Dissertationen: „Transmission electron microscopy (TEM)“

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TIYYAGURA, MADHAVI. „TRANSMISSION ELECTRON MICROSCOPY STUDIES IN SHAPE MEMORY ALLOYS“. Master's thesis, University of Central Florida, 2005. http://digital.library.ucf.edu/cdm/ref/collection/ETD/id/3913.

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In NiTi, a reversible thermoelastic martensitic transformation can be induced by temperature or stress between a cubic (B2) austenite phase and a monoclinic (B19') martensite phase. Ni-rich binary compositions are cubic at room temperature (requiring stress or cooling to transform to the monoclinic phase), while Ti-rich binary compositions are monoclinic at room temperature (requiring heating to transform to the cubic phase). The stress induced transformation results in the superelastic effect, while the thermally induced transformation is associated with strain recovery that results in the shape memory effect. Ternary elemental additions such as Fe can additionally introduce an intermediate rhombohedral (R) phase between the cubic and monoclinic phase transformation. This work was initiated with the broad objective of connecting the macroscopic behavior in shape memory alloys with microstructural observations from transmission electron microscopy (TEM). Specifically, the goals were to examine (i) the effect of mechanical cycling and plastic deformation in superelastic NiTi; (ii) the effect of thermal cycling during loading in shape memory NiTi; (iii) the distribution of twins in martensitic NiTi-TiC composites; and (iv) the R-phase in NiTiFe. Both in situ and ex situ lift out focused ion beam (FIB) and electropolishing techniques were employed to fabricate shape memory alloy samples for TEM characterization. The Ni rich NiTi samples were fully austenitic in the undeformed state. The introduction of plastic deformation (8% and 14% in the samples investigated) resulted in the stabilization of martensite in the unloaded state. An interlaying morphology of the austenite and martensite was observed and the martensite needles tended to orient themselves in preferred orientations. The aforementioned observations were more noticeable in mechanically cycled samples. The observed dislocations in mechanically cycled samples appear to be shielded from the external applied stress via mismatch accommodation since they are not associated with unrecoverable strain after a load-unload cycle. On application of stress, the austenite transforms to martensite and is expected to accommodate the stress and strain mismatch through preferential transformation, variant selection, reorientation and coalescence. The stabilized martensite (i.e., martensite that exists in the unloaded state) is expected to accommodate the mismatch through variant reorientation and coalescence. On thermally cycling a martensitic NiTi sample under load through the phase transformation, significant variant coalescence, variant reorientation and preferred variant selection was observed. This was attributed to the internal stresses generated as a result of the thermal cycling. A martensitic NiTi-TiC composite was also characterized and the interface between the matrix and the inclusion was free of twins while significant twins were observed at a distance away from the matrix-inclusion interface. Incorporating a cold stage, diffraction patterns from NiTiFe samples were obtained at temperatures as low as -160ºC. Overall, this work provided insight in to deformation phenomena in shape memory materials that have implications for engineering applications (e.g., cyclic performance of actuators, engineering life of superelastic components, stiffer shape memory composites and low-hysteresis R-phase based actuators). This work was supported in part by an NSF CAREER award (DMR 0239512).
M.S.M.E.
Department of Mechanical, Materials and Aerospace Engineering;
Engineering and Computer Science
Materials Science and Engineering

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Karlsson, Linda. „Transmission Electron Microscopy of 2D Materials : Structure and Surface Properties“. Doctoral thesis, Linköpings universitet, Tunnfilmsfysik, 2016. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-127526.

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During recent years, new types of materials have been discovered with unique properties. One family of such materials are two-dimensional materials, which include graphene and MXene. These materials are stronger, more flexible, and have higher conductivity than other materials. As such they are highly interesting for new applications, e.g. specialized in vivo drug delivery systems, hydrogen storage, or as replacements of common materials in e.g. batteries, bulletproof clothing, and sensors. The list of potential applications is long for these new materials. As these materials are almost entirely made up of surfaces, their properties are strongly influenced by interaction between their surfaces, as well as with molecules or adatoms attached to the surfaces (surface groups). This interaction can change the materials and their properties, and it is therefore imperative to understand the underlying mechanisms. Surface groups on two-dimensional materials can be studied by Transmission Electron Microscopy (TEM), where high energy electrons are transmitted through a sample and the resulting image is recorded. However, the high energy needed to get enough resolution to observe single atoms damages the sample and limits the type of materials which can be analyzed. Lowering the electron energy decreases the damage, but the image resolution at such conditions is severely limited by inherent imperfections (aberrations) in the TEM. During the last years, new TEM models have been developed which employ a low acceleration voltage together with aberration correction, enabling imaging at the atomic scale without damaging the samples. These aberration-corrected TEMs are important tools in understanding the structure and chemistry of two-dimensional materials. In this thesis the two-dimensional materials graphene and Ti3C2Tx MXene have been investigated by low-voltage, aberration-corrected (scanning) TEM. High temperature annealing of graphene covered by residues from the synthesis is studied, as well as the structure and surface groups on single and double Ti3C2Tx MXene. These results are important contributions to the understanding of this class of materials and how their properties can be controlled.

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Wan, Qian. „Transmission electron microscopy study of heterostructures grown on GaAs (110)“. Doctoral thesis, Humboldt-Universität zu Berlin, Mathematisch-Naturwissenschaftliche Fakultät I, 2014. http://dx.doi.org/10.18452/16949.

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In der Arbeit werden die mikrostrukturellen Eigenschaften von an (110)-Flächen orientierten Heterostrukturen auf GaAs-Substraten mittels verschiedener Techniken der Transmissionselektronenmikroskopie untersucht. Kubisch flächenzentrierte (Al,Ga)As/AlAs/GaAs Mehrschichtstrukturen auf GaAs(110) weisen in orthogonalen Richtungen parallel zur Substratoberfläche verschiedene Mechanismen zur Aufnahme der Verspannungen aufgrund von Fehlanpassungen auf. Defektfreie Strukturen sind durch eine geeignete, kurz periodische AlAs/GaAs-Überstruktur erfolgreich realisiert worden. Abschließend sind künstliche Defekte per Nanoindentation in den defektfreien Proben erzeugt worden, um die Auswirkung kurzperiodischer Übergitter zu prüfen. Das System aus hexagonal dicht gepacktem MnAs auf GaAs(110) zeichnet sich durch anisotrope Gitterfehlanpassung von -7.5% und 0.7% entsprechend der [11-20] und der [0001] Richtungen aus. Eine Benetzungsschicht, die der Entstehung von Inseln vorausgeht, wird beobachtet, was das Stranski-Krastanov-Wachstum von MnAs belegt. Die Dehnung durch die Gitterfehlpassung von 0.7% wird elastisch eingebaut, während die Spannung durch die Gitterfehlanpassung in der senkrechten [11-20] Richtung durch die Entstehung einer periodischen Anordnung, vollständiger Gitterfehlanpassungsversetzungen abgebaut wird, die sich von der Grenzfläche entfernt im MnAs-Gitter befinden. Das aus der Versetzungsanordnung resultierende Dehnungsfeld ist auf eine Dicke von 3.4 nm um die Grenzfläche beschränkt. Eine atomare Struktur der Grenzfläche wird basierend auf dem Vergleich von HRTEM-Aufnahmen und Simulationen vorgeschlagen. CoAl-Legierungen in der B2-Phase sind zum Vergleich auf (001) und auf (110) orientierten GaAs-Substraten hergestellt worden. Beide Fälle weisen die Koexistenz der B2-Phase und der ungeordneten, kubisch raumzentrierten Variante auf. Die Unordnung wird teilweise durch die epitaktische Dehnung und teilweise durch Diffusion von Punktdefekten hervorgerufen.
In the work, we systematically investigate the microstructural properties of (110) oriented heterostructures on GaAs substrates by means of different transmission electron microscopy techniques. Fcc-type (Al,Ga)As/AlAs/GaAs multilayer structure on GaAs (110) presents different mismatch strain accommodation mechanisms along the perpendicular in-plane directions. Defect-free structures are successfully acquired by an appropriate type of AlAs/GaAs short period superlattice. Finally, artificial defects are intentionally produced by nano-indentation to the defect-free sample to verify the effect of short period superlattices. Hcp-type MnAs on GaAs (110) system is characterized by anisotropic lattice mismatches of -7.5% and 0.7% along the [11-20] and [0001] direction, respectively. A wetting layer is observed prior to the formation of islands, indicating a Stranski-Krastanov growth mode of MnAs. The strain corresponding to the 0.7% lattice misfit is accommodated elastically, whereas the mismatch stress along perpendicular [11-20] direction is relived by the formation of a periodic array of perfect misfit dislocations with a stand-off position in MnAs lattice. The long range strain field associated with the dislocation array is constrained at the interface within a thickness of about 3.4 nm. An interfacial atomic configuration is also proposed based on the comparison between HRTEM image and the simulations. B2-type CoAl alloys are realized on (001) and (110) oriented GaAs substrates for comparison. They are both characterized by a coexistence of B2 phase and its disordered version bcc phase. The disordering is induced partially by the epitaxial strain and partially by the diffusion of point defects.

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Asaulenko, L. G., L. M. Purish und D. R. Abdulina. „Use of the Transmission Electron Microscopy for Examination of Biofilms Structure“. Thesis, Sumy State University, 2013. http://essuir.sumdu.edu.ua/handle/123456789/35267.

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Combination of transmission electron microscopy technics with colloidal gold labeled lectin staining allowed investigating glycoconjugates in biofilms of the corrosion relevant bacteria. Lectins with the same specificity were found to express different affinity to the compounds of the bacterial biofilms. LBA lectin showed the highest binding capacity to N-acetyl-D-galactosamine in Desulfovibrio sp. 10 and Bacillus subtilis 36 biofilms. For the assessment of N-acetyl-D-glucosamine presence in Bacillus subtilis 36 and Pseudomonas aeruginosa 27 biofilms WGA lectin was the most efficient. Staining with lectins labeled with the colloidal gold was proved to be a promising express technique for the investigations of glycoconjugate distribution and localization in bacterial biofilms. When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/35267

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Cardoch, Sebastian. „Studying Atomic Vibrations by Transmission Electron Microscopy“. Thesis, Uppsala universitet, Materialteori, 2016. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-305370.

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We employ the empirical potential function Airebo to computationally model free-standing Carbon-12 graphene in a classical setting. Our objective is to measure the mean square displacement (MSD) of atoms in the system for different average temperatures and Carbon-13 isotope concentrations. From results of the MSD we aim to develop a technique that employs Transmission Electron Microscopy (TEM), using high-angle annular dark filed (HAADF) detection, to obtain atomic-resolution images. From the thermally diffusive images, produced by the vibrations of atoms, we intent to resolve isotopes types in graphene. For this, we establish a relationship between the full width half maximum (FWHM) of real-space intensity images and MSD for temperature and isotope concentration changes. For the case of changes in the temperature of the system, simulation results show a linear relationship between the MSD as a function of increased temperature in the system, with a slope of 7.858×10-6 Å2/K. We also note a power dependency for the MSD in units of [Å2] with respect to the FWHM in units of [Å] given by FWHM(MSD)=0.20MSD0.53+0.67. For the case of increasing isotope concentration, no statistically significant changes to the MSD of 12C and 13C are noted for graphene systems with 2,000 atoms or more. We note that for the experimental replication of results, noticeable differences in the MSD for systems with approximately 320,000 atoms must be observable. For this, we conclude that isotopes in free-standing graphene cannot be distinguished using TEM.

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Agnese, Fabio. „Advanced transmission electron microscopy studies of semiconductor nanocrystals synthesized by colloidal methods“. Thesis, Université Grenoble Alpes (ComUE), 2018. http://www.theses.fr/2018GREAY043/document.

