No description available.

No description available.

Die vorliegende Arbeit beschreibt die Implementierung ionenstrahlanalytischer Methoden zur Charakterisierung der Probenzusammensetzung in einem Helium-Ionen-Mikroskop mit einem auf unter einen Nanometer fokussierten Ionenstrahl. Zur Bildgebung wird dieser im Mikroskop über Probenoberflächen gerastert und die lokale Ausbeute an Sekundärelektronen gemessen. Obwohl sich damit ein hoher topografischer Kontrast erzeugen lässt, lassen sich weder aus der Ausbeute noch aus der Energieverteilung der Sekundärelektronen verlässliche Aussagen zur chemischen Zusammensetzung der Probe treffen. Daher wurden in dieser Arbeit verschiedene ionenstrahlinduzierte Sekundärteilchen hinsichtlich ihrer Eignung für die Elementanalytik im Helium-Ionen-Mikroskop verglichen. Zur Evaluation standen der Informationsgehalt der Teilchen, deren Analysierbarkeit sowie deren verwertbare Ausbeute. Die Spektrometrie rückgestreuter Teilchen sowie die Sekundärionen-Massenspektrometrie wurden dabei als die geeignetsten Methoden identifiziert und im Detail untersucht. Gegenstand der Untersuchung waren physikalische Limitierungen und Nachweisgrenzen der Methoden sowie deren Eignung zum Einbau in ein Helium-Ionen-Mikroskop. Dazu wurden verschiedene Konzepte von Spektrometern evaluiert, erprobt und hinsichtlich ihrer Effizienz, Energieauflösung und Umsetzbarkeit im Mikroskop bewertet. Die Flugzeitspektrometrie durch Pulsen des primären Ionenstrahls konnte als die geeignetste Technik identifiziert werden und wurde erfolgreich in einem Helium-Ionen-Mikroskop implementiert. Der Messaufbau, die Signal- und Datenverarbeitung sowie vergleichende Simulationen werden detailliert beschrieben. Das Spektrometer wurde weiterhin ausführlich hinsichtlich Zeit-, Energie- und Massenauflösung charakterisiert. Es werden ortsaufgelöste Rückstreuspektren vorgestellt und damit erstmalig die Möglichkeit zur Ionenstrahlanalytik im Helium-Ionen-Mikroskop auf einer Größenskala von ≤ 60 nm aufgezeigt. Das Pulsen des primären Ionenstrahls erlaubt es zudem, die Technik der Sekundärionen-Massenspektrometrie anzuwenden. Diese Methode bietet Informationen zur molekularen Probenzusammensetzung und erreicht für einige Elemente niedrigere Nachweisgrenzen als die Rückstreuspektrometrie. Damit konnten erstmalig im Helium-Ionen-Mikroskop gemessene Sekundärionen-Massenspektren sowie die ortsaufgelöste Elementanalyse durch spektrometrierte Sekundärionen demonstriert werden. Die Ergebnisse dieser Arbeit sind in der Fachzeitschrift Ultramicroscopy Band 162 (2016) S. 91–97 veröffentlicht. Ab Oktober 2016 werden diese auch in Form eines Buchkapitels in dem Buch „Helium Ion Microscopy“, Springer Verlag Heidelberg zur Verfügung stehen. / The present work describes the implementation of ion beam analysis methods in a helium-ion-microscope for the determination of sample compositions with a focused ion beam of < 1 nm size. Imaging in the microscope is realized by scanning the focused ion beam over the sample surface while measuring the local secondary electron yield. Although this procedure leads to a high topographical contrast, neither the yield nor the energy distribution of the secondary electrons deliver reliable information on the chemical composition of the sample. For this purpose, in this work different ion beam induced secondary particles were compared with respect to their suitability for the analysis of the chemical composition in the helium-ion-microscope. In particular the information content of the particles, their analysability and their yield were evaluated. As a result, the spectrometry of backscattered particles and the mass spectrometry of sputtered secondary ions were identified as the most promising methods and regarded in detail. The investigation focused on physical limitations and detection limits of the methods as well as their implementability into a helium-ion-microscope. Therefor various concepts of spectrometers were evaluated, tested and validated in terms of their efficiency, energy resolution and practicability in the microscope. Time-of-flight spectrometry by pulsing the primary ion beam could be identified as the most suitable technique and has been successfully implemented in a helium-ion-microscope. The measurement setup, signal processing and data handling as well as comparative simulations are described in detail. Further the spectrometer was characterized explicitly in terms of time, energy and mass resolution. Spatially resolved backscattering spectra will be shown demonstrating the feasibility of performing ion beam analysis in a helium-ion-microscope for the first time on a size scale of ≤ 60 nm. By pulsing the primary ion beam the technique of secondary ion mass spectrometry becomes automatically accessible. This method provides information on the molecular composition of samples and can reach higher detection limits than those from backscattering spectrometry. For the first time, in a helium-ion-microscope measured secondary ion mass spectra and spatially resolved elemental analysis by spectrometry of secondary ions, could be demonstrated. The results of this work are published 2016 in the scientific journal Ultramicroscopy, volume 162 on pages 91 to 971. In October 2016 there will be another publication as a book chapter in „Helium Ion Microscopy“ (publisher: Springer Verlag Heidelberg).

