O objetivo desse trabalho foi estudar a viabilidade de adaptação do Implantador Iônico da Universidade de São Paulo para a técnica de Accelerator Mass Spectrometry (AMS), tendo em vista as baixas energias utilizadas por este acelerador de partículas. A técnica de AMS, amplamente utilizada para a análise de Carbono-14 no estudo de datação de fósseis, requer que algum componente do acelerador garanta a quebra de moléculas de massa 14, contaminantes no processo de medição dos átomos de carbono com massa 14. Com a utilização de energias da ordem de dezenas de keV no acelerador, o estudo do processo de quebra de moléculas para estas energias foi realizado através do projeto, construção e caracterização de um stripper gasoso. Para caracterizar o stripper implementado foram realizadas medidas de seção de choque para troca de carga do feixe e quebra molecular em função da pressão de gás injetado no stripper. Também investigou-se a influência do átomo utilizado como gás, através de três diferentes gases injetados no stripper: Hélio, Argônio e Xenônio. Alguns feixes posivos foram produzidos no Implantador para o estudo destas seções de choques: Ar+, Ar(2+), CO+, CO2(+) e O2(+). O projeto do stripper foi idealizado para minimizar a variação de pressão no interior do implantador, visando preservar as condições da fonte de íons. Curvas de perfil de pressão de gás dentro do tubo do stripper foram calculadas segundo as teorias da Tecnologia do Vácuo que permitiram tanto a estimativa desta variação quanto a quantidade de gás no interior do stripper. Também foram realizados estudos do perfil de pressão em stripper com outras geometrias (cônicas abertas e fechadas), buscando estimar a otimização da espessura do stripper em função da injeção de gás em sua base. Baseando-se nos resultados, foram apontadas mudanças necessárias no atual estágio de adaptação desse acelerador de partículas para que se torne possível a concepção de um sistema AMS em sua linha de pesquisa. / The present work aimed on studying the feasibility of adapting the Ion Implanter of University of Sao Paulo to the Accelerator Mass Spectrometry technique, taking into account the low energies employed by this type of particle accelerator. The AMS technique, largely applied to the Carbon-14 analysis for fossil dating, requires the breaking of molecules with mass 14 by some component in the accelerator, since these lead to interference on the Carbon-14 counting process. By employing energies on the level of keV in the accelerator, the study of the breaking process of the molecules for this energy was accomplished by means desiring, building and characterization of a gaseous stripper. In order to characterize the installed stripper, measurements were taken of the charge state exchange and molecular break up process as a function of the pressure of the gas injection into the stripper. The influence of the atom employed as gas was also investigated. The experiments were realized with the following different gases: Helium, Argon and Xenon. Some positive beams were produced on the implanter: Ar+, \\Ar(2+), CO+, CO2(+) and O2(+). The designed stripper was idealized to minimize the pressure variation on the inside of the implanter in order to preserve the conditions of the ion source. Pressure profiles of the gas inside the stripper were calculated according to the Vacuum Technology theory, which allowed estimating the quantity of gas inside the stripper. Studies on the pressure profile for different stripper geometries (open and closed conic forms) were also carried out to estimate the optimization of the stripper thickness as a function of the gas injection on its base. Based on the results, specifications for further work and changes on the current system were listed to make it possible to implement the AMS system.

