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The ideal properties of a structural material are light weight with extensive strength and ductility. A composite with high strength and tailorable ductility was developed consisting of nanocrystalline AA5083, boron carbide and coarser grained AA5083. The microstructure was determined through optical microscopy and transmission electron microscopy. A technique was developed to determine the nitrogen concentration of an AA5083 composite from secondary ion mass spectrometry utilizing a nitrogen ionimplanted standard. Aluminum nitride and amorphous nitrogen-rich dispersoids were found in the nanocrystalline aluminum grain boundaries. Nitrogen concentration increased as a function of cryomilling time up to 72hours. A greater nitrogen concentration resulted in an enhanced thermal stability of the nanocrystalline aluminum phase and a resultant increase in hardness. The distribution of the nitrogen-rich dispersoids may be estimated considering their size and the concentration of nitrogen in the composite. Contributions to strength and ductility from the Orowan relation can be more accurately modeled with the quantified nitrogen concentration.

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a powerful technique for the analysis of organic surfaces and interfaces for many innovative technologies. However, despite recent developments, there are still many issues and challenges hindering the robust, validated use of ToF-SIMS for quantitative measurement. These include: the lack of metrology and fundamental understanding for the use of novel cluster primary ion beams such as C60ⁿ⁺ and Ar₂₀₀₀⁺; the need for validated and robust measurement protocols for difficult samples, such as those with significant micron scale surface topography; the lack of guidance on novel data analysis methods including multivariate analysis which have the potential to simplify many time-consuming and intensive analyses in industry; and the need to establish best practice to improve the accuracy of measurements. This thesis describes research undertaken to address the above challenges. Sample topography and field effects were evaluated experimentally using model conducting and insulating fibres and compared with computer simulations to provide recommendation to diagnose and reduce the effects. Two popular multivariate methods, principal component analysis (PCA) and multivariate curve resolution (MCR), were explored using mixed organic systems consisting of a simple polymer blend and complex hair fibres treated with a multi-component formulation to evaluate different multivariate and data preprocessing methods for the optimal identification, localisation and quantification of the chemical components. Finally, cluster ion beams C60ⁿ⁺ and Ar_500-2500⁺ were evaluated on an inorganic surface and an organic delta layer reference material respectively to elucidate the fundamental metrology of cluster ion sputtering and pave the way for their use in organic depth profiling. These studies provide the essential metrological foundation to address frontier issues in surface and nanoanalysis and extend the measurement capabilities of ToF-SIMS.

Au cours de ces travaux de thèse, nous avons étudié la redistribution atomique de contaminantsmétalliques dans le silicium et au voisinage d'une interface SiO2/Si. Pour mener à bien cetteétude, trois techniques de caractérisation complémentaires ont été utilisées (TEM,APT,SIMS).Nous avons dans un premier temps étudié la diffusion ainsi que la ségrégation d'équilibre de contaminants à une interface SiO2/Si, et plus particulièrement, la diffusion du W et du Mo. Le Wprésente une cinétique de diffusion extrêmement lente. Les caractérisations réalisées par TEM et APT nous ont permis de discuter les profils de concentrations mesurés par SIMS et nous ont guidés dans le choix du modèle de diffusion proposé. L'étude de la diffusion du Mo révéle que cette espèce présente une limite de solubilité faible dans le silicium et une forte interaction avec des défauts d'irradiation, provoquant sa précipitation.Dans un second volet, nous nous sommes intéressés à l'effet d'une interface mobile, lors d'une réaction, sur la redistribution atomique des contaminants proches de cette interface. Nous avons ainsiréalisé une étude comparative des comportements du Fe et W lors de procédés d'oxydation.Le tungstène précipite dans le volume et est progressivement rejeté par l'oxydation. Le ferprécipite à l'interface SiO2/Si, provoquant un effet de masquage dont nous avons montré qu'il étaitresponsable de la formation de défauts pyramidaux d'interface, caractéristiques d'une contaminationen fer du silicium. Le procédé de germano-siliciuration de nickel, réalisé à basses températures a également été investigué. Cette réaction provoque le rejet 3D du germanium à l'interface NiSiGe/SiGe. / During this thesis work, we studied the atomic redistribution of metallic contaminantsin silicon and near a SiO2/Si interface. To conduct this study, we used three complementary characterisation techniques : transmission electron microscopy (TEM), atomic probe tomography (APT) and secondary ion mass spectrometry (SIMS).We first studied the diffusion and equilibrium segregation of various contaminants at a SiO2/Si interface, and more particularly, the diffusion of W and Mo. W exhibits a very slow diffusion kinetic.Physico-chemical characterizations performed by TEM and APT allowed discussing the concentrationprofiles obtained by SIMS leading to the diffusion model that we proposed. The study of Mo diffusionrevealed that this specy exhibits a low solubility limit in silicon and strongly interacts with irradiation-induced defects, leading to its precipitation.In a second phase, we studied the effect of a mobile interface, during a reaction, on the atomic redistribution of contaminants near this interface. We performed a comparative study of the behaviourof Fe and W during oxidation processes. W precipitates in the silicon substrate and is progressivelyrejected (snowplow) by the oxidation. Fe preferentially precipitates at the SiO2/Si interface. Theseprecipitates mask a part of the silicon substrate and thus hinder its oxidation, leading to the formation of characteristics pyramidal-shaped defects at the interface. Low temperature nickel germano-silicide formation have also been investigated. This reaction leads to the 3D snowplow of germanium atoms at the NiSiGe/SiGe interface.