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Les recherches sur les nanocristaux semiconducteur (NCs) ont conduit à des résultats scientifiques fascinants, spécialement pour l'application en dispositifs optoelectroniques. Afin de répondre à certaines exigences comme des coûts mineurs, des gains d'efficacité, des composants respectueux de l'environnement, etc., des nouvelles méthodes sont explorées: dans les procédés en solution, dans l'ingénierie de bande et des niveaux d'énergie. En particulier, la méthode de synthèse peut influencer les propriétés optoélectroniques. Par conséquent, une meilleure compréhension des facteurs complexes pendant la synthèse entraînera une amélioration des performances.La microscopie électronique avancée fournit un moyen précis de recueillir des informations sur la morphologie, la structure cristalline et la composition chimique des matériaux avec une résolution spatiale au niveau atomique. La première partie de cette thèse traite de la synthèse et de la préparation des échantillons pour la microscopie électronique à transmission en haute résolution (HRTEM).La deuxième partie traite du mécanisme de croissance des NCs Cu2ZnSnS4 synthétisés par une méthode colloïdale. La morphologie et la stoechiométrie des intermédiaires de réaction extraits après différents intervalles de temps sont déterminés par HRTEM et analyse dispersive en énergie (EDS).Deux méthodes complémentaires, la diffraction par nanofaisceau d’électrons en précession (NPED) et la microscope électronique en transmission par balayage à haute résolution avec imagerie en champ sombre avec détecteur annulaire à grand angle (HRSTEM-HAADF) permettent une profonde caractérisation de la structure cristalline.En outre, la structure cristalline de NCs CsPbBr3 est résolue avec simulations de STEM-HAADF. Cet approche peut différencier entre structures cristallines cubiques et orthorhombiques, impossible avec techniques de diffraction traditionnelles. Enfin, l'influence des méthodes de synthèse sur la morphologie et sur la structure cristalline de NCs CuFeS2 pour applications dans le domaine de la thermoélectricité est analysée par HRTEM
The investigations of semiconductor nanocrystals (NCs) led to fascinating scientific results in optoelectronic devices. In order to fulfill certain requirements, i.e. cheaper costs, higher efficiencies, environmental friendly components etc., new methods are explored in solution-processing, band gap and energy level engineering. Particularly, the method of synthesis can alter the optoelectronic properties. Therefore, a better understanding of the intricate factors during synthesis will lead to improved performances. Advanced electron microscopy provides a precise way to gather information about morphology, crystal structure and chemical composition of materials with a spatial resolution down to the atomic level. The first part of this thesis deals with the optimization of the synthesis and sample preparation for high resolution transmission electron microscopy (HRTEM).The second part deals with the growth mechanism of Cu2ZnSnS4 NCs synthesized by a colloidal method. The morphology and stoichiometry of the samples extracted after different time intervals are characterized by HRTEM and electron dispersion spectroscopy (EDS). Two complementary methods, Nanobeam Precession Electron Diffraction (NPED) and High Resolution Scanning Transmission Electron Microscopy by High Angle Annular Dark-Field Imaging (HRSTEM-HAADF), provide an in-depth crystal structure characterization.Moreover, the crystal structure of CsPbBr3 NCs is solved by probing STEM-HAADF simulations. This approach is able to differentiate cubic and orthorhombic crystal structures, which is otherwise impossible by diffraction techniques. Finally, the influence of synthesis methods on the morphology and crystal structure of CuFeS2 NCs is investigated by HRTEM for thermoelectric applications

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Sharp, Joanne. „Electron tomography of defects“. Thesis, University of Cambridge, 2010. https://www.repository.cam.ac.uk/handle/1810/228638.

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Tomography of crystal defects in the electron microscope was first attempted in 2005 by the author and colleagues. This thesis further develops the technique, using a variety of samples and methods. Use of a more optimised, commercial tomographic reconstruction program on the original GaN weak beam dark-field (WBDF) tilt series gave a finer reconstruction with lower background, line width 10-20 nm. Four WBDF tilt series were obtained of a microcrack surrounded by dislocations in a sample of indented silicon, tilt axes parallel to g = 220, 220, 400 and 040. Moiré fringes in the defect impaired alignment and reconstruction. The effect on reconstruction of moiré fringe motion with tilt was simulated, resulting in an array of rods, not a flat plane. Dislocations in a TiAl alloy were reconstructed from WBDF images with no thickness contours, giving an exceptionally clear reconstruction. The effect of misalignment of the tilt axis with systematic row g(ng) was assessed by simulating tilt series with diffraction condition variation across the tilt range of Δn = 0, 1 and 2. Misalignment changed the inclination of the reconstructed dislocation with the foil surfaces, and elongated the reconstruction in the foil normal direction; this may explain elongation additional to the missing wedge effect in experiments. Tomography from annular dark-field (ADF) STEM dislocation images was also attempted. A tilt series was obtained from the GaN sample; the reconstructed dislocations had a core of bright intensity of comparable width to WBDF reconstructions, with a surrounding region of low intensity to 60 nm width. An ADF STEM reconstruction was obtained from the Si sample at the same microcrack as for WBDF; here automatic specimen drift correction in tomography acquisition software succeeded, a significant improvement. The microcrack surfaces in Si reconstructed as faint planes and dislocations were recovered as less fragmented lines than from the WBDF reconstruction. ADF STEM tomography was also carried out on the TiAl sample, using a detector inner angle (βin) that included the first order Bragg spots (in other series βin had been 4-6θ B). Extinctions occurred which were dependent on tilt; this produced only weak lines in the reconstruction. Bragg scattering in the ADF STEM image was estimated by summing simulated dark-field dislocation images from all Bragg beams at a zone axis; a double line was produced. It was hypothised that choosing the inner detector angle to omit these first Bragg peaks may preclude most dynamical image features. Additional thermal diffuse scattering (TDS) intensity due to dilatation around an edge dislocation was estimated and found to be insignificant. The Huang scattering cross section was estimated and found to be 9Å, ten times thinner than experimental ADF STEM dislocation images. The remaining intensity may be from changes to TDS from Bloch wave transitions at the dislocation; assessing this as a function of tilt is for further work. On simple assessment, only three possible axial channeling orientations were found over the tilt range for GaN; if this is typical, dechanneling contrast probably does not apply to defect tomography.

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Lai, Pooi-fun. „TEM and structural investigations of synthesized and modified carbon materials /“. Connect to thesis, 1999. http://eprints.unimelb.edu.au/archive/00000770.

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Caballero-Alias, Ana Maria. „The role of silica in mineralising tissues“. Thesis, Nottingham Trent University, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.302515.

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10

Xin, Renlong. „TEM studies of calcium phosphates for the understanding of biomineralization /“. View abstract or full-text, 2006. http://library.ust.hk/cgi/db/thesis.pl?MECH%202006%20XIN.

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Melichárek, Václav. „Návrh manipulátoru pro TEM“. Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2020. http://www.nusl.cz/ntk/nusl-417138.

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The topic of this master’s thesis is the design of a sample manipulator for TEM. Regarding which the segment of the sample manipulator used to move the sample in the direction of the x-axis (so-called x-stage) was designed. The introductory theoretical part is concerned with a brief description of transmission electron microscopy focused on the imaging methods used in TEM and the procedures of preparing and loading TEM samples. The theoretical part follows with the design of precise mechanisms, especially with respect to the inaccuracies of their operation and the technological aspect of the design. In the practical part, a detailed analysis of the design of the x-stage is presented. Kinematics and dynamics of the mechanism is analyzed in depth, following with the description of the overall design of the mechanism and some of its parts in detail.

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Vaughn, Joel M. „Manipulation Of Nanoscale Objects in the Transmission Electron Microscope“. Ohio University / OhioLINK, 2007. http://rave.ohiolink.edu/etdc/view?acc_num=ohiou1191525305.

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Tyborowski, Tobias. „Determining the interwall spacing in carbon nanotubes by using transmission electron microscopy“. Thesis, Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), 2016. http://urn.kb.se/resolve?urn=urn:nbn:se:kau:diva-45754.

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The interwall spacing of multi-walled carbon nanotubes has an effect on their physical and chemical properties. Tubes with larger interwall spacing - compared to the spacing where the carbon atoms are in their natural distance to each other - are for instance expected to be mechanically less stable. Considering the MWCNT interwall spacing’s dependence on the tube size, three interesting previous studies with slightly different conclusions can be found. All of them conclude an increase of the interwall spacing with a decreasing tube size. We describe their analysis procedure, compare them to each other and to our own measured data. In the beginning of our analyses, we determine the expected inaccuracy for measured distances out of TEM images being up to 10 % and we show the impacts of the TEM’s defocus, a powerful setting in TEM imaging. Finally, we suppose that the interwall spacings are not as strongly varying as one previous study concludes, but our analyses are relatively in harmony with the two other studies. The interwall spacings from tubes with an inner diameter larger than 5 nm are relatively constant within the whole tube. Furthermore, it appears that the middle spacings (excluding the outer- and innermost ones) show values that are most consistent with the interlayer spacings of turbostratic graphite. In underfocused images, the outer- and innermost spacings tend to have values being slightly smaller than the middle ones from the same tube.

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Barrett, Heather A. „A COMPARATIVE TRANSMISSION ELECTRON MICROSCOPY INVESTIGATION OF DEFECTS AND TEXTURES IN CRYPTOMELANE“. Miami University / OhioLINK, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=miami1375787636.

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Nukala, Haritha. „QUANTITATIVE THICKNESS MAPPING IN HIGH-ANGLE ANNULAR DARK-FIELD (HAADF) SCANNING TRANSMISSION ELECTRON MICROSCOPY (STEM)“. Master's thesis, University of Central Florida, 2008. http://digital.library.ucf.edu/cdm/ref/collection/ETD/id/4292.

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Only a few methods are currently available for the measurement of sample thicknesses in Transmission Electron Microscopy (TEM). These methods, Convergent-Beam Electron Diffraction (CBED) and thickness mapping in Energy-Filtered TEM (EFTEM), are either elaborate or complex. In this present work, I have investigated and come up with a simple straight-forward method to measure the local thickness of a TEM sample with the atomic number (Z-contrast) imaging using High-Angle Annular Dark Field (HAADF) Scanning Transmission Electron Microscopy (STEM). HAADF STEM shows atomic number contrast for high scattering angles of the electrons, owing to predominant electron scattering at the potential of the nucleus similar to Rutherford scattering. The characterization of materials by STEM helps to identify microstructures and nanostructures within a sample and to analyze defects in samples. HAADF STEM imaging is capable of resolving atomic structures with better than 2 Å lateral resolution. However, HAADF STEM has so far not been systematically used to measure sample thicknesses. In Z-contrast imaging, it was known that the intensity of the electrons scattered to high angles increases with increase in the atomic number (Z) of the element/compound with increasing thickness of the sample based on the equation, I ~ t.Zα Where t, is the thickness and α, is a parameter between 1 and 2. This project was started with this simple approach, but the experimental results within the thesis show that the relation between the intensity and the atomic number is not well described by this equation. A more reliable parameter, σZ, the interaction coefficient of the material was calculated. Samples containing Ag2Al platelets in Al matrix were used for calibration purposes. Additional samples containing layers of known elements/compounds were obtained from TriQuint Semiconductors and from the Physics department of UCF to calculate σ for various elements/compounds. These experimental values were used to measure the local thicknesses in nanoparticles and also the total volume of the nanoparticles. This quantitative HAADF STEM analysis represents a new method, which can be added to the list of methods used for the purpose of measurement of the local thickness of a sample in the TEM. This method is especially useful for the thickness measurement of nanoparticles. The other two methods, CBED and thickness maps in EFTEM are strongly affected by the sample orientation and therefore not appropriate for the study of nanoparticle thicknesses, whereas orientation effects are negligible for the conditions used in this HAADF STEM analysis.
M.S.
Department of Mechanical, Materials and Aerospace Engineering;
Engineering and Computer Science
Materials Science & Engr MSMSE

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Wu, Mingjian. „Advanced transmission electron microscopy investigation of nano-clustering in Gd-doped GaN“. Doctoral thesis, Humboldt-Universität zu Berlin, Mathematisch-Naturwissenschaftliche Fakultät I, 2014. http://dx.doi.org/10.18452/16950.