O grafeno é um material que apresenta propriedades físicas e químicas superiores aos materiais tradicionalmente utilizados na fabricação de diferentes dispositivos. Porém, para substituir tais materiais, é imprescindível o conhecimento e controle de processos de adsorção e incorporação de diferentes compostos na superfície do grafeno, crescido ou transferido, sobre diferentes substratos. A investigação da síntese e caracterização de filmes de grafeno com a finalidade de controlar as propriedades físico-químicas e elétricas é um esforço da comunidade científica atualmente. Nesse trabalho, tivemos o objetivo de investigar o processamento térmico do grafeno em vapor de água e em óxido nítrico e sua síntese pela técnica de MBE, caracterizando as estruturas resultantes através de técnicas de análise por feixes de íons, espectroscopia de fotoelétrons e espectroscopia Raman. No caso do processamento em vapor de água, as amostras foram submetidas a tratamentos térmicos em ampla faixa de temperatura (200-1000°C), sendo possível distinguir três diferentes regimes de interação do grafeno com a água. A baixas temperaturas de processamento (200-400°C), nenhuma modificação considerável é observada. Na faixa entre 400-500°C, a estrutura plana do grafeno é corrugada para acomodar os novos grupamentos funcionais formados. A partir de 600°C, os domínios cristalinos diminuem e observa-se alto nível de dopagem oxidativa. Já no processamento em NO, evidenciou- se a introdução de N na rede cristalina e etching do grafeno em altas temperaturas. Quanto ao crescimento de grafeno sobre substratos de Si3N4 e AlN(0001) por MBE, este trabalho mostrou a viabilidade de se obter filmes de nanografeno com uma taxa de crescimento de 1 monocamada por minuto, onde a qualidade cristalina do filme formado e a espessura dependem do tempo de crescimento. / Graphene is a material which presents physical and chemical properties superior than the materials traditionally used in different devices. In order to use graphene rather than those materials, it is necessary to understand and control the adsorption process and incorporation of different compounds on graphene, grown or transferred, on different substrates. The scientific community has made efforts to control the physicochemical and electrical properties of graphene films. The objective of thesis is to investigate the physicochemical modifications of graphene induced by annealing in water vapor and nitric oxide and to grow graphene by MBE. Resulting structures were characterized by ion beam analysis, x-ray spectroscopy and Raman spectroscopy. Concerning samples treated in water vapor, annealings were performed at temperatures ranging from 200 to 1000ºC. Results evidence three different regimes with respect to annealing temperature. In the low temperature range (200–400°C), no prominent modification of graphene itself is observed. At higher temperatures (400–500°C), to accommodate newly formed oxygen functionalities, the flat and continuous sp2 bonding network of graphene is disrupted, giving rise to a puckered layer. For 600°C and above, shrinking of graphene domains and a higher doping level take place. Regarding graphene processing in NO, results show N incorporation in graphene crystal network and etching of graphene at higher temperatures. Concerning graphene synthesis on Si3N4 and AlN(0001) by MBE, this work demonstrates the feasibility of growing nanographene with a growth rate of one monolayer per minute. In addition, the crystal quality of the films and their thickness depends on growing time.