Many space probes have conducted in situ explorations of asteroids, in recent decades, intent on identifying evidence of the solar system's earliest processes of formation within the asteroids' interiors. Several future asteroid missions are planned, among which include ESA's Hera mission to explore the Didymos binary asteroid pair. An ion mass analyzer is currently being designed at the Swedish Institute of Space Physics for use as part of the Hera mission. This thesis aims to optimize the instrument such that each of its parameters meets the requirement for performance. A computer simulation is used to calculate the trajectories of low-energy ions inside the instrument, where the electrostatic potential are imposed by grids and electrodes embedded inside the instrument. From the data analysis of the simulation results, the performance for each parameter can be derived. By changing the settings of the grids and electrodes (e.g., positions and voltages), the instrument parameters are to be optimized. Two tasks are set up in this project--- the first task is to optimize the focusing system of the incoming ions at the instrument's entrance, and the second task is to investigate the reflectron system so that the mass resolution of the instrument can be optimized via reducing the spread of the ions' time of flight spectra. The focusing system is found to already be optimized, but instead, a relation between its position of the grid at the instrument's entrance and the instrument's performance is derived. The method of and parameters for optimization within the reflectron are extensively tested individually during this project. Although several performances in each trial from the reflectron analysis cannot meet at least one of the requirements, enough scenarios are examined such that every parameter tested ends with a value suitable to be applied individually to optimize the ion mass analyzer. The findings from the individual tests done in this project can be applied to further optimization, particularly to optimize multiple parameters simultaneously in the near future.

Thesis (Ph. D.)--University of Washington, 2006. / Vita. Includes bibliographical references (leaves 132-140).

When and how life first emerged on the Earth is an area of intense research. Signs of the first life on Earth, including morphological fossils, are scarce and hard to interpret. An alternative approach is to study organic biomarkers, which are molecular fossils commonly considered as bona fide biosignatures. The main objective of the project is to develop an approach for analysis of single oil-bearing fluid inclusions and most importantly the detection of organic biomarkers in these inclusions. Analysis of oil-bearing fluid inclusions is advantageous since the inclusions may provide an uncontaminated sample source of Precambrian hopanes and steranes, which are key biomarkers for tracing the early evolution of life on Earth. Due to the presence of several inclusion generations, single inclusion analysis is desired in order to constrain biomarkers to specific inclusions. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) could be an excellent tool for analysis of these types of samples. The development of the approach for analysis of single oil-bearing inclusions was done in a two-step process; i) a number of crude oils were analysed with ToF-SIMS and gas chromatography mass-spectrometry (GC-MS) to facilitate interpretation of ToF-SIMS spectra of these types of samples and, ii) a procedure that combines micrographs with ion etching and ToF-SIMS analysis was developed for analysis of inclusions. The feasibility of the technique was demonstrated for oil inclusions from the Siljan impact crater in which hopanes and steranes where detected. Single oil-bearing fluid inclusions trapped in mid-Proterozoic sandstones from Northern Australia were subsequently analyzed, and steranes and hopanes were detected in these inclusions. If applied on older inclusions this approach may help answer some of the questions regarding the emergence and evolution of life on Earth, and if applied on extraterrestrial samples, also the possibility of life on other planets and moons. / Livets uppkomst och tidiga utveckling på jorden är ett hett forskningsfält. Hur och när livet och dess olika domäner (arkéer, bakterier och eukaryoter) uppstod på jorden är fortfarande oklart vilket beror på att de första tecknen på liv, vilka inkluderar morfologiska fossil, spårfossil och isotoper, är få och svåra att tolka. Ett alternativt sätt att studera det tidiga livet är att studera organiska biomarkörer som är organiska molekyler som anses unika för liv. Huvudmålet med projektet är att utveckla en metod som kan detektera organiska biomarkörer i enskilda oljebärande vätskeinneslutningar. Vätskeinneslutningar, som är små mängder vätska (picoliter) infångad in en sten, är intressanta då de är en potentiell provkälla för prekambriska (äldre än 500 miljoner år) biomarkörer, som hopaner och steraner, vilka används för att utforska livets tidiga utveckling på jorden. Analys av enskilda inneslutningar är emellertid oftast nödvändigt för att kunna tidsavgränsa biomarkörer. På grund av att de flesta inneslutningar är små (10 µm i diameter) är det inte möjligt att analysera en enskild vätskeinneslutning med standardtekniken gaskromatografi-masspektrometri (GC-MS). Time-of-flight secondary ion mass spektrometri (ToF-SIMS) med sin höga känslighet, höga massupplösning och kapacitet för 2D-representation av analysdata och djupprofilering av prover är en utmärkt teknik för analys av enskilda inneslutningar. Metoden för analys av enskilda inneslutningar utvecklades i två steg. Först analyserades ett antal råoljor med ToF-SIMS och GC-MS för att underlätta förståelsen av ToF-SIMS-spektra från dessa typer av prover. Därefter utvecklades en metod som bestod av mikroskopering för att lokalisera inneslutningen, jonetsning för att öppna inneslutningen och ToF-SIMS analys av det exponerade innehållet. Metoden testades framgångsrikt på enskilda inneslutningar i hydrotermala vener av flusspat och kalcit i ordovicisk (488-443 miljoner år sedan) kalksten. Därefter användes den utvecklade metoden för att analysera enskilda vätskeinneslutningar i 1,43 miljarder år gammal sandsten från norra Australien, i vilka hopaner och steraner detekterades. De detekterade steranerna visar att trots att havet under denna tid var syrefritt existerade det lokala syrerika miljöer där eukaryoter kunde överleva. Om den utvecklade metoden används på ännu äldre inneslutningar, vilka har daterats till 3,2 miljarder år, kan den komma att svara på några de mest fundamentala frågorna kring livets uppkomst och tidiga utveckling. Om metoden används på utomjordiska prover kan den svara på frågan om det finns liv på andra planeter eller månar. / At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 3: Manuscript. Paper 4: Submitted.

