ ainsi que les sources électroniques X-FEG haute brillance, rendant l’analyse STEM EDX 2D très rapide, ont relancé la possibilité de la tomographie chimique ; la technique demande toutefois à être mise au point et évaluée (performances et complexité). Nous avons travaillé sur un microscope Tecnai Osiris permettant d’acquérir des cartographies chimiques EDX de centaines de milliers de pixels avec une résolution de l’ordre du nanomètre en quelques minutes. Nous avons choisi de préparer par FIB des échantillons en forme de pointe et d’utiliser un porte-objet permettant une exploration angulaire de 180° sans ombrage. Puis, à l’aide d’échantillons modèles (billes de SiO2 dans une résine), nous avons évalué les déformations d’échantillon par l’irradiation du faisceau électronique. Ceci nous a permis de proposer une méthode pour limiter cet effet par déposition d’une couche de 20 nm de chrome. Des simulations d’images ont permis d’évaluer les logiciels et méthodes de reconstruction. La méthodologie de chaque étape d’une analyse de tomographie STEM EDX a ensuite été expliquée, et l’intérêt de la technique démontré grâce à la comparaison de l’analyse 2D et 3D d’un transistor FDSOI 28 nm. La qualité des reconstructions (rapport signal-sur-bruit, résolution spatiale) a été évaluée en fonction des paramètres expérimentaux à l’aide de simulations et d’expériences. Une résolution de 4 nm est démontrée grâce à l’analyse d’une mire et d’un transistor « gate all around ». Pour ce même transistor, la possibilité et l’intérêt d’analyse de défaillance à l’échelle nanométrique est prouvée. Une analyse d’un défaut de grille d’une SRAM ou de trous dans un pilier en cuivre permettent d’expliquer l’intérêt d’une combinaison d’un volume HAADF (morphologie et résolution < 4 nm) et du volume EDX (information chimique). La conclusion est que cette technique, qui reste encore à améliorer du point de vue de sa simplicité, montre déjà son utilité pour l’analyse et la mise au point des technologies avancées (nœud 20 nm et après)This thesis focuses on the evaluation of the STEM EDX chemical tomography technique: development of experimental procedures, data processing and volumes reconstruction, quality analysis of the results and evaluation of the overall complexity. Until now, STEM EDX analysis performances were very limited, so only few studies about this technique have been realized. However, very significant progress procured by the new SDD detectors as well as by the high brightness electronic sources (X-FEG), making the STEM EDX 2D analysis very fast, have revived the possibility of the chemical tomography, although the technique has to be developed and evaluated (performance and complexity). We have worked on a Tecnai Osiris which acquires EDX chemical mapping of hundreds of thousands of pixels with resolution of one nanometer and in a few minutes. We chose to prepare the rod-shaped samples by FIB and use a sample holder allowing an angle of exploration of 180° without shadowing effects. Then, using model samples (SiO2 balls in resin), we evaluated the sample deformation due to the electron beam irradiation. This allowed us to propose a method to reduce this effect by depositing a 20 nm chromium layer. Images simulations were used to evaluate the software and the reconstruction methods. The methodology of each step of the STEM EDX tomography analysis is then explained and the technique interest is demonstrated by comparing the 2D and the 3D analysis of a transistor 28 nm FDSOI. The quality of the reconstructions (signal-to-noise ratio, spatial resolution) was evaluated, in function of experimental parameters, using simulations and experiments. A resolution of 4 nm is demonstrated through the analysis of a test pattern and a "gate all around” transistor. For the same transistor, the possibility and the interest of a failure analysis at the nanoscale is proven. Analyses of a SRAM gate fail or of the holes in a copper pillar explain the benefits of a combination between a HAADF volume (morphology and resolution < 4 nm) and an EDX volume (chemical information). To conclude, this technique, which still needs to be improved in terms of simplicity, is already showing its usefulness for the analysis and the development of advanced technologies (20nm node and beyond)
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Tsai, Wei-Huan, and 蔡維桓. "Design and Fabrication of Integrated In-Situ Liquid Transmission Electron Microscopy Specimens." Thesis, 2017. http://ndltd.ncl.edu.tw/handle/b7r9rj.
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碩士國立交通大學
材料科學與工程學系所
105
Nowadays, The new development of liquid specimen became an important technique in biomedical engineering, chemical synthesis, and interfacial science, which enables the object to be observed in liquid phase. However, the present liquid specimen are fabricated by sealing top and bottom chips with epoxy after assembly. The total thickness is large and the large sealed area may result in the leakage. In this work, we developed a new type of liquid TEM specimen, Integrated liquid specimen, which could overcome the above disadvantages. The integrated liquid specimen was fabricated by one chip without the bonding/sealing process, which declined the leakage issue in the TEM vacuum environment, and it was suitable for all the model of JEOL TEM. Besides, we adopt solution to this specimen to observe the motion and growth mechanism of Au nanoparticles, demonstrating the practicability of Integrated liquid specimen.
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"An Automated System for Cryo-Electron Microscopy Sample Preparation." Thesis, 2011. http://hdl.handle.net/1911/70475.