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Předložená diplomová práce se zabývá implementací metody rentgenové emisne indukované částicemi do experimentálního uspořádání za účelem doplnění rodiny metod založených na iontových technikách, tj. Rutherfordovy zpětné rozptylové spektrometrie, spektrometrie elastického zpětného rozptylu a analýzy detekce doby letu/energie elastického odrazu. Výhoda více-metodického přístupu je demonstrována na vrstvách ze slitin přechodných kovů obsahujících lehké prvky, kde samo-konzistentní analýza poskytuje výrazně zlepšené a přesné informace o stechiometrii, hloubkovém rozložení a tloušťce slitiny. Hmotnostní spektrometrie sekundárních iontů je použita pro porovnání a doplnění získaných výsledků.

This thesis involves the study of dust particles trapped in silica aerogel for fusion dust diagnostics purpose. The low velocity impact experiments are done by implanting predefined dust particles into silica aerogel by using a springpiston air gun. The impact experiment results show that the hypervelocity impact model may not suitable for describing the fusion characteristic dust particles. The samples made by impact experiment are analyzed by ion microbeam analysis methods: Rutherford backscattering spectrometry (RBS) and Particle-induced X-ray Emission spectrometry (PIXE). The elements of dust particles are well identified by the X-ray spectra. The X-ray maps clearly show the dust shape. RBS and NRA spectra of an individual particle or a specific region show the depth information of the trapped particles, which is useful for determining the dust velocities. For the interpretation of ion beam analysis result, simulation of dust particles for RBS and NRA are done. The accessible depth for ion beam analysis in silica aerogel can be several hundred micrometers, which is adequate for dust diagnostics.

The goal for this project was to analyze and understand the noise of the ion beam analysis technique, Elastic Recoil Detection Analysis (ERDA). This was done by examining two models: Classical models and a prediction model. The prediction model is a parameterized noise distribution model. After examining the models, we concluded that both models had advantages and disadvantages for ERDA analysis. This information could be applicable to our understanding of how ERDA could improve for our analysis of wall materials, which could lead to the overall development of fusion reactors. / Målet för detta projekt var att analysera och förstå brus från jonstråleanalystekniken, Elastic Recoil Detection Analysis (ERDA). Detta gjordes genom att granska två modeller: Klassiska brusreduceringsmodeller och en förutsägelsemodell. Förutsägelsemodellen är en parametrerad brusfördelningsmodell. Efter granskningen av modellerna drog vi slutsatsen att båda modellerna hade fördelar och nackdelar för ERDA-analys. Denna information kan vara tillämplig på vår förståelse av hur ERDA kan förbättras för vår analys av väggmaterial, vilket kan leda till den övergripande utvecklingen av fusionsreaktorer. / Kandidatexjobb i elektroteknik 2021, KTH, Stockholm

Accurate knowledge of stopping powers is essential for these for quantitative analysis and surface characterization of thin films using ion beam analysis (IBA). These values are also of interest in radiobiology and radiotherapy, and in ion- implantation technology where shrinking feature sizes puts high demands on the accuracy of range calculations. A theory that predicts stopping powers and ranges for all projectile-target combinations is needed. The most important database used to report the stopping powers is the SRIM/TRIM program developed by Ziegler and coworkers. However, other researchers report that at times, these values differ significantly from experimental values. In this study the stopping powers of Si, P and S ions have been measured in Ni, Cu, Ge and GaAs absorbers in the energy range ~ 2-10 MeV. For elemental films of Ni, Cu and Ge, the stopping of heavy ions was measured using a novel ERD (Elastic Recoil Detection) based technique. In which an elastically recoiled lighter atom is used to indirectly measure the energy of the incoming heavy ion using a surface barrier detector. In this way it was possible to reduce the damage and to improve the FWHM of the detector. The results were compared to SRIM-2000 predictions and other experimental measurements. A new technique derived from Molecular Beam Epitaxy (MBE) was developed to prepare stoichiometric GaAs films on thin carbon films for use in transmission ion beam experiments. The GaAs films were characterized using X-ray Photoelectron Spectroscopy (XPS) and Particle Induced X-ray Emission (PIXE). These films were used to investigate the stopping powers of energetic heavy ions in GaAs and to provide data for the calculation of Bethe-Bloch parameters in the framework of the Modified Bethe-Bloch theory. As a result of this study, stopping power data are available for the first time for Si and P ions in the energy range 2-10 MeV stopping in GaAs absorbers.