Elektronentomographie erlaubt die dreidimensionale (3D) Charakterisierung von Kristalldefekten auf der Nanometerskala. Die Anwendung in der Forschung an epitaktischen Halbleiterheterostrukturen ist bisher nicht durchgesetzt worden, obwohl kleiner werdende Bauteile mit zunehmend dreidimensionaler Struktur entsprechende Untersuchungen verlangen, um die Beziehung von Struktur und physikalischen Eigenschaften in entsprechenden Materialsystemen zu verstehen. Die vorliegende Arbeit demonstriert die konsequente Anwendung der Elektronentomographie auf eine III-Sb basierte Laser- und eine 3D (In,Ga)N/GaN Nanosäulenheterostruktur. Die unerlässliche Zielpräparation von Proben mittels FIB-SEM-Zweistrahlmikroskops wird herausgestellt. Die kontrollierte Orientierung der Probe während der Präparation und die sorfältige Auswahl eines Abbildungsverfahrens im STEM werden detailliert beschrieben. Die umfassende räumliche Mikrostrukturanalyse einer antimonidbasierten Schichtstruktur folgt der Dimensionalität von Kristalldefekten. Die Facettierung und Lage einer Pore (3D Defekt), deren Auftreten in der MBE gewachsenen GaSb-Schicht untypisch ist, werden bestimmt. Das Zusammenspiel von anfänglich abgeschiedenen AlSb-Inseln auf dem Si-Substrat, der Ausbildung eines Fehlversetzungsnetzwerkes an der Grenzfläche der Heterostruktur (2D Defekt) und dem Auftreten von Durchstoßversetzungen wird mit Hilfe der Kombination tomographischer und komplementärer TEM-/STEM-Ergebnisse untersucht. Die räumliche Anordnung von Versetzungen (1D Defekte), die das ganze Schichtsystem durchziehen, wird mit Elektronentomographie offenbart. Die Wechselwirkung dieser Versetzungen mit Antiphasengrenzen und anderen Liniendefekten sind ein einzigartiges Ergebnis der Elektronentomographie. Abschließend sind Unterschiede im Indiumgehalt und in der Schichtdicke von (In,Ga)N-Einschlüssen auf verschiedenen Facetten schief aufgewachsener GaN-Nanosäulen einmalig per Elektronentomographie herausgearbeitet worden. / Electron tomography exhibits a very poor spread in the research field of epitaxial semiconductor heterostructures in spite of the ongoing miniaturization and increasing three-dimensional (3D) character of nano-structured devices. This necessitates a tomographic approach at the nanometre scale in order to characterize and understand the relation between structure and physical properties of respective material systems. The present work demonstrates the rigorous application of electron tomography to an III-Sb based laser and to an (In,Ga)N/GaN nanocolumn heterostructure. A specific target preparation using a versatile FIB-SEM dual-beam microscope is emphasized as indispensable. The purposeful orientation of the specimen during preparation and the careful selection of an imaging mode in the scanning-/transmission electron microscope (S/TEM) are regarded in great detail. The comprehensive spatial microstructure characterization of the antimonide based heterostructure follows the dimensionality of crystal defects. The facetting and position of a pore (3D defect) which is unexpected in the MBE grown GaSb layer, is determined. The interplay of the initially grown AlSb islands on Si, the formation of a misfit dislocation network at the heterostructure interface (2D defect) and the presence of threading dislocations is investigated by the correlation of tomographic and complementary S/TEM results. The spatial arrangement of dislocations (1D defects) penetrating the whole stack of antimonide layers is revealed by electron tomography. The interaction of these line defects with anti-phase boundaries and with other dislocations is exclusively observed in the 3D result. The insertion of (In,Ga)N into oblique GaN nanocolumns is uniquely accessed by electron tomography. The amount of incorporated indium and the (In,Ga)N layer thickness is shown to vary on the different facets of the GaN core.

<p>Materials prepared on the nanoscale often exhibit many different properties compared to the same materials in their bulk-state. Interest in nanostructured materials has increased because of these properties in fields such as microelectronics, catalysis, optics and sensors. This increased interest in nanostructured materials calls for new and more precise fabrication techniques.</p><p>This thesis describes how to use the porous anodic aluminium oxide as a template for the fabrication of a variety of nanostructured materials. Palladium and copper nanoparticles were deposited along the pore walls in anodic aluminum oxide using electroless deposition and atomic layer deposition. In both cases, it was possible to control the size of the nanoparticles by carefully monitoring the deposition parameters. The thesis also describes how Prussian blue nanoparticles and nanotubes can be fabricated using the anodic aluminium oxide as a template. The deposition of Prussian blue was performed by a sequential wet-chemical method. By using atomic layer deposition, it was also possible to deposit thin films of amorphous Nb2O5 on the pore walls. When the template was removed by etching, freestanding nanotubes were obtained. The anodic aluminium oxide membrane was also used as a mask for high energy (MeV) ion irradiation of an underlying substrate. The tracks produced were etched away with hydrogen fluoride. In this way, it was possible to transfer the highly ordered porous pattern from the mask onto other oxides such as SiO2 and TiO2.</p><p>All fabricated structures were characterized using a variety of analysis techniques: scanning electron microscopy for evaluating sample morphology; transmission electron microscopy for better resolved investigations of the morphology; X-ray diffraction to assess crystallinity; energy dispersive spectroscopy and X-ray fluorescence spectroscopy to determine the elemental composition and identify possible contaminants.</p><p>The general aim of the work described in this thesis has been to create a set of tools for use in the fabrication of a variety of nanostructured materials, whose dimensions composition can be tailored by selecting appropriate fabrication methods and parameters.</p>