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Das zentrale Ziel der vorliegenden Arbeit besteht einerseits darin, die Verteilung von Gd in GaN:Gd mit Gd-Konzentrationen von 10^16–10^19 cm^-3 mittels fortgeschrittener (Raster-) Transmissionselektronenmikroskopie [(S)TEM] zu bestimmen. Darauf basierend wird zum anderen das Verständnis des Mechanismus, der diese Verteilungen bewirkt, entwickelt. Wir diskutieren detailliert die Anwendung und die Grenzen von (S)TEM-Abbildungsmethoden und quantitativen Analysenmethoden und von Modellierungsmethoden, um Nano-Cluster in epitaktischen Halbleiterschichten zu beobachten und zu analysieren. Außerdem werden Fallstudien zweier Materialsysteme betrachtet, die offensichtlich Nano-Cluster aufweisen. Schließlich sind wir in der Lage, die in GaN:Gd auftretenden GdN-Cluster zu identifizieren und ihre atomare Struktur zu bestimmen. Dehnungskontrastabbildungen mit Kontrastberechnungen belegen eindeutig das Auftreten von kleinen, plättchenförmigen GdN-Clustern. Diese Cluster weisen nahezu gleiche Abmessungen auf und liegen mit der ausgedehnten Fläche parallel zu den GaN(0001)-Basalebenen. Dieses Ergebnis wird durch Dunkelfeld-STEM-Abbildungen (Z-Kontrast), bestätigt. Die starke, lokale Gitterdehnung (Verzerrungsfeld), die durch die Cluster hervorgerufen wird, ist in HRTEM-Aufnahmen abgebildet und quantitativ ausgewertet worden. Durch den Vergleich von Verzerrungsfeldern, die experimentell ermittelt worden sind, mit theroretischen Feldern schließen wir auf Cluster aus zweilagigen GdN-Plättchen mit einem Durchmesser von wenigen Gd-Atomen. Ihre interne Struktur entspricht etwa der NaCl-Phase des GdN. Dieses atomare Strukturmodell erlaubt unsere Diskussion der Energieverhältnisse der Cluster. Die Ergebnisse implizieren, dass die treibende Kraft für die beobachtete Plättchengröße ein Gleichgewicht zwischen der Zunahme von kohäsiver Energie und der Einschränkung durch die Dehnungsenergie an der Grenzfläche zwischen GdN-Cluster und GaN-Wirtsgitter aufgrund der Gitterfehlanpassung ist.
The central goal of this dissertation is (1) to clarify the distribution of Gd atoms in GaN:Gd with Gd concentration in the range between 10^16–10^19 cm^-3 by means of advanced (scanning) transmission electron microscopy [(S)TEM]; and based on that, (2) to understand the mechanisms that control such distribution. We discuss in detail the application and limitations of (S)TEM imaging and analysis techniques and modeling methods dedicated to the study of embedded nano-clusters. Besides, two case studies of semiconductor material systems that contain apparently observable nano-clusters are considered. One is about intentionally grown InAs nano-clusters embedded in Si and the other study the formation and phase transformation of Bi-containing clusters in annealed GaAsBi epilayers. Finally, we are able to identify the occurrence of GdN clusters in GaN:Gd samples and to determine their atomic structure. Strain contrast imaging in conjunction with contrast simulation unambiguously identifies the occurrence of small, platelet-shaped GdN clusters. These clusters are nearly uniform in size with their broader face parallel to the GaN (0001) basal plane. The result is confirmed by dark-field STEM Z-contrast imaging. The strong local lattice distortion (displacement field) induced by the clusters is recorded by HRTEM images and quantitatively analyzed. By comparing the displacement fields which are analyzed experimentally with these fields that are derived from energetically favored models, we conclude that the clusters are bilayer GdN with platelet diameter of only few Gd atoms; their internal structure is close to rocksalt GdN. This atomic structure model enables our discussion about the energetics of the clusters. The results indicate that the driving force for the formation of observed platelet in specific size is a compromise between the gain in cohesive energy and the penalty from interfacial strain energy due to lattice mismatch between the GdN cluster and GaN host.

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Lozano-Perez, Sergio. „TEM crack tip investigations of SCC“. Thesis, University of Oxford, 2002. http://ora.ox.ac.uk/objects/uuid:7e503ff9-782a-4f74-b184-dddaa96e03e2.

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Over the last few years, TEM has become a powerful technique to study cracks and specially crack tips. However, the number of publications including TEM results has not grown as it was expected. The main reason for this might be difficulties in the sample preparation. In this work we present a novel FIB sample preparation technique which has proved to be an ideal tool for preparing cross sectional samples containing crack tips. The morphology of intergranular stress corrosion cracking (IGSCC) has been investigated in Alloy 600 subjected to constant load and slow strain rate tests in simulated primary circuit pressurized water reactor conditions. Cracks were observed to nucleate at high-angle grain boundaries and propagate to depths of a few tens of micrometer along such boundaries, still in the initiation stage. Electron diffraction, energy dispersive x-ray (EDX) and electron energy loss spectroscopy (EELS) have been used to identify the different corrosion products and precipitates. Elemental mapping was employed to reveal changes in composition in the crack tip area. Major observations at cracks and grain boundaries include: the presence of different oxides in different locations, differences in grain boundary oxides and open crack/free surface oxides. These observations suggest that IGSCC involves oxygen diffusion through a porous oxide region along grain boundaries to the bare metal. This is a novel concept that offers an alternative to previous mechanisms proposed in the literature e.g. H embrittlement, slip-dissolution, etc., for which no supporting evidence has been found.

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Toth-Antal, Bence Materials Science &amp Engineering Faculty of Science UNSW. „Development of copper-alumina composites for abrasive wear applications“. Awarded By:University of New South Wales. Materials Science & Engineering, 2008. http://handle.unsw.edu.au/1959.4/44504.

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Copper-alumina composites were developed for testing in abrasive wear applications. The composites featured a porous continuous ceramic-preform network infiltrated by a liquid metal to form the final consolidated composite. The liquid metal phase was pure copper. Six different ceramic preform variants were tested. Ceramic volume fractions of 40, 50 and 60% were used, of two preform types; one pure-alumina, and one with additional 2wt% copper(I) oxide (CU20), functioning as an infiltration aid, the effects of which were determined in a previous study; the copper-oxide reduced infiltration pressure and allowed the use of higher ceramic phase volume fraction in the final composite. Abrasive wear tests against two automotive braking system materials were conducted. Grey cast iron of alloy type GG15 was used to establish a baseline for behaviour of the six different composite samples and compare them. Following this, the three volume fraction variants of samples using the copper-oxide infiltration aid were trialled against a commercially-available European passenger vehicle brake pad friction material; ABEX 6091. Wear tests were conducted on a pin-on-disc tribometer. Hemispherical-headed pins were made from the composite and tested against rotating discs of the grey cast iron and the ABEX friction material. Contact velocity was kept constant at Ims-?? at room temperature in air, and contact loads up to 15N were used. Test loads of 1-4N were used against grey cast iron, and 15N against the ABEX friction material. Optical micrography was used to monitor the wear rate of samples tested against grey cast iron. Scanning electron microscopy (SEM) was used to characterise bulk microstructures and evaluate surface wear features. Transmission electron microscopy (TEM) was used for further microstructural investigation of the sintering and interfacial features of the undamaged pin samples, as well as damage zones and tribofilm compositions. Focussed ion beam (FIB) milling was used to create subsurface cross-sections of wear regions and prepare TEM samples. The wear performance of the different sample types was compared by ceramic content and preform additives. It was found that the wear resistance of pure-alumina preform composites was dependent on ceramic volume fraction. Increasing ceramic content lead to increased wear resistance. The lower sinter temperature of the samples with the copper oxide additive led to reduced wear resistance compared with the monolithic alumina preforms and changes in ceramic volume fractions were not discernable in wear resistance against grey cast iron. This could be further supported by qualitative micrographic observations. All tests against grey cast iron were dominated by tribochemical film formation, which was determined to be oxidation of the iron which formed at the composite pin contact surface. Further testing of the copper-oxide containing samples against the ABEX friction material revealed a mixed result; the 50 and 60% ceramic volume samples produced near-identical wear performance, while the 40% sample suffered poor wear resistance. The dominant wear mechanism of composite pins tested against the ABEX friction material was abrasive wear. Sub-surface analysis of wear pins revealed a prominent damage layer forming at the contact surface of all pin samples which progressively grew into the bulk material. This layer was believed to have an important effect on the wear behaviour of the materials.

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Narangifard, Ali. „The multislice method in transmission electron microscopy simulation : An implementation in the TEM-simulator software package“. Thesis, KTH, Skolan för teknik och hälsa (STH), 2013. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-134189.

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This report introduces the multislice method for modeling the interaction between an electron and the atoms in the specimen (electron-specimen interaction). The multislice method is an approximation to the full quantum mechanical model for this interaction. After introducing the theory, we discuss how the multislice method is implemented and integrated into TEM-simulator, a software for simulation of Transmission Electron Microscope (TEM) images.

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Rooney, Aidan. „Characterisation of buried interfaces in van der Waals materials by cross sectional scanning transmission electron microscopy“. Thesis, University of Manchester, 2017. https://www.research.manchester.ac.uk/portal/en/theses/characterisation-of-buried-interfaces-in-van-der-waals-materials-by-cross-sectional-scanning-transmission-electron-microscopy(dd5565b9-1709-4d28-b4ce-9cd675fb36eb).html.

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Graphene and other two-dimensional materials can be stacked together to form vander Waals heterostructures: synthetic crystals composed of different atomically thin layers with a bespoke electronic band structure. Structural characterisation of vander Waals heterostructures is difficult using conventional methods as the properties are almost entirely defined by the nature of the buried interfaces between dissimilar crystals. These methods also fall short of resolving the atomic structure of buried defects in van der Waals materials such as graphite. This work demonstrates the refinement and successful application of ion beam specimen preparation to produce cross sectional slices through these unique crystals so that they can be characterised by high resolution scanning transmission electron microscopy (STEM). Cross sectional specimen were prepared using in situ lift-out in a focused ion beam (FIB) dual-beam instrument. The fine polishing steps were optimised to prevent damage to the core of the specimen. High resolution STEM imaging of twin defects in graphene, hexagonal boron ni-tride and MoSe2 revealed that the boundaries are not atomically sharp but extended across many atoms. Advanced processing and analysis of these images uncovered fundamental mechanics which govern their geometry. This technique was further applied to complex transition metal dichalcogenide heterostructures to quantitatively determine the properties of buried interfaces between atomically thin crystals.

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Berlin, Katja. „In-situ transmission electron microscopy on high-temperature phase transitions of Ge-Sb-Te alloys“. Doctoral thesis, Humboldt-Universität zu Berlin, 2018. http://dx.doi.org/10.18452/19219.

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Das Hochtemperaturverhalten beeinflusst viele verschiedene Prozesse von der Materialherstellung bis hin zur technologischen Anwendung. In-situ Transmissionselektronenmikroskopie (TEM) bietet die Möglichkeit, die atomaren Prozesse während struktureller Phasenübergänge direkt und in Realzeit zu beobachten. In dieser Arbeit wurde in-situ TEM angewendet, um die Reversibilität des Schmelz- und Kristallisationsprozesses, sowie das anisotropen Sublimationsverhaltens von Ge-Sb-Te (GST) Dünnschichten zu untersuchen. Die gezielte Probenpräparation für die erfolgreiche Beobachtung der Hochtemperatur-Phasenübergänge wird hervorgehoben. Die notwendige Einkapselung für die Beobachtung der Flüssigphase unter Vakuumbedingungen und die erforderliche sauberer Oberfläche für den Sublimationsprozess werden detailliert beschrieben. Außerdem wird die Elektronenenergieverlustspektroskopie eingesetzt um die lokale chemische Zusammensetzung vor und nach den Übergängen zu bestimmen. Die Untersuchung der Grenzflächenstruktur und Dynamik sowohl beim Phasenübergang fest-flüssig als auch flüssig-fest zeigt Unterschiede zwischen den beiden Vorgängen. Die trigonale Phase von GST weist beim Schmelzen eine teilweise geordnete Übergangszone an der fest-flüssig-Grenzfläche auf, während ein solcher Zwischenzustand bei der Erstarrung nicht entsteht. Außerdem läuft der Schmelzvorgang zeitlich linear ab, während die Kristallisation durch eine Wurzelabhängigkeit von der Zeit mit überlagerter Start-Stopp-Bewegung beschrieben werden kann. Der Einfluss der Substrat-Grenzfläche wird diskutiert und die Oberflächenenergie von GST bestimmt. Die anisotrope Dynamik führt beim Phasenübergang fest-gasförmig der kubischen Phase von GST zur Ausbildung stabiler {111} Facetten. Dies erfolgt über die Bildung von Kinken und Stufen auf stabilen Terrassen. Die Keimbildungsrate und die bevorzugten Keimbildungsorte der Kinken wurden identifiziert und stimmen mit den Voraussagen des Terrassen-Stufen-Kinken Modells überein.
High-temperature behavior influence many different processes ranging from material processing to device applications. In-situ transmission electron microscopy (TEM) provides the means for direct observation of atomic processes during structural phase transitions in real time. In this thesis, in-situ TEM is applied to investigate the reversibility of the melting and solidification processes as well as the anisotropic sublimation behavior of Ge-Sb-Te (GST) thin films. The purposeful sample preparation for the successful observation of the high-temperature phase transitions is emphasized. The required encapsulation for the observation of the liquid phase inside the vacuum conditions and the necessary clean surface for sublimation process are discussed in detail. Additionally electron energy-loss spectroscopy in the TEM is used to determine the local chemical composition before and after the phase transitions. The analysis of the interface structure and dynamic during the solid-to-liquid as well as the liquid-to-solid phase transition shows differences between both processes. The trigonal phase of GST exhibits a partially ordered transition zone at the solid-liquid interface during melting while such an intermediate state does not form during solidification. Additionally the melting process proceeds with linear dependence on time, whereas crystallization can be described as having a square-root time-dependency featuring a superimposed start-stop motion. The influence of the interface is addressed and the surface energies of GST are determined. The anisotropic dynamic of the solid-to-gas phase transition of the cubic GST phase leads to the formation of stable {111} facets. This happens via kink and step nucleation on stable terraces. The nucleation rates and the preferred kink nucleation sites are identified and are in accordance with the predictions of terrace-step-kink model.