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Cryo-electron microscopy (CryoEM) is a procedure that has become popular for imaging radiation intolerant structures under electron microscopes. CryoEM involves maintaining the sample at cryogenic temperatures throughout the imaging process This has the effect of minimizing damage caused by the electron beam, and results in higher quality images than can be obtained through more traditional imaging methods. The preparation of samples for cryo-electron microscopy studies is currently a labor and time intensive process. Samples must be applied to an imaging substrate under tightly controlled environmental conditions, formed into a thin film, vitrified with liquid ethane, and placed into temporary storage under cryogenic conditions. The grid preparation process is very sensitive to procedural factors, thus the successful creation of viable samples depends on tightly controlling the conditions under which grids are prepared. Several devices which automate portions of the specimen preparation process are currently in use; however, these systems heavily rely on a human operator to function properly. This thesis describes a system that is capable of fully automating the sample preparation process. The resulting system minimizes the need for human input during specimen preparation, improves process control, and provides similar levels of environmental control. Testing shows that the resulting system is capable of preparing samples without human interaction.
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Frangakis, Achilleas S. [Verfasser]. "Noise reduction and segmentation techniques developed for multidimensional electron microscopy of biological specimens / Achilleas S. Frangakis." 2001. http://d-nb.info/962126888/34.
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Thwala, Lungile Nomcebo. "Preparation and characterization of alginate-chitosan nanoparticles as a drug delivery system for lipophilic compounds." Thesis, 2012. http://hdl.handle.net/10210/6192.
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M.Sc.Despite several decades of extensive research and development in pharmaceutical chemistry, the poor solubility of lipophilic compounds in aqueous media remains a major barrier to their absorption, bioavailability and clinical efficacy. This poor solubility is also a problem in other areas such as the flavour and fragrance industry. In cosmetics, for example, poor aqueous solubility and instability of oily compounds causes problems in formulation and fragrance stability. One approach to overcome these difficulties is to encapsulate oily compounds in biocompatible materials. As a drug delivery system such an approach is attractive if the size of the capsule is reduced to the micrometer or nanometer scale. Naturally occurring polysaccharides like sodium alginate (NaALG) and chitosan (CS) are generally regarded as safe (GRAS) for use in human use and have therefore gained much attention recently. As a drug delivery system, this polymer matrix can be used to prevent drug degradation in the gastro intestinal tract (GIT) and often provides controlled release of the encapsulant. Cyclodextrins (CDs) on the other hand offer an alternative approach. These cyclic oligosaccharides have the ability to form non-covalent inclusion complexes with a range of organic compounds, and in so doing alter their physiochemical properties such as solubility. This study was aimed at exploring these concepts by using ALG and CS as an entrapment matrix for an essential oil, tagette oil (used as a model oily drug) that is insoluble in aqueous media. Alginate/chitosan (ALG/CS) nanoparticles were prepared in a 3-step procedure; emulsification of tagette oil in aqueous Na-ALG solution, followed by ionotropic pre-gelation of the ALG core with CaCl2 and further crosslinking with CS. Morphology and particle size measurements were performed by scanning and transmission electron microscopy (SEM and TEM), and Malvern Zetasizer.
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Kiesel, Sharon Mary. "Transmission electron microscopy preparation and characterization of bulk ZnO and Au(111) / ZnO(0001̄) heterostructures." 2003. http://www.lib.ncsu.edu/theses/available/etd-11242003-211411/unrestricted/etd.pdf.
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Ya, Chin Chiou. "Preparation of Silicon Nanoribbons and Investigation on the Formation of the Nickel Silicide Nanoribbons by In situ Transmission Electron Microscopy." 2006. http://www.cetd.com.tw/ec/thesisdetail.aspx?etdun=U0016-1303200709274066.
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Chiou, Ya Chin, and 邱雅琴. "Preparation of Silicon Nanoribbons and Investigation on the Formation of the Nickel Silicide Nanoribbons by In situ Transmission Electron Microscopy." Thesis, 2006. http://ndltd.ncl.edu.tw/handle/36957931335808308498.
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碩士國立清華大學
材料科學工程學系
94
Arrays of aligned silicon nanoribbons were prepared on silicon substrates in the solution containing aqueous HF and AgNO3 by metal-nanoparticel-assisted etching technique. The in situ investigations of a solid-state reaction where the silicon nanoribbons transformed into nickel silicide nanoribbons are achieved in the silicon nanoribbons/Ni grid system. The results indicate that Ni atoms are still the dominant diffusing species in Ni/Si system at nanometer scale. The condition for the in situ experiments is under Ni-rich situation so that the final phases of the formed silicides are all Ni-rich phases. We also investigate the transformation of Si nanoribbons into nickel silicide nanoribbons at elevated temperature. The activation energy (1.06 eV) for the growth of nickel silicide nanoribbons was obtained from an Arrhenius plot. The approach is useful to clarify the silicidation mechanisms and phase transformation at the nanoscale. In addition, using the method of comparison of the experimental high-resolution TEM images with the simulated images, the thickness of nanoribbons could be determined.
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Lewis, Colin A., and G. A. S. Armstrong. "An evaluation of different methods of preparation of quartz grains for study of their surface features by scanning electron microscopy." 1994. http://hdl.handle.net/10962/d1006741.
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Sediments from periglacial and glacial environments were subjected to initial preparation and portions were subsequently further prepared using either the dichromate or the hydrogen peroxide method before being examined by scanning electron microscopy. Statistically significant differences did not occur in the results obtained for samples subjected only to initial or to initial and either of the two further preparations: it is concluded that initial preparation is satisfactory and further preparation unnecessary.
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Platzmann, Florian Peter. "Methods to improve the sample quality of macromolecular complexes for structure determination by 3D Electron Cryo-Microscopy." Doctoral thesis, 2012. http://hdl.handle.net/11858/00-1735-0000-000D-F0B2-C.
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