La coloration d'un béton, matériau faiblement chromatique, est obtenue soit par introduction de pigments dans son volume, soit par application d'un revêtement coloré sur sa surface. Ces travaux de thèse s'intéressent à une voie de coloration alternative innovante, qui consiste à introduire les pigments dans l'agent de décoffrage afin qu'ils soient transférés durablement vers la surface du béton frais au moment où celui-ci est coulé dans le coffrage. Cette méthode s'apparente beaucoup à la technique de peinture à fresque, qui a largement fait ses preuves en terme de durabilité. Dans un premier temps, l'étude de fresques sur chaux et sur ciment anciennes, ainsi que de reconstitutions, a permis d'identifier les principaux paramètres qui régissent le dépôt des pigments et leur adhésion durable au support : compatibilité du liant avec l'eau capillaire de l'enduit, granulométrie des pigments,cisaillement du pinceau à la surface de la fresque. Dans un second temps, la transposition de ces paramètres au cas du béton a conduit à l'identification de solutions satisfaisantes en terme de transfert et de durabilité de la couleur, mais aussi d'état de surface du béton (rugosité, porosité, homogénéité) : remplacement de l'huile de décoffrage par des tensioactifs non ioniques de faible viscosité et emploi de pigments correctement dispersés dans l'agent décoffrant. Finalement, l'étude des interfaces béton- agent décoffrant - coffrage a montré que le transfert durable des pigments repose sur un double mécanisme de démouillage de l'agent décoffrant par le béton en écoulement et de mélange des deux phases au niveau du front de la coulée, qui aboutit à la formation d'une inter phase pigments - béton de plusieurs dizaines de micromètres d'épaisseur. La profondeur de pénétration des pigments sous la surface a pu être quantifiée grâce à la combinaison d'observations en microscopie électronique à balayage et d'analyses en spectroscopie de rétrodiffusion Rutherford. La durabilité de la coloration a été évaluée par des mesures colorimétriques dans l'espace CIELab. / Concrete is an achromatic material that can be coloured through two main techniques: introduction of pigments in the bulk of the material, or application of a coloured layered on the hardened surface. This work focuses on an innovating alternative technique: the pigments are mixed with the demoulding agent, so that they can be transferred to the fresh concrete while it is poured into the mould. This method is ver y similar to the long-lasting fresco painting technique. The first par t of this work was dedicated to the study of ancient frescoes on lime or cement, in order to identify the main parameters responsible for the transfer and durable adhesion of the pigments to the plaster : compatibility between the binder and the capillar y water of the plaster, grain size of the pigments and shear stress between the brush and the plaster surface. In the second par t, these parameters were transposed to the case of concrete, which lead to satisfactor y solutions in terms of colour transfer and durability as well as surface proper ties of the concrete: the demoulding oil was replaced by low-viscosity non-ionic surfactants and the pigments were chosen to be finely dispersed in the demoulding solution. The last part consisted of a study of the mould - demoulding agent - concrete system and showed that the pigments are transferred to the concrete through the dewetting of the demoulding agent by the flowing concrete and the mixing of the two phases. This mechanism leads to the formation of a pigments - concrete interphase with a thickness of several tens micrometers. The depth of the pigments was quantified through a combination of scanning electron microscopy and Rutherford back-scattering spectroscopy. The durability of the colour was evaluated by colour measurements in the CIELab colorimetric space.