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Ben, ammar Hichem. „Investigation of ternary ΑlΙnΝ and quaternary ΑlGaΙnΝ alloys for high electron mobility transistors by transmission electron microscopy“. Thesis, Normandie, 2017. http://www.theses.fr/2017NORMC241/document.

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Les semi-conducteurs III-V à base d’azote et leurs alliages possèdent des propriétés remarquables et sont largement étudiés depuis les années 90. En comparaison à d'autres semi-conducteurs III-V, Les alliages de type ; AlGaN, InGaN et AlInN, ont leurs bandes interdites, directes, du lointain ultra-violet au proche infrarouge. Ainsi, ils sont appropriés pour de nombreuses applications dans des domaines tant civils que militaires tout en montrant de meilleures performances. De plus, l'alliage quaternaire AlGaInN montre des propriétés intéressantes car il peut être épitaxié soit avec un paramètre de maille ou une polarisation ou une bande interdite accordé au GaN. De plus, avec AlInN, ces deux alliages pourraient, à terme, remplacer les barrières conventionnelles AlGaN/GaN pour les applications aux Transistors à Haute Mobilité Électroniques (HEMT) grâce à des performances supérieures prouvées théoriquement.Dans ce travail, nous avons étudié les alliages AlInN et AlGaInN dont la croissance a été faite par épitaxie en phase vapeur d’organométalliques (MOVPE). Pour cela, la microscopie électronique en transmission a été notre principal outil de caractérisation. Le but était de caractériser les défauts et les mécanismes de croissance pendant la MOVPE. Dans cette optique, l'incorporation de gallium dans la barrière en raison de la géométrie de la chambre de croissance menant à un alliage quaternaire a été étudiée. Le contrôle du taux de gallium est réalisé soit par un processus de nettoyage entre les épitaxies soit par les conditions de croissance. Les défauts ont été ensuite différenciés comme extrinsèques et intrinsèques. En effet, les dislocations et les domaines d'inversion dans le GaN produisent des défauts extrinsèques, tandis que, les « pinholes » non connectés aux dislocations et les « hillocks » responsables de la rugosité de surface sont définis comme intrinsèques. Les origines des défauts intrinsèques dépendent fortement des propriétés physiques des composés parents binaires. Ces dégradations systématiques sont observées même lorsque les conditions de croissance sont optimisées et quand la composition du film mince est changée ou son épaisseur augmentée.Notre travail propose des mécanismes différents pour expliquer les processus de dégradation pour les différents défauts observés et constitue donc un pas en avant pour la réalisation de HEMT à base de AlInN et AlGaInN de meilleure qualité
Group III-Nitrides and their alloys exhibit outstanding properties and are being extensively investigated since the 90’s. In comparison to other III-V semiconductors, III-nitrides (AlGaN, InGaN, and AlInN) cover from deep ultraviolet (UV) to near infrared (IR) across the visible range of wavelengths. Thus, they are suitable for numerous applications both in civilian and military fields showing higher performances. Moreover, the quaternary alloy AlGaInN shows versatile properties as it can grow either lattice or polarization or bandgap matched to GaN. Alongside to AlInN, these two alloys are expected to replace conventional AlGaN/GaN High Electron Mobility Transistors (HEMT) barriers as higher performances have been theoretically demonstrated.In this work, we have studied AlInN and AlGaInN grown by metal organic vapor phase epitaxy (MOVPE) using mainly TEM. The aim was to characterize defects and the MOVPE growth alloying process. In this instance, the gallium incorporation in the barrier due to the geometry of the growth chamber leading to a quaternary alloy was studied. The control of the gallium content is achieved by a cleaning process between runs or by the growth condition. Defects were then differentiated as extrinsic and intrinsic. In this way, dislocations and inversion domains from the GaN buffer layer generate extrinsic defects, while, pinhole not connected to dislocations and individual hillocks responsible of surface roughening are termed as intrinsic. The origins of the latter defects depend strongly on the physical mismatches of the end-binary compound. These systematic degradations happen also with optimized growth conditions as soon as the nominal composition is changed and/or the thickness is increased.Our work proposes different mechanisms to explain defects generation processes which constitutes a forward step for higher quality HEMTs

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Hurm, Christian. „Towards an unambiguous electron magnetic chiral dichroism (EMCD) measurement in a transmission electron microscope (TEM)“. Berlin Logos-Verl, 2008. http://d-nb.info/992155444/04.

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Liu, Yang. „‘Tri-3D’ electron microscopy tomography by FIB, SEM and TEM : Application to polymer nanocomposites“. Thesis, Lyon, INSA, 2013. http://www.theses.fr/2013ISAL0076/document.

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Ce travail a porté sur la caractérisation et la quantification en 3D de la répartition de charges de différents types (nanoparticules, nanotubes, etc.) dans des matrices polymères. Nous nous focalisons sur les techniques de tomographie en microscopie électronique. Une approche multiple en tomographie électronique a été réalisée : la tomographie en FIB/MEB (faisceau d’ions focalisé/microscope électronique à balayage), la tomographie en MEB et la tomographie en MET (microscope électronique en transmission). Les nanocomposites polymère sont généralement élaborés aux fins d’améliorer les propriétés physiques (mécanique, électrique, etc.) du matériau polymère constituant la matrice, grâce à une addition contrôlée de charges nanométriques. La caractérisation de tels matériaux, et l’établissement de corrélations précises entre la microstructure et les propriétés d’usage, requièrent une approche tri-dimensionnelle. En raison de la taille nanométrique des charges, la microscopie électronique est incontournable. Deux systèmes de nanocomposite polymère ont été étudiés par une approche multiple de tomographie électronique : P(BuA-stat-S)/MWNTs (copolymère statistique poly (styrène-co-acrylate de butyl) renforcé par des nanotubes de carbone multi-parois), et P(BuA-stat-MMA)/SiO2 (copolymère statistique poly(butyl acrylate-co-methyl methacrylate) renforcé par des nanoparticules de silice). Par combinaison de divers techniques, la caractérisation et la quantification des nanocharges ont été possibles. En particulier, la taille, la fraction volumique et la distribution des charges ont été mesurées. Cette étude a ainsi fourni des informations en 3D qui contribuent à mieux comprendre les propriétés des nanocomposites. Une attention particulière a été portée aux artefacts et causes d’erreur possibles durant l’étape de traitement 3D. Nous avons également essayé de comparer les différentes techniques utilisées du point de vue de leurs avantages et inconvénients respectifs, en dégageant des possibilités d’amélioration future
This work is focused on the characterization and quantification of the 3D distribution of different types of fillers (nanoparticles, nanotubes, etc.) in polymer matrices. We have essentially used tomography techniques in electron microscopy. Multiple approaches to electron tomography were performed: FIB-SEM (focused ion beam/scanning electron microscope) tomography, SEM tomography and TEM (transmission electron microscope) tomography. Polymer nanocomposites are basically synthesized in order to improve the physical properties (mechanical, electric, etc.) of the pure polymer constituting the matrix, by a controlled addition of fillers at the nanoscale. The characterization of such materials and the establishment of accurate correlations between the microstructure and the modified properties require a three-dimensional approach. According to the nanometric size of the fillers, electron microscopy techniques are needed. Two systems of polymer nanocomposites have been studied by multiple electron tomography approaches: P(BuA-stat-S)/MWNTs (statistical copolymer poly(styrene-co-butyl acrylate) reinforced by multi-walled carbon nanotubes) and P(BuA-stat-MMA)/SiO2 (statistical copolymer poly(butyl acrylate-co-methyl methacrylate) reinforced by silica nanoparticles). By combining various techniques, the characterization and the quantification of nanofillers were possible. In particular, statistics about size, distribution and volume fraction of the fillers were measured. This study has then provided 3D information, which contributes to a better understanding of properties of the nanocomposites. Attention has been paid to analyze carefully original data, and artifacts and causes of errors or inaccuracy were considered in the 3D treatments. We also attempted to compare benefits and drawbacks of all techniques employed in this study, and perspectives for future improvements have been proposed

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Wang, Hao. „In-situ transmission electron microscopy investigation of deformation-induced microstructural evolution of a FeCoCrNiMn high-entropy alloy“. Thesis, The University of Sydney, 2018. http://hdl.handle.net/2123/20068.

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High-entropy alloys (HEAs) are alloys with multiple (usually ≥5) principal elements. HEAs are attracting increasing interest because of their promising mechanical properties and phase stability, which can be used for various applications, such as high-speed cutting tools, anticorrosive high-strength parts in chemical plants and deep-sea exploration due to the excellent mechanical properties at cryogenic temperatures. Thorough understanding of the structural evolution during deformation of HEAs is a prerequisite for understanding and further improving their superior mechanical properties, which is critical for future production of high-entropy alloys with desirable properties. Many HEAs form a stable single solid-solution phase. However, phase transformation could occur in some HEAs under certain circumstances, including high stress. Because stress concentration usually occurs at crack tips during deformation, it is interesting to check if any deformation-induced phase transformation would occur at crack tips during the deformation processes of HEAs. This thesis aims at using various transmission electron microscopy techniques to investigate the structural evolution of HEAs at room temperature. Research results showed surprisingly crystalline to amorphous phase transformation at crack tips in a FeCoCrNiMn HEA with an ultrafine-grained structure. Details of the phase transformation process was video recorded. The mechanism responsible for the phase transformation is discussed based on the observed microstructural evolution. Toughening introduced by nanobridging and the phase transformation is also briefly discussed.

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Berthier, Rémy. „Development of characterization methods for in situ annealing and biasing of semiconductor devices in the TEM“. Thesis, Université Grenoble Alpes (ComUE), 2018. http://www.theses.fr/2018GREAY014/document.

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Dans cette thèse, nous abordons les défis rencontrés lors de la caractérisation des mémoires non volatiles par microscopie en transmission in situ. Les innovations récentes menées sur les porte-objets de TEM in situ basés sur l'utilisation de puces en silicium apportent de grands avantages comparée aux précédents modèles. Cependant, cette technique reste complexe et les expériences de MET in situ sont difficiles à mener à terme. Ce manuscrit tente d'apporter de nouvelles solutions pour permettre l'observation à l'échelle atomique pendant le recuit, ou la polarisation d'un échantillon dans le MET. Ce projet a été mené à travers plusieurs améliorations effectuées au cours des différentes étapes des expériences de MET in situ. Cette thèse se focalise plus particulièrement sur les problèmes rencontrés lors de la polarisation de dispositifs de mémoires résistives de taille nanométrique. Ces travaux furent conduits à travers une étude des instruments utilisés, le développement de nouvelles méthodes de préparation d'échantillons, et une analyse de l'impact de l'imagerie électronique sur le fonctionnement d'un dispositif dans le MET.Tout d’abord, une nouvelle méthode est développée spécifiquement pour les expériences de MET in situ en température. Grâce à ces développements, la cristallisation de mémoires à changement de phase en GeTe est observée en temps réel. Ces résultats ont notamment permis d'obtenir des informations utiles pour le développement de mémoires à changement de phase de type chalcogénure. Ensuite, de nouvelles puces en silicium dédiées à la polarisation in situ sont développées et produites. Une étude est ensuite menée sur la préparation d'échantillons par FIB afin d'améliorer la qualité des contacts électriques pour la polarisation in situ, ainsi que la technique de préparation elle-même. La qualité de cette méthode est ensuite démontrée à travers des mesures quantitatives obtenues pendant la polarisation in situ d'un échantillon de référence de type jonction PN. Ces développements sont ensuite appliqués afin d’observer des dispositifs de mémoires résistives de type CBRAM en fonctionnement dans le microscope électronique en transmission. Ces résultats ont permis d'apporter de nouvelles informations sur les mécanismes de fonctionnement des mémoires résistives, ainsi que sur la technique de polarisation in situ
In this work, we address the current challenges encountered during in situ Transmission Electron Microscopy characterization of emerging non volatile data storage technologies. Recent innovation on in situ TEM holders based on silicon micro chips have led to great improvements compared to previous technologies. Still, in situ is a particularly complicated technique and experiments are extremely difficult to implement. This work provides new solutions to perform live observations at the atomic scale during both heating and biasing of a specimen inside the TEM. This was made possible through several improvements performed at different stages of the in situ TEM experiments. The main focus of this PhD concerned the issues faced during in situ biasing of a nanometer size resistive memory device. This was made possible through hardware investigation, sample preparation method developments, and in situ biasing TEM experiments.First, a new sample preparation method has been developed specifically to perform in situ heating experiments. Through this work, live crystallization of a GeTe phase change Memory Material is observed in the TEM. This allowed to obtain valuable information for the development of chalcogenide based Phase Change Resistive Memories. Then, new chips dedicated to in situ biasing experiments have been developed and manufactured. The FIB sample preparation is studied in order to improve electrical operation in the TEM. Quantitative TEM measurements are then performed on a reference PN junction to demonstrate the capabilities of this new in situ biasing experimental setup. By implementing these improvements performed on the TEM in situ biasing technique, results are obtained during live operation of a Conductive Bridge Resistive Memory device. This allowed to present new information on the resistive memories functioning mechanisms, as well as the in situ TEM characterization technique itself

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Park, Chun-sŏk. „Structural characterization of hard materials by transmission electron microscopy (TEM) : diamond-silicon carbide composites and yttria-stabilized zirconia /“. May be available electronically:, 2008. http://proquest.umi.com/login?COPT=REJTPTU1MTUmSU5UPTAmVkVSPTI=&clientId=12498.