Print quality demands for coated papers are steadily growing, and achieving coating uniformity is crucial for high image sharpness, colour fidelity, and print uniformity. Coating uniformity may be divided into two scales: coating thickness uniformity and coating microstructure uniformity, the latter of which includes pigment, pore and binder distributions within the coating layer. This thesis concerns the investigation of both types of coating uniformity by using an approach of quantitative microscopy.First, coating thickness uniformity was analysed by using scanning electron microscope (SEM) images of paper cross sections, and the relationships between local coating thickness variations and the variations of underlying base sheet structures were determined. Special attention was given to the effect of length scales on the coating thickness vs. base sheet structure relationships.The experimental results showed that coating thickness had a strong correlation with surface height (profile) of base sheet at a small length scale. However, at a large length scale, it was mass density of base sheet (formation) that had the strongest correlation with coating thickness. This result explains well the discrepancies found in the literature for the relationship between coating thickness variation and base sheet structure variations. The total variance of coating thickness, however, was dominated by the surface height variation in the small scale, which explained around 50% of the variation. Autocorrelation analyses were further performed for the same data set. The autocorrelation functions showed a close resemblance of the one for a random shot process with a correlation length in the order of fibre width. All these results suggest that coating thickness variations are the result of random deposition of particles with the correlation length determined by the base sheet surface textures, such as fibre width.In order to obtain fundamental understandings of the random deposition processes on a rough surface, such as in paper, a generic particle deposition model was developed, and systematic analyses were performed for the effects of particle size, coat weight (average number of particles), levelling, and system size on coating thickness variation. The results showed that coating thickness variation3grows with coat weight, but beyond a certain coat weight, it reaches a plateau value. A scaling analysis yielded a universal relationship between coating thickness variation and the above mentioned variables. The correlation length of coating thickness was found to be determined by average coat weight and the state of underlying surfaces. For a rough surface at relatively low coat weight, the correlation length was typically in the range of fibre width, as was also observed experimentally.Non-uniformities within the coating layer, such as porosity variations and binder distributions, are investigated by using a newly developed method: field emission scanning electron microscopy (FESEM) in combination with argon ion beam milling technique. The combination of these two techniques produced extremely high quality images with very few artefacts, which are particularly suited for quantitative analyses of coating structures. A new evaluation method was also developed by using marker-controlled watershed segmentation (MCWS) of the secondary electron images (SEI).The high resolution imaging revealed that binder enrichment, a long disputed subject in the area, is present in a thin layer of a 500 nm thickness both at the coating surface and at the base sheet/coating interface. It was also found that the binders almost exclusively fill up the small pores, whereas the larger pores are mainly empty or depleted of binder.

Dry etching is an important technique for pattern transferin fabrication of most opto-electronic devices, since it canprovide good control of both structure size and shape even on asub-micron scale. Unfortunately, this process step may causedamage to the material which is detrimental to deviceperformance. It is therefore an objective of this thesis todevelop and investigate low damage etching processes for InPbased devices. An ion beam system in combination with hydrocarbon (CH4) based chemistries is used for etching. At variousion energies and gas flows the etching is performed in twomodes, reactive ion beam etching (RIBE) and chemical assistedion beam etching (CAIBE). How these conditions affect both etchcharacteristics (e.g. etch rates and profiles, surfacemorphology and polymer formation) and etch induced damage (onoptical and electrical properties) is evaluated and discussed.Attention is also paid to the effects of typical post etchingtreatments such as annealing on the optical and electricalproperties. An important finding is the correlation betweenas-etched surface morphology and recovery/degradation inphotoluminescence upon annealing in PH3. Since this type of atmosphere is typical forcrystal regrowth (an important process step in III/Vprocessing) a positive result is imperative. A low ion energy N2/CH4/H2CAIBE process is developed which not onlysatisfies this criteria but also exhibits good etchcharacteristics. This process is used successfully in thefabrication of laser gratings. In addition to this, the abilityof the ion beam system to modify the surface morphology in acontrollable manner is exploited. By exposing such modifiedsurfaces to AsH3/PH3, a new way to vary size and density of InAs(P)islands formed on the InP surfaces by the As/P exchangereaction is presented. This thesis also proposes a new etch chemistry, namelytrimethylamine ((CH3)3N or TMA), which is a more efficient methyl sourcecompared to CH4because of the low energy required to break the H3C-N bond. Since methyl radicals are needed for theetching it is presumably a better etching chemistry. A similarinvestigation as for the CH4chemistry is performed, and it is found that bothin terms of etch characteristics and etch induced damage thisnew chemistry is superior. Extremely smooth morphologies, lowetch induced damage and an almost complete recovery uponannealing can be obtained with this process. Significantly,this is also so at relatively high ion energies which allowshigher etch rates. <b>Keywords:</b>InP, dry etching, ion beam etching, RIBE,CAIBE, hydrocarbon chemistry, trimethylamine, As/P exchangereaction, morpholoy, low damage, AFM, SCM, annealing