This thesis studies comparison and connection of two spectrometric methods – low energy ion scattering spektrometry (LEIS) and secondary ion mass spectrometry (SIMS). SIMS method, despite its many positive qualities, suffers of so called matrix effect, which makes quantifiaction of data very difficult. LEIS method on the other hand is immune to this effect and so it’s suitable completion of SIMS method. As a convenient sample have been chosen AlGaN samples with various concentration of gallium and aluminium. In the first part of thesis is introduced physical essence of SIMS and LEIS method, experimental details and studied samples. In second part of the thesis there’s a description of measurements and comparison of data gained by each method.

Die Erweiterung experimenteller Infrastrukturen um neuartige Sensor eröffnen die Möglichkeit, qualitativ neuartige Erkenntnisse zu gewinnen. Um diese Informationen vollständig zu erschließen ist ein Abdecken der gesamten Verarbeitungskette von der Datenauslese bis zu anwendungsbezogenen Auswertung erforderlich. Eine Erweiterung bestehender wissenschaftlicher Instrumente beinhaltet die strukturelle und zeitbezogene Integration der neuen Sensordaten in das Bestandssystem. Das hier vorgestellte Framework bietet durch seinen flexiblen Ansatz das Potenzial, unterschiedliche Sensortypen in unterschiedliche, leistungsfähige Plattformen zu integrieren. Zwei unterschiedliche Integrationsansätze zeigen die Flexibilität dieses Ansatzes, wobei einer auf die Steigerung der Sensitivität einer Anlage zur Sekundärionenmassenspektroskopie und der andere auf die Bereitstellung eines Prototypen zur Untersuchung von Rezyklaten ausgerichtet ist. Die sehr unterschiedlichen Hardwarevoraussetzungen und Anforderungen der Anwendung bildeten die Basis zur Entwicklung eines flexiblen Softwareframeworks. Um komplexe und leistungsfähige Applikationsbausteine bereitzustellen wurde eine Softwaretechnologie entwickelt, die modulare Pipelinestrukturen mit Sensor- und Ausgabeschnittstellen sowie einer Wissensbasis mit entsprechenden Konfigurations- und Verarbeitungsmodulen kombiniert.:1. Introduction 2. Hardware Architecture and Application Background 3. Software Concept 4. Experimental Results 5. Conclusion and Outlook / Novel sensors with the ability to collect qualitatively new information offer the potential to improve experimental infrastructure and methods in the field of research technology. In order to get full access to this information, the entire range from detector readout data transfer over proper data and knowledge models up to complex application functions has to be covered. The extension of existing scientific instruments comprises the integration of diverse sensor information into existing hardware, based on the expansion of pivotal event schemes and data models. Due to its flexible approach, the proposed framework has the potential to integrate additional sensor types and offers migration capabilities to high-performance computing platforms. Two different implementation setups prove the flexibility of this approach, one extending the material analyzing capabilities of a secondary ion mass spectrometry device, the other implementing a functional prototype setup for the online analysis of recyclate. Both setups can be regarded as two complementary parts of a highly topical and ground-breaking unique scientific application field. The requirements and possibilities resulting from different hardware concepts on one hand and diverse application fields on the other hand are the basis for the development of a versatile software framework. In order to support complex and efficient application functions under heterogeneous and flexible technical conditions, a software technology is proposed that offers modular processing pipeline structures with internal and external data interfaces backed by a knowledge base with respective configuration and conclusion mechanisms.:1. Introduction 2. Hardware Architecture and Application Background 3. Software Concept 4. Experimental Results 5. Conclusion and Outlook

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