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Melinte, Georgian. „Advanced 3D and in-situ TEM approaches applied to carbon-based and zeolitic nanomaterials“. Thesis, Strasbourg, 2015. http://www.theses.fr/2015STRAE009/document.

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Dans le cadre de cette thèse, des techniques avancées de Microscopie électronique à transmission (MET)ont été utilisées dans le but de caractériser et de fabriquer de nouveaux nanomatériaux pour des applications dans les domaines de la nanoélectronique et de la catalyse. Trois types de matériaux fonctionnalisés sont étudiés: le graphène multifeuillets (FLG– Few-Layer Graphene) avec des nanomotifs,des nanotubes de carbone (CNTs - Carbon Nanotubes en anglais) et des zéolithes mésoporeux. La formation de nanomotifs de tranchées et de tunnels sur des flocons de FLG à l’aide de nanoparticules(NPs) de fer est étudiée dans une approche qui combine la tomographie électronique et la MET environnementale. Le rôle des facettes de la nanoparticule et des paramètres topographiques de FLG a été déterminé du point de vue quantitatif, ce qui a mené à la mise en évidence du mécanisme de formation des nanomotifs de tranchées et de tunnels. Le transfert de nanoparticules à base de métal entre deux nanostructures de carbone a été également étudié, en temps réel, en employant un porte-échantillon MET couplé avec un dispositif STM (Scanning Tunneling Microscope en anglais). Le protocole de contrôle du transfert des nanoparticules, les transformations chimiques et structurales subies par celles-ci, le mécanisme de croissance de nouvelles nanoparticules et d’autres phénomènes liés à ces effets ont été étudiés avec attention. La dernière partie de la thèse est centrée sur l’étude de la tomographie électronique à faible dose de la porosité induite dans deux classes de zéolithes, ZSM-5 et zéolithe Y, en utilisant un traitement chimique novateur à base de fluor
In this thesis, advanced Transmission Electron Microscopy (TEM) techniques are used to characterize and fabricate new nanomaterials with applications in nanoelectronics and catalysis. Three types of functionalized materials are investigated: nanopatterned few-layer graphene (FLG), carbon nanotubes(CNTs) and mesoporous zeolites. The nanopatterning process of FLG flakes by iron nanoparticles (NPs) is studied using an approach combining electron tomography (ET) and environmental TEM. The role of the nanoparticle faceting and of the FLG topographic parameters has been quantitatively determined leading to the first determination of the operating mechanism of the patterning process. The mass transfer of metallic-based NPs between two carbon nanostructures was studied as well in real-time by using a TEMSTMholder. The protocol of controlling the mass transfer, the chemical and structural transformations of the NPs, the growth mechanism of the new NPs and other related phenomena were carefully investigated.The last part deals with the low-dose ET investigation of the porosity induced in two classes of zeolites,ZSM-5 and zeolite Y, by an innovative fluoride-based chemical treatment

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Haddad, Farah. „Transmission electron microscopy study of low-temperature silicon epitaxy by plasma enhanced chemical vapor deposition“. Thesis, Université Paris-Saclay (ComUE), 2016. http://www.theses.fr/2016SACLX107/document.

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Cette thèse s’intéresse à la croissance épitaxiale à basse température (~200°C) des couches minces de silicium par dépôt chimique en phase vapeur assisté par plasma (PECVD), pour des applications aux cellules solaires. L’objectif de départ était de mieux comprendre cette croissance épitaxiale, en utilisant la microscopie électronique en transmission (MET) comme principal outil expérimental. D’abord, nous avons étudié les premiers stades de cette croissance épitaxiale en chimie SiF4/H2/Ar, en menant une série de dépôts courts – quelques dizaines jusqu’à quelques centaines de secondes – sur différents types de substrats. Nous avons établi une corrélation entre les images MET de coupes et de vues planes et les mesures d’ellipsométrie in-situ. Nous avons discuté les mécanismes de croissance en nous basant sur l’hypothèse de la croissance traditionnelle à base d’atomes, radicaux et ions et l’hypothèse (relativement nouvelle) reposant sur la fonte des nanoparticules générées par le plasma au moment de l’impact avec le substrat. De plus, pour comprendre comment l’épitaxie par PECVD à basse température se maintient, nous avons étudié comment elle se brise ou se perd. Pour cela, des expériences de perte d’épitaxie ont été visées en augmentant soit la puissance de la source RF, soit le flux d’hydrogène, toujours pour une chimie SiF4/H2/Ar. Dans les deux cas, le mécanisme de brisure d’épitaxie fait intervenir des macles et des fautes d’empilement qui interrompent la configuration épitaxiale ; ceci est accompagné par une rugosification de surface. Grâce à cette nouvelle compréhension de la brisure d’épitaxie, nous proposons quelques moyens pour maintenir l’épitaxie pour de plus grandes épaisseurs. En outre, nous avons observé une fascinante quasi-symétrie cinq dans les diagrammes de diffraction pour ces couches et aussi pour d’autres élaborées par un plasma de chimie SiH4/H2/HMDSO/B2H6/Ar. Nous avons attribué une telle symétrie à une brisure d’épitaxie par l’intermédiaire d’un maclage multiple. Nous avons développé une méthode d’analyse quantitative qui permet de discriminer les positions de maclage de celles du microcristal aléatoire dans les diagrammes de diffraction et d’estimer le nombre des opérations de maclage. Nous avons aussi discuté quelques raisons probables pour l’incidence du maclage et du maclage multiple sous forme de symétrie cinq. Finalement, une importante réalisation pour le monde de la MET, durant ce travail doctoral, a été l’optimisation de la préparation traditionnelle d’échantillon (polissage par tripode). Nous l’avons transformée d’une méthode longue et ennuyeuse en une méthode rapide qui devient compétitive par rapport à la technique du FIB relativement chère
This thesis focuses on low temperature (LT, ~200°C) epitaxial growth of silicon thin films by plasma enhanced chemical vapor deposition (PECVD) for solar cell applications. Our starting goal was to acquire a better understanding of epitaxial growth, by using transmission electron microscopy (TEM) as the main experimental tool. First, we investigated the initial stages of epitaxial growth using SiF4/H2/Ar chemistry by performing a series of short depositions – from few tens to few hundred of seconds – on different types of substrates. We made a correlation between cross-sectional and plan-view TEM images and in-situ ellipsometry measurements. We discussed the growth mechanisms under the hypotheses of the traditional growth mediated by atoms, radicals and ions and the relatively new approach based on the melting of plasma generated nanoparticles upon impact with the substrate. Additionally, in order to understand how epitaxy by LT-PECVD is sustained, we studied how it is lost or how it breaks down. For that, experiments of intentional breakdown of epitaxy were performed by either increasing the RF power or the hydrogen flow rate using the same SiF4/H2/Ar chemistry. In both cases, the breakdown mechanism was based on the development of twins and stacking faults thus disrupting epitaxial configuration; this was accommodated with surface roughening. Thanks to this new understanding of epitaxy breakdown, we can propose some ways to sustain epitaxy for higher thicknesses. Moreover, we fascinatingly observed a quasi-fivefold symmetry in the diffraction patterns for these layers and for layers deposited using SiH4/H2/HMDSO/B2H6/Ar plasma chemistry as well. We attributed such symmetry to the breakdown of epitaxy through multiple twinning. We developed a quantitative analysis method to discriminate twin positions from random microcrystalline ones in the diffraction patterns and to estimate the number of twin operations. We also discussed some probable reasons for the occurrence of twinning and multiple twinning in a fivefold symmetry fashion. Finally, one important achievement to the TEM world is the optimization, during this doctoral work, of the traditional TEM sample preparation (tripod polishing), transforming it from a long and boring method to a fast method that is competitive with the relatively expensive focus ion beam (FIB) technique

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Kylberg, Gustaf. „Automatic Virus Identification using TEM : Image Segmentation and Texture Analysis“. Doctoral thesis, Uppsala universitet, Avdelningen för visuell information och interaktion, 2014. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-217328.

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Viruses and their morphology have been detected and studied with electron microscopy (EM) since the end of the 1930s. The technique has been vital for the discovery of new viruses and in establishing the virus taxonomy. Today, electron microscopy is an important technique in clinical diagnostics. It both serves as a routine diagnostic technique as well as an essential tool for detecting infectious agents in new and unusual disease outbreaks. The technique does not depend on virus specific targets and can therefore detect any virus present in the sample. New or reemerging viruses can be detected in EM images while being unrecognizable by molecular methods. One problem with diagnostic EM is its high dependency on experts performing the analysis. Another problematic circumstance is that the EM facilities capable of handling the most dangerous pathogens are few, and decreasing in number. This thesis addresses these shortcomings with diagnostic EM by proposing image analysis methods mimicking the actions of an expert operating the microscope. The methods cover strategies for automatic image acquisition, segmentation of possible virus particles, as well as methods for extracting characteristic properties from the particles enabling virus identification. One discriminative property of viruses is their surface morphology or texture in the EM images. Describing texture in digital images is an important part of this thesis. Viruses show up in an arbitrary orientation in the TEM images, making rotation invariant texture description important. Rotation invariance and noise robustness are evaluated for several texture descriptors in the thesis. Three new texture datasets are introduced to facilitate these evaluations. Invariant features and generalization performance in texture recognition are also addressed in a more general context. The work presented in this thesis has been part of the project Panvirshield, aiming for an automatic diagnostic system for viral pathogens using EM. The work is also part of the miniTEM project where a new desktop low-voltage electron microscope is developed with the aspiration to become an easy to use system reaching high levels of automation for clinical tissue sections, viruses and other nano-sized particles.

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Nováková, Kateřina. „Využitie slepej filtrácie obrazu pre snímky z TEM mikroskopov“. Master's thesis, Vysoké učení technické v Brně. Fakulta elektrotechniky a komunikačních technologií, 2018. http://www.nusl.cz/ntk/nusl-377660.

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Předložená práce se zabývá problematikou slepé filtrace obrazů z transmisního elektronového mikroskopu. V úvodu práce je uveden popis transmisního elektronového mikroskopu. Navazující část popisuje mechanismy interakce elektronů se zkoumaným vzorkem a z toho vyplývající zobrazovací techniky elektronové mikroskopie. Poslední kapitola teoretické části práce zahrnuje popis vybraných metod slepé filtrace obrazu zejména s využitím dekompozice obrazu na charakteristické složky. Taktéž je zde uveden výčet metod pro zhodnocení úspěšnosti filtrace. V praktické části jsou popsány aplikované metody slepé filtrace obrazů a výsledky filtrování. Jednotlivé metody jsou mezi sebou porovnány. Získané výsledky a využitelnost aplikovaných metod jsou zhodnoceny v diskuzi.

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Amaduci, Marcia Regina Lombardo. „Efeitos do campo eletromagnetico em celulas e bacterias“. [s.n.], 2007. http://repositorio.unicamp.br/jspui/handle/REPOSIP/259947.