Materials prepared on the nanoscale often exhibit many different properties compared to the same materials in their bulk-state. Interest in nanostructured materials has increased because of these properties in fields such as microelectronics, catalysis, optics and sensors. This increased interest in nanostructured materials calls for new and more precise fabrication techniques. This thesis describes how to use the porous anodic aluminium oxide as a template for the fabrication of a variety of nanostructured materials. Palladium and copper nanoparticles were deposited along the pore walls in anodic aluminum oxide using electroless deposition and atomic layer deposition. In both cases, it was possible to control the size of the nanoparticles by carefully monitoring the deposition parameters. The thesis also describes how Prussian blue nanoparticles and nanotubes can be fabricated using the anodic aluminium oxide as a template. The deposition of Prussian blue was performed by a sequential wet-chemical method. By using atomic layer deposition, it was also possible to deposit thin films of amorphous Nb2O5 on the pore walls. When the template was removed by etching, freestanding nanotubes were obtained. The anodic aluminium oxide membrane was also used as a mask for high energy (MeV) ion irradiation of an underlying substrate. The tracks produced were etched away with hydrogen fluoride. In this way, it was possible to transfer the highly ordered porous pattern from the mask onto other oxides such as SiO2 and TiO2. All fabricated structures were characterized using a variety of analysis techniques: scanning electron microscopy for evaluating sample morphology; transmission electron microscopy for better resolved investigations of the morphology; X-ray diffraction to assess crystallinity; energy dispersive spectroscopy and X-ray fluorescence spectroscopy to determine the elemental composition and identify possible contaminants. The general aim of the work described in this thesis has been to create a set of tools for use in the fabrication of a variety of nanostructured materials, whose dimensions composition can be tailored by selecting appropriate fabrication methods and parameters.

The utilization of ferromagnetic shape memory alloys (FSMAs) in small scale devices has attracted considerable attention within the last decade. However, the lack of sufficient studies on their reversible shape change mechanisms, i.e, superelasticity, magnetic field-induced martensite variant reorientation and martensitic phase transformation, at the micron and submicron length scales prevent the further development and the use of FSMAs in small scale devices. Therefore, investigating the size effects in these mechanisms has both scientific and technological relevance. Superelastic behavior of Ni54Fe19Ga27 shape memory alloy single crystalline pillars was studied under compression as a function of pillar diameter. Multiple pillars with diameters ranging between 200 nm and 10 µm were cut on a single crystalline bulk sample oriented along the [110] direction in the compression axis and with fully reversible two-stage martensitic transformation. The results revealed size dependent two-stage martensitic transformation which was suppressed for pillar sizes of 1 µm and below. We also demonstrated that the reduction in pillar diameter decreases the transformation temperature due to the difficulty of martensite nucleation in small scales. Size effects in the magnetic field-induced martensite variant reorientation were investigated in the Ni50Mn28.3Ga21.7 single crystals oriented along the [100] direction of the austenite phase. Single crystalline compression pillars were fabricated on the martensite twins between the sizes of 630 nm and 20 µm. It was found that the stress-induced and magnetic field-induced martensite variant reorientation are size dependent and became more difficult with the reduction in sample size. Surprisingly, it was still possible to magnetically activate the shape change in the micropillars which indicates the fact that magnetocrystalline anisotropy energy increases with the reduction in sample dimensions. Ni45Mn36.6Co5In13.4 pillars between the 600 nm and 10 µm diameters were investigated along the [100] direction of the austenite to study the size effects in the magnetic field-induced phase transformation (MFIPT). MFIPT was obtained down to 5 µm size in these pillars with reasonable magnetic field levels similar to their bulk counterparts.

One major step needed for fusion to become a reliable energy source is the development of materials for the extreme conditions (high temperature, radioactivity and erosion) caused by hot plasmas. The main goal of the present study is to use and optimise ion beam methods (lateral resolution and sensitivity) to characterise the distribution of hydrogen isotopes that act as fuel. Materials from the test reactors JET (Joint European Torus), TEXTOR (Tokamak Experiment for Technology Oriented Research) and Tore Supra have been investigated. Deuterium, beryllium and carbon were measured by elastic recoil detection analysis (ERDA) and nuclear reaction analysis (NRA). To ensure high 3D spatial resolution a nuclear microbeam (spot size &lt;10 µm) was used with 3He and 28Si beams. The release of hydrogen caused by the primary ion beam was monitored and accounted for. Large variations in surface (top 10 µm) deuterium concentrations in carbon fibre composites (CFC) from