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Orientador: Vitor Baranauskas
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Eletrica e de Computação
Made available in DSpace on 2018-08-11T09:59:32Z (GMT). No. of bitstreams: 1 Amaduci_MarciaReginaLombardo_M.pdf: 2445338 bytes, checksum: 4bb1cb55957a33fb2a440282e189204d (MD5) Previous issue date: 2007
Resumo: Este trabalho refere-se a alguns efeitos de um campo eletromagnético aplicados em colônias bacterianas. A bactéria escolhida é bastante conhecida no mundo científico e tratase da Escherichia coli (E. coli). A parte experimental divide-se entre a análise quantitativa, qualitativa e morfológica sobre o ciclo de vida da E. coli. O circuito eletromagnético foi gerado a partir de uma freqüência de 60Hz. Durante um período de 18h, as bactérias acopladas ao circuito eletromagnético se proliferaram em meio aquoso e a cada fase do ciclo de vida da E. coli, foram realizadas diluições em tubos de ensaio para a análise da absorbância e contagem de bactérias viáveis. Ao mesmo tempo foram colocados em uma estufa, na mesma temperatura do circuito, tubos contendo a mesma amostra em quantidade e qualidade, para uma análise paralela do seu ciclo de vida. O trabalho inclui análise morfológica, com a utilização da microscopia eletrônica de transmissão (MET) e da microscopia eletrônica de varredura (MEV)
Abstract: This research work studies some effects of an electromagnetic field applied on bacteria. The chosen bacterium is quite known in the scientific world, the Escherichia coli (E. coli). The experimental part was divided into the quantitative, qualitative and morphologic analysis on the life of bacterium Escherichia coli. The electromagnetic circuit was generated from a frequency of 60Hz. During a period of 18h, the bacteria connected to the electromagnetic circuit proliferated in watery way, and for each phase of the life cycle of E. coli LT1, dilutions in test tube were performed for the analysis of the absorbancy and counting of viable bacteria. At the same time, other test tubes holding the same sample in amount and quality were placed in a incubator, at the same temperature of the circuit, for a parallel analysis of its cycle of life. The work includes morphologic analysis, with the use of transmission electronic microscopy (TEM), and scanning electronic microscopy (SEM)
Mestrado
Eletrônica, Microeletrônica e Optoeletrônica
Mestre em Engenharia Elétrica

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Lin, Hong. „Etude couplée par TEM/EELS et STM/STS des propriétés structurales et électroniques des nanotubes C et CNx“. Paris 6, 2009. http://www.theses.fr/2009PA066494.

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Ce travail de thèse est dédié à l’étude couplée par TEM/EELS et STM/STS des propriétés structurales et électroniques des nanotubes de carbone purs et des nanotubes dopés à l’azote. Nous mettons d’abord en évidence le rôle des effets à N corps sur les spectres électroniques des tubes mesurés par STS et l’influence du substrat métallique. Ensuite nous présentons une étude systématique des fonctions d’ondes électroniques dans les tubes associées aux singularités de Van-Hove. Nous avons mis en évidence la brisure de symétrie de ces états qui est bien décrite par un modèle de liaisons fortes et qui a été confirmée par des calculs ab-initio. La dernière partie concerne l’étude de nanotubes dopés par des atomes d’azote. Des mesures de EELS montrent la présence d’azote dans les tubes et permet d’identifier des liaisons de type pyridinique. Les mesures STM font apparaître plusieurs défauts. Au final nous proposons que les atomes d’azote soient généralement accompagnés de défauts structuraux.

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Nemavhulani, Shonisani. „Bacteriophage diversity in haloalkaline environments“. University of the Western Cape, 2013. http://hdl.handle.net/11394/4313.

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>Magister Scientiae - MSc
There are limited reports on virus population in haloalkaline environments; therefore the aim of this study was to investigate the genetic diversity and biology of bacteriophage communities in these environments. Bacteria were isolated to be used as phage hosts. One bacterium from Lake Magadi and four bacteria from Lake Shala were successfully isolated from sediment samples. A further two Lake Shala bacterial hosts from the IMBM culture collection were also used to isolate bacteriophages. Bacterial isolates were identified to be most closely related to Bacillius halodurans, Halomonas axialensis, Virgibacillus salarius, Bacillus licheniformis, Halomonas venusta, Bacillus pseudofirmus and Paracoccus aminovorans. Bacteriophages were screened using all bacteria against sediment samples from both Lake Shala and Lake Magadi. One phage was identified from Lake Magadi sediments (MGBH1) and two phages from Lake Shala sediments (SHBH1 and SHPA). TEM analysis showed that these phages belong to three different dsDNA phage families; Siphoviridae (MGBH1), Myoviridae (SHBH1) and Podoviridae (SHPA). All phages showed different genome sizes on agarose gel. Due to the small genome size, phage SHPA was chosen for further investigation. Partial, genome sequence analysis showed homology to both bacterial and phage proteins. A further investigation of phage diversity in this environment is essential using metagenomic approaches to understand these unique communities.

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Stempinski, Erin S. „SYN3 in Chloroplasts of Arabidopsis thaliana: Effects of Knockdown and Overexpression and Localization Techniques“. Miami University / OhioLINK, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=miami1376057385.

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Yoo, Kyung-Dong. „Two-dimensional dopant profiling for shallow junctions by TEM and AFM“. Thesis, University of Oxford, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.342122.

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Lidbaum, Hans. „Transmission Electron Microscopy for Characterization of Structures, Interfaces and Magnetic Moments in Magnetic Thin Films and Multilayers“. Doctoral thesis, Uppsala universitet, Experimentell fysik, 2009. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-107941.

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Structural characterization is essential for the understanding of the magnetic properties of thin films and multilayers. In this thesis, both crystalline and amorphous thin films and multilayers were analyzed utilizing transmission electron microscopy (TEM). High resolution TEM and electron diffraction studies emphasize on the growth of amorphous Fe91Zr9 and Co68Fe24Zr8 on both Al2O3 and Al70Zr30 in multilayer structures by magnetron sputtering. The properties of the growth surfaces were found to strongly influence the formation of nano-crystallites of the magnetic material at interfaces. Field induced uniaxial magnetic anisotropy was found to be possible to imprint into both fully amorphous and partially crystallized Co68Fe24Zr8 layers, yielding similar magnetic characteristics regardless of the structure. These findings are important for the understanding of both growth and magnetic properties of these amorphous thin films. As magnetic systems become smaller, new analysis techniques need to be developed. One such important step was the realization of electron energy-loss magnetic circular dichroism (EMCD) in the TEM, where information about the ratio of the orbital to spin magnetic moment (mL/mS) of a sample can be obtained. EMCD makes use of angular dependent inelastic scattering, which is characterized using electron energy-loss spectroscopy. The work of this thesis contributes to the development of EMCD by performing quantitative measurements of the mL/mS ratio. Especially, methods for obtaining energy filtered diffraction patterns in the TEM together with analysis tools of the data were developed. It was found that plural inelastic scattering events modify the determination of the mL/mS ratio, wherefore a procedure to compensate for it was derived. Additionally, utilizing special settings of the electron gun it was shown that EMCD measurements becomes feasible on the nanometer level through real space maps of the EMCD signal.

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Cikánek, Martin. „Detekce biologických struktur ve snímcích z TEM mikroskopu“. Master's thesis, Vysoké učení technické v Brně. Fakulta elektrotechniky a komunikačních technologií, 2019. http://www.nusl.cz/ntk/nusl-400528.

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The aim of the first part of this thesis is to explain the theoretical basis of transmission electron microscopy and to mention fundamental parts of transmission electron microscopes. The next part of this work is focused on possible methods of image segmentation, the use of neural networks in the detection of objects in an image and the subsequent clustering of results. The theoretical part of the thesis is concluded with an explanation of some already published methods of automatic detection of biological structures in microscopic images and theoretical design of the algorithm, which will be subsequently developed. The process of training neural networks in order to automatically detect biological structures in an image is described at the beginning of the practical part. This is followed by an evaluation of the results achieved by these networks. Subsequently, cluster analysis methods are applied to these results, the products of which are compared with each other and also with the results obtained by already published methods.

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Cenker, Emre. „Imaging measurements of soot particle size and soot volume fraction with laser-induced incandescence at Diesel engine conditions“. Thesis, Châtenay-Malabry, Ecole centrale de Paris, 2014. http://www.theses.fr/2014ECAP0049/document.

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Le travail présenté dans ce manuscrit concerne les mesures de taille de particule et de fraction volumique de suies dans des conditions moteur Diesel. Les techniques utilisées sont la laser-Induced incandescence (LII), la méthode d’extinction laser (LEM), la pyrométrie, et l’analyse d’images de microscopie électronique par transmission (TEM) d’échantillons prélevés in-Situ. Des stratégies de mesure de tailles de particules sont développées en se basant sur l’utilisation d’un modèle LII et en analysant la poly-Dispersion des tailles de particules, aussi bien à partir de signaux de LII résolu en temps (mesures ponctuelles) à pression atmosphérique, que d’informations résolues spatialement provenant d’images acquises a deux instants différents. Des mesures sont effectuées avec ces stratégies sur une flamme à pression atmosphérique et dans des conditions représentatives des conditions moteur Diesel pour évaluer leur applicabilité. Des mesures supplémentaires de température et de fraction volumique de suies sont aussi réalisés.Une nouvelle méthode, appelée two-Exponential reverse fitting (TERF) est introduite. Elle vise à extraire des informations sur la distribution de tailles de particules. Cette méthode est basée sur l’utilisation de fits mono-Exponentiel du signal de décroissance de LII à différents intervalles de temps. La distribution de tailles de particules est approximée par la combinaison de deux distributions de tailles de particules mono-Disperses : une petite et une large. Aucune hypothèse sur la forme de la distribution n’est nécessaire. La méthode permet aussi de fournir le ratio de la proportion respective des deux classes de particules. L’erreur systématique induite par la description mono-Exponentielle de la décroissance du signal de LII a été calculée et est inférieure à 2% pour des décroissances de signal de LII d’aggregats mono-Disperses avec des températures de chauffe pour lesquels la sublimation des suies est négligeable. La méthode a été appliquée à des données de LII obtenus sur une flamme laminaire atmosphérique éthylene/air à différentes hauteurs. Les résultats obtenus montrent un bon accord entre les tailles des grosses particules évaluées avec la méthode TERF et celle obtenue par analyse des images TEM. En revanche l’accord n’est pas obtenu pour les petites particules, ce qui est attribué à un manque d’information sur cette classe de particule dans l’analyse TEM.Des champs de fraction volumique de suies sont ensuite obtenus dans une cellule haute pression haute température dans les conditions opératoires du réseau ECN (Engine Combustion Network) par technique combinée de LEM et LII simultanées. Les mesures sont réalisées dans les conditions du spray A et incluent des variations paramétriques (température et dilution). La distance de Lift Off de la flamme est déterminée en parallèle par visualisation directe de la chimiluminescence OH. Des niveaux de fraction volumique maximale de 2-3ppm sont obtenus dans les conditions nominales du spray A (i.e. 900K), et peuvent atteindre 12 pmm à haute température (1030K). L’effet des variations de température et de concentration d’oxygène sur la formation et l’oxydation des suies et cohérente avec les résultats issus de la littérature.Une méthode d’imagerie de taille de particules est développée. Elle est basée sur l’acquisition de deux images de LII obtenues à deux instants différents après le pulse laser et l’analyse de ces images à l’aide de la simulation du signal LII pour déduire les tailles des particules à partir du rapport des images. Une stratégie basée sur une analyse par modèle LII est développée pour évaluer les incertitudes de mesure. La dépendance aux conditions limites de l’imagerie de taille de particule par LII est ainsi évaluée. [...]
This work focuses on measurements of soot particle size and volume fraction at Diesel engine conditions. A combination of laser-Induced incandescence (LII) imaging, line-Of-Sight laser extinction, soot pyrometry, and transmission electron microscopy (TEM) measurements of thermophoretically-Sampled soot was used. Particle sizing strategies were developed with LII model for the analysis of particle-Size poly-Dispersity with time-Resolved LII signal that is suitable for point-Wise measurements at atmospheric pressure, and for spatially-Resolved characterization with two-Time-Step LII imaging. Measurements were performed with these strategies in a flame at atmospheric pressure and in Diesel engine combustion to investigate their applicability. Additional measurements were performed for temperature and soot volume fraction.A novel method, called two-Exponential reverse fitting (TERF), is introduced to extract information about the size distribution. The method is based on mono-Exponential fits to the LII signal decay at a delayed time. It approximates the particle-Size distribution as a combination of one large and one small mono-Disperse equivalent mean particle size and does not require a distribution assumption. It also provides a ratio of the contribution of both size classes. The systematic error caused by de-Scribing LII signals by mono-Exponential decays was calculated as less than 2% for LII signals simulated for mono-Disperse aggregated soot with heat-Up temperatures for which evaporation is negligible. The method was applied to LII data acquired in a laminar non-Premixed ethylene/air flame at various heights above the burner. The particle size of the large particle-Size class evaluated with the method showed good consistency with TEM results, however the size of the small particle-Size class and its relative contribution could not be compared due to insufficient information in the TEM results for small particles. Simultaneous line-Of-Sight laser extinction measurements and LII imaging were performed to de-Rive the soot volume fraction in a high-Temperature high-Pressure constant-Volume pre-Combustion vessel under the Engine Combustion Network’s (ECN) "Spray A" conditions with parametric variations of gas temperature and composition. Extinction measurements were used to calibrate LII images for quantitative soot distribution measurements. OH-Chemiluminescence imaging was used to determine the lift-Off length, and used to interpret the soot measurements. Maximum soot volume fractions around 2–3 ppm were obtained at the nominal ambient temperature defined for Spray A (i.e. 900 K) that rise to 12 ppm at elevated temperature (1030 K). Variations of ambient temperature and oxygen concentration were carried out showing effects on soot formation and oxidation that are consistent with the literature.The method for particle-Size imaging is based on evaluating gated LII signals acquired with two cameras consecutively after the laser pulse and using LII modeling to deduce particle size from the ratio of local signals. A strategy was developed with a model-Based analysis: the dependence of LII particle-Size imaging on the assumed boundary conditions was identified such as bathgas temperature, pressure, particle heat-Up temperature, thermal accommodation coefficients, and soot morphology. Various laser-Fluence regimes and gas pressures were considered. Effects of laser attenuation were evaluated. A combination of one detection gate starting with the particle-Heating and the other starting with 11 ns delay with twice as long gate width was found to provide the highest sensitivity for particle sizing at 60 bar. The optimum gate delays for different pressures were calculated. The effects of timing jitter for laser pulse and poly-Dispersity were investigated. Systematic errors in pyrometry imaging at 60 bar was evaluated. [...]

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Andersen, Ingrid Marie. „2D and 3D quantitative TEM mapping of CoNi nanowires“. Thesis, Toulouse 3, 2020. http://www.theses.fr/2020TOU30205.

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Les nanofils magnétiques constituent un domaine de recherche en plein essor. De section cylindrique, ils permettent la propagation des parois de domaines magnétiques à très grandes vitesses et des interactions fortes avec les ondes de spin, ce qui les rend particulièrement intéressants pour le développement de futurs composants de la spintronique. L'objectif de ce travail de thèse est de fournir une analyse quantitative et qualitative complète de la configuration magnétique locale dans des nanofils magnétiques cylindriques d'alliage CoNi à anisotropie magnétocristalline perpendiculaire en utilisant les techniques d'imagerie magnétique avancées de la microscopie électronique à transmission (MET), principalement axées sur l'holographie électronique (HE). Une étude corrélative entre les propriétés structurales, les variations locales de composition et les configurations magnétiques de ces nanofils a été réalisée. De plus, les configurations tridimensionnelles (3D) complexes des domaines et des parois magnétiques ont été analysées par tomographie holographique de champ vectoriel (THCV) afin d'obtenir les trois composantes de l'induction magnétique. Enfin, un protocole a été développé pour étudier in situ par microscopie de Lorentz la configuration magnétique de ces nanofils lors de l'injection d'impulsions de courant. La première partie de ce travail est focalisée sur la corrélation des configurations magnétiques de nanofils individuels de CoNi avec les propriétés structurales et chimiques locales. L'orientation de la phase cristalline a été cartographiée en diffraction électronique par précession et combinée à des mesures de composition par spectroscopie de perte d'énergie des électrons. Les résultats révèlent une coexistence de grains de phase cfc et de phase hcp, cette dernière présente sa direction cristallographique c orientée presque perpendiculairement à l'axe du nanofil. Cette coexistence de phases cristallographiques est à l'origine de variations localisées et abruptes de la configuration magnétique. Deux nanofil configurations principales ont été observées : une chaîne d'états transversaux par rapport à l'axe du, de type vortex, et un état longitudinal. Nous avons observé que les états transversaux sont liés à la phase hcp possédant une forte anisotropie magnétocristalline perpendiculaire, ce que confirment les simulations micromagnétiques. Une autre partie de ce travail concerne l'étude de la structure magnétique 3D des domaines et des parois de domaines dans la phase hcp. Cette étude a été menée pour des états rémanents différents en fonction de l'application d'un champ de saturation perpendiculaire et parallèle à l'axe du nanofil. Les mesures ont été réalisées par la méthode THCV afin d'extraire les trois composantes de l'induction magnétique et reconstruire en 3D la configuration magnétique locale du nanofil. Les résultats montrent une stabilisation d'une chaîne de vortex dans le cas d'une saturation perpendiculaire, et des états d'enroulement longitudinaux séparés par des parois de domaine transversales après l'application d'un champ externe parallèle à l'axe du fils. La dernière partie du manuscrit présente les résultats obtenus en microscopie de Lorentz in situ démontrant la possibilité de manipuler les parois des domaines magnétiques d'un nanofil de CoNi par injection d'impulsions électriques. Cette preuve de concept est considérée comme le précurseur des observations in situ de la dynamique des parois de domaines en EH. Un protocole précis, axé sur les étapes cruciales de préparation des échantillons et les développements à poursuivre pour réaliser ces expériences délicates, est détaillé
Cylindrical magnetic nanowires (NWs) are currently subjects of high interest due to fast domain wall velocities and interaction with spin-waves, which are considered interesting qualities for developing future spintronic devices. This thesis aims to provide a wholesome quantitative and qualitative analysis of the local magnetic configuration in cylindrical Co-rich CoNi NWs with perpendicular magnetocrystalline anisotropy using state-of-the-art transmission electron microscopy (TEM) magnetic imaging techniques, mainly focused on two-dimensional (2D) and three-dimensional (3D) electron holography (EH). A correlative study between the NW's texture, modulation in composition, and magnetic configuration has been conducted. Further, the complex 3D nature of the domain and domain wall configurations have been analyzed using holographic vector field electron tomography (VFET) to retrieve all three components of the magnetic induction. Finally, I have successfully manipulated the magnetic configuration observed by Lorentz microscopy in Fresnel mode by the in situ injection of a current pulse. A TEM study comparing the magnetic configuration to the local NW structure was performed on single NWs. The crystal phase analysis was done by precession electron diffraction assisted automated crystal orientation mapping in the TEM combined with compositional analysis by scanning-TEM (STEM) electron energy loss spectroscopy (EELS) for a detailed correlation with the sample's magnetic configuration. The results reveal a coexistence of fcc grains and hcp phase with its c-axis oriented close to perpendicular to the wire axis in the same NW, which is identified as the origin of drastic local changes in the magnetic configuration. Two main configurations are observed in the NW region: a chain of transversal vortex-like states and a longitudinal curling state. The chain or vortices are linked to the hcp grain with the perpendicular magnetocrystalline anisotropy, as confirmed by micromagnetic simulations. The 3D magnetic structure of the domains and domain walls observed in the hcp grain of the NWs has been studied for two different remnant states: after the application of a saturation field perpendicular (i) and parallel (ii) to the NW axis. The measurements were done using state-of-the-art holographic VFET to extract all three components of the magnetic induction in the sample, as well as a 3D reconstruction of the volume from the measured electric potentials, giving insight into the local morphology of the NW. The results show a stabilization of a vortex chain in the case of perpendicular saturation, but longitudinal curling states separated by transversal domain walls after applying a parallel external field. Finally, preliminary Lorentz microscopy results are presented, documenting the manipulation of magnetic domain walls by the in situ injection of electrical pulses on a single cylindrical CoNi nanowire contacted by focused ion beam induced deposition. This is believed to be the forerunner for quantitative electrical measurements and in situ observations of domain wall dynamics using EH at the CEMES. A detailed protocol focusing on the crucial steps and challenges ahead for such a delicate experiment is presented, together with suggestions for future work to continue the developments

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Shipkova, I. G., V. S. Chumak, M. V. Reshetnyak, A. Y. Devizenko und Y. P. Pershyn. „Estimation of interlayer composition in WC/Si multilayer X-ray mirrors (MXMs) at nanometer scale“. Thesis, НТУ "ХПІ", 2016. http://repository.kpi.kharkov.ua/handle/KhPI-Press/28180.

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42

Martin, Yannick. „Development of electron microscopy diffraction techniques for the study of two and three dimensional materials“. Thesis, Grenoble, 2014. http://www.theses.fr/2014GRENY066/document.

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De par leurs propriétés physico-chimiques spécifiques, les nanomatériaux attirent de plus en plus la communauté scientifique. Dans ce contexte, il est important d'améliorer les techniques de caractérisation à l'échelle nanométrique. Ce travail de thèse est basé sur le développement de techniques de diffraction électronique pour l'étude de matériaux bi-dimensionnels et tri-dimensionnels.La diffraction électronique en faisceau convergent contient de nombreuses informations sur la structure l'échantillon. Ces informations, portées par les lignes de HOLZ, permettent de déterminer l'épaisseur de l'échantillon, le facteur de structure, la direction d'observation, la tension d'accélération des électrons, ainsi que la longueur de caméra. Des ambiguïtés existent dans la détermination de l'état de contraintes car un cliché expérimental est une projection bi-dimensionnelle d'une information tri-dimensionnelle. Il a été possible au cours de cette thèse de réduire ces ambiguïtés et de déterminer ainsi les composantes diagonales du tenseur de déformation à partir d'une seule direction d'observation. En étudiant l'élargissement des lignes de HOLZ, dû à une déformation non uniforme dans le sens de propagation des électrons, il a été possible de remonter au champ de déplacement suivant l'axe du faisceau d'électrons.La seconde partie de cette thèse s'intéresse aux matériaux bi-dimensionnels comme le Graphène, le Nitrure de Bore (BN) et le disulfure de Molybdène (MoS2). L'interprétation du contraste d'une image de microscopie électronique en transmission haute résolution est discutée, notamment sur l'importance de l'orientation de l'échantillon et des aberrations. Une méthode de mesure de l'orientation d'un échantillon bi-dimensionnel basée sur la projection des tâches de diffraction est présentée. Enfin, trois techniques de mesure d'épaisseur sont comparées en les appliquant à quelques couches atomique de MoS2 et BN
The small dimensions of nanomaterials give them remarkable properties attracting the scientific community. In order to understand and control these properties, it is essential to characterize them at the nanometer scale. This thesis work is based on the development of electron microscopy diffraction techniques for the study of two and three dimensional materials.Convergent Beam Electron Diffraction patterns contain large amount of information on the sample geometry. This information, carried by HOLZ lines, allows to determine the sample thickness, the structure factor, the direction of observation, the electron acceleration voltage and the camera length. Ambiguities in strain measurement arise from the experimental two-dimensional projection of three-dimensional information. During this thesis, it has been possible to reduce these ambiguities and therefore to measure the diagonal components of the deformation gradient tensor from one direction of observation only. By studying the HOLZ lines broadening, due to a non-uniform strain along the electron beam direction, it has been possible to retrieve the displacement field along the beam direction.The second part of this thesis is focused on the study of two-dimensional materials such as Graphene, Boron Nitride (BN) or Molybdenum disulfide (MoS2). The delicate interpretation of the contrast of high-resolution transmission electron microscopy images and especially the importance of aberrations and sample tilt on this contrast is discussed. A method to quantify two-dimensional sample orientation using diffraction spots projection effect is presented. Finally, three thickness measurement techniques are compared by applying them to few-layered MoS2 et BN

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Lepot, Kevin. „Recherche et caractérisation de traces fossiles d'activité microbienne archéenne (Pilbara Drilling Project, Australie)“. Paris, Institut de physique du globe, 2007. http://www.theses.fr/2007GLOB0007.

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Les stromatolites, dépôts carbonatés aux morphologies singulières, sont parmi les plus notables Archéenne (2,5 à 4 milliards d'années). Si on sait que de tels dépôts se forment sous l'influence de tapis microbiens dans lesenvironnements modernes, l'origine biologique des stromatolites "fossiles"Archéensreste débattue. L'utilisation de techniques de microscopie et spectroscopie de haute résolution a permis d'étudier la matière organique et les minéraux associés directement au sein de la roche jusqu'à l'échelle du nanomètre. Cette étude a révélé la présence de globules de matière organique évoquant des microorganismes procaryotes dans les stromatolites de Tumbiana (2,7 milliards d'années). Ces globules sont intimement associés à des nano-cristaux d'aragonite. La haute similitude de cette association avec les nanocomposites organo-minéraux formant les stromatolites modernes défend l'origine biologique des stromatolites de Tumbiana. Cette aragonite, présumée hautement instable, est 2,3 milliards d'années plus ancienne que les autres aragonites découvertes jusqu'alors. L'étude systématique des associations organo-minérales dans ces stromatolites montre l'absence de textures caractéristiques d'une remobilisation de matière organique en association avec les globules, ce qui soutient leur interprétation en tant que microbes fossiles. Cette distribution, ainsi que la spectroscopie (NEXAFS, EDX) de la matière organique, suggèrent de plus que la préservation des globules est liée à une action commune de la sulphurisation de la matière organique et de son encapsulation par les minéraux

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Motylenko, Mykhaylo. „Beitrag zur Analyse von Disklinationsstrukturen in plastisch verformten Metallen“. Doctoral thesis, Technische Universitaet Bergakademie Freiberg Universitaetsbibliothek "Georgius Agricola", 2011. http://nbn-resolving.de/urn:nbn:de:bsz:105-qucosa-67416.

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Gegenstand der Arbeit ist die Analyse der bei hohen Verformungsgraden in Werkstoffen durch kollektive Bewegung der Versetzungen entstandenen neuen Defektkonfigurationen, die auf der mesoskopischen Skala agieren. Diese so genannte Disklinationen rufen neben starken Gitterdehnungen auch erhebliche lokale Gitterrotationen hervor. Es wurde der Nachweis der Existenz der Disklinationen in plastisch verformten Kristallen geliefert sowie die qualitative und quantitative Analyse der Disklinationskonfigurationen und der Disklinationsstärke durchgeführt. Die Untersuchungen an stark verformten Ein- und Vielkristallen wurden mittels sowohl lokalen Methoden der Transmissions- (TEM, CBED) und Rasterelektronenmikroskopie (REM, EBSD) als auch der integralen Methoden der Röntgenstrukturanalyse (XRD) durchgeführt. Die Ergebnisse haben gezeigt, dass die Entwicklung der Zellblockstruktur mit erheblichem Anstieg der Desorientierungen und Versetzungsdichten in Versetzungswänden verbunden ist und durch die Bildung der Netzwerke von Disklinationen gefördert wird.

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Dickinson, Calum. „Metal oxide porous single crystals and other nanomaterials : an HRTEM study“. Thesis, University of St Andrews, 2007. http://hdl.handle.net/10023/217.

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Three-dimensional porous single crystals (PSCs) are a recent development in the growing world of mesoporous material. The mesoporosity allows for the material to retain their nanoproperties whilst being bulk in size. The current work concentrates on chromium oxide and cobalt oxide PSCs formed in the templates SBA-15 and KIT-6. HRTEM is the main technique used in this investigation, looking at the morphology and single crystallinity of these materials. A growth mechanism for the PSC material is proposed based on HRTEM observations. XRD studies revealed that the confinement effect, caused by the mesopores, reduces the temperature for both cobalt and chromium oxide crystallisation, as well as a different intermediate route from the metal nitrates. The properties of chromium oxide PSC are also investigated magnetically and catalytically. Some metal oxides in different templates are also presented, despite no PSC forming. HRTEM work on other nanomaterials, based on collaboration, is also presented.

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Polcer, Simon. „Detekce a rozměření elektronového svazku v obrazech z TEM“. Master's thesis, Vysoké učení technické v Brně. Fakulta elektrotechniky a komunikačních technologií, 2020. http://www.nusl.cz/ntk/nusl-413022.

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This diploma thesis deals with automatic detection and measurement of the electron beam in the images from a transmission electron microscope (TEM). The introduction provides a description of the construction and the main parts of the electron microscope. In the theoretical part, there are summarized modes of illumination from the fluorescent screen. Machine learning, specifically convolution neural network U-Net is used for automatic detection of the electron beam in the image. The measurement of the beam is based on ellipse approximation, which defines the size and dimension of the beam. Neural network learning requires an extensive database of images. For this purpose, the own augmentation approach is proposed, which applies a specific combination of geometric transformations for each mode of illumination. In the conclusion of this thesis, the results are evaluated and summarized. This proposed algorithm achieves 0.815 of the DICE coefficient, which describes an overlap between two sets. The thesis was designed in Python programming language.

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Karathanou, Argyro. „Image processing for on-line analysis of electron microscope images : automatic Recognition of Reconstituted Membranes“. Phd thesis, Université de Haute Alsace - Mulhouse, 2009. http://tel.archives-ouvertes.fr/tel-00559800.

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The image analysis techniques presented in the présent thesis have been developed as part of a European projeet dedicated to the development of an automatic membrane protein crystallization pipeline. A large number of samples is simultaneously produced and assessed by transmission electron microscope (TEM) screening. Automating this fast step implicates an on-fine analysis of acquired images to assure the microscope control by selecting the regions to be observed at high magnification and identify the components for specimen characterization.The observation of the sample at medium magnification provides the information that is essential to characterize the success of the 2D crystallization. The resulting objects, and especially the artificial membranes, are identifiable at this scale. These latter present only a few characteristic signatures, appearing in an extremely noisy context with gray-level fluctuations. Moreover they are practically transparent to electrons yielding low contrast. This thesis presents an ensemble of image processing techniques to analyze medium magnification images (5-15 nm/pixel). The original contribution of this work lies in: i) a statistical evaluation of contours by measuring the correlation between gray-levels of neighbouring pixels to the contour and a gradient signal for over-segmentation reduction, ii) the recognition of foreground entities of the image and iii) an initial study for their classification. This chain has been already tested on-line on a prototype and is currently evaluated.

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Song, Haiwen. „Diesel soot oxidation under controlled conditions“. Thesis, Brunel University, 2003. http://bura.brunel.ac.uk/handle/2438/4814.

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In order to improve understanding of diesel soot oxidation, an experimental rig was designed and set up, in which the soot oxidation conditions, such as temperature, oxygen partial pressure, and CO2 partial pressure, could be varied independently of each other. The oxidizing gas flow in the oxidizer was under laminar condition. This test rig comprised a naturally-aspirated single cylinder engine which acted as the soot generator, and a separate premixed oxidation burner system in which soot extracted from the engine was oxidized under controlled conditions. Diesel soot was extracted from the engine exhaust pipe and from the engine pre-combustion chamber, and the soot-laden gas was then conveyed to the burner where it was oxidized. The burner was positioned vertically and it had a flat flame whose thickness was only a few millimetres. The hot gases from the flame flew upwards through a quartz transparent tube which acted as the soot oxidation duct. The soot-laden gas from the engine was premixed with the feedgas (itself a premixed mixture of methane, air, oxygen, and nitrogen) to the burner. The soot particles passed vertically through the flame front and continued burning in the post-flame gas flowing through the quartz tube oxidation duct. The oxygen concentration and temperature of the post-flame soot oxidation gas were controllable by adjusting the flowrate and composition of the burner feedgas. Diesel soot particles were sampled at different heights along the centreline of the quartz tube above the burner. Profiles of oxygen concentration, temperature, and soot particle velocity in the oxidation zone were thus measured. Morphology and size distributions of the sampled diesel soot particles were analyzed by means of Transmission Electron Microscopy (TEM) and a computer software called ImagePro Plus. Subsequently, the specific surface oxidation rates of the soot particles were worked out based on soot particle size distributions. The TEM micrographs obtained in this study showed that the diesel soot agglomerates existed in forms of clusters and chains, each containing between a small number and thousands of individual, mostly spherical tiny particles. Of order 97% of the individual spherical particles (spherules) had a size range from 10 to 80 nm. Occasionally, individual spherules of about 150 nm in diameter could be observed. The diesel soot particles sampled from the pre-chamber of the engine had different size distributions from those sampled from the exhaust of the engine, indicating that the soot underwent an oxidation process in the combustion chamber. Soot oxidation experiments were performed in the burner post-flame gas under oxygen partial pressures ranging from 0.010 to 0.050 atm and temperatures from 1520 to 1820 K. The test results showed that the oxidation rates of the diesel soot extracted from the diesel engine were generally lower than those predicted by the well-known Nagle and Strickland-Constable formula; however, the measured oxidation rates were higher than the predictions made with another well-known formula - the Lee formula. The soot extracted from the engine pre-chamber appeared not to oxidize as fast as the soot extracted from the exhaust of the engine. CO2 gas injection to the post-flame oxidation gas at constant oxygen partial pressure and oxidation temperature seemed to have accelerated the diesel soot oxidation rate. Based on the experimental results of this study and the results of other researchers, modifications to the Nagle and Strickland-Constable formula and to the Lee formula were accomplished. Also, an empirical expression, as an alternative to semi-empirical formulae, was worked out and presented in the thesis.

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Mohseni, Hamidreza. „Tribological Improvements of Carbon-Carbon Composites by Infiltration of Atomic Layer Deposited Lubricious Nanostructured Ceramic Oxides“. Thesis, University of North Texas, 2011. https://digital.library.unt.edu/ark:/67531/metadc84254/.

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A number of investigators have reported enhancement in oxidation and wear resistant of carbon-carbon composites (CCC) in the presence of protective coating layers. However, application of a surface and subsurface coating system that can preserve its oxidation and wear resistance along with maintaining lubricity at high temperature remains unsolved. To this end, thermodynamically stable protective oxides (ZnO/Al2O3/ZrO2) have been deposited by atomic layer deposition (ALD) to infiltrate porous CCC and graphite foams in order to improve the thermal stability and wear resistance in low and high speed sliding contacts. Characterization of microstructural evolution was achieved by using energy dispersive x-ray spectroscopy (EDS) mapping in scanning electron microscope (SEM) coupled with focused ion beam (FIB), x-ray tomography, high resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy (STEM) and X-ray diffraction (XRD). Evaluation of the tribological properties of CCC coated with abovementioned ALD thin films were performed by employing low speed pure sliding tribometer and a high speed/frequency reciprocating rig to simulate the fretting wear behavior at ambient temperature and elevated temperatures of 400°C.It was determined with x-ray tomography imaging and EDS mapping that ALD ZnO/Al2O3/ZrO2 nanolaminates and baseline ZrO2 coatings exhibited excellent conformality and pore-filling capabilities down to ~100 μm and 1.5 mm in the porous CCC and graphite foam, respectively, which were dependent on the exposure time of the ALD precursors. XRD and HRTEM determined the crystalline phases of {0002} textured ZnO (wurtzite), amorphous Al2O3, and {101}-tetragonal ZrO2. Significant improvements up to ~65% in the sliding and fretting wear factors were determined for the nanolaminates in comparison to the uncoated CCC. A tribochemical sliding-induced mechanically mixed layer (MML) was found to be responsible for these improvements. HRTEM confirmed the presence of a high density of ZnO shear-induced basal stacking faults inside the wear tracks responsible for intrafilm shear velocity accommodation that mitigated friction and wear.

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Mühlbacher, Marlene. „High-resolution characterization of TiN diffusion barrier layers“. Licentiate thesis, Linköpings universitet, Tunnfilmsfysik, 2015. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-120394.

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Titanium nitride (TiN) films are widely applied as diffusion barrier layers in microelectronic devices. The continued miniaturization of such devices not only poses new challenges to material systems design, but also puts high demands on characterization techniques. To gain understanding of diffusion processes that can eventually lead to failure of the barrier layer and thus of the whole device, it is essential to develop routines to chemically and structurally investigate these layers down to the atomic scale. In the present study, model TiN diffusion barriers with a Cu overlayer acting as the diffusion source were grown by reactive magnetron sputtering on MgO(001) and thermally oxidized Si(001) substrates. Cross-sectional transmission electron microscopy (XTEM) of the pristine samples revealed epitaxial, single-crystalline growth of TiN on MgO(001), while the polycrystalline TiN grown on Si(001) exhibited a [001]-oriented columnar microstructure. Various annealing treatments were carried out to induce diffusion of Cu into the TiN layer. Subsequently, XTEM images were recorded with a high-angle annular dark field detector, which provides strong elemental contrast, to illuminate the correlation between the structure and the barrier efficiency of the single- and polycrystalline TiN layers. Particular regions of interest were investigated more closely by energy dispersive X-ray (EDX) mapping. These investigations are completed by atom probe tomography (APT) studies, which provide a three-dimensional insight into the elemental distribution at the near-interface region with atomic chemical resolution and high sensitivity. In case of the single-crystalline barrier, a uniform Cu-enriched diffusion layer of 12 nm could be detected at the interface after an annealing treatment at 1000 °C for 12 h. This excellent barrier performance can be attributed to the lack of fast diffusion paths such as grain boundaries. Moreover, density-functional theory calculations predict a stoichiometry-dependent atomic diffusion mechanism of Cu in bulk TiN, with Cu diffusing on the N-sublattice for the experimental N/Ti ratio. In comparison, the polycrystalline TiN layers exhibited grain boundaries reaching from the Cu-TiN interface to the substrate, thus providing direct diffusion paths for Cu. However, the microstructure of these columnar layers was still dense without open porosity or voids, so that the onset of grain boundary diffusion could only be found after annealing at 900 °C for 1 h. The present study shows how to combine two high resolution state-of-the-art methods, TEM and APT, to characterize model TiN diffusion barriers. It is shown how to correlate the microstructure with the performance of the barrier layer by two-dimensional EDX mapping and three-dimensional APT. Highly effective Cu-diffusion barrier function is thus demonstrated for single-crystal TiN(001) (up to 1000 °C) and dense polycrystalline TiN (900 °C).

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Dissertationen zum Thema „Transmission electron microscopy (TEM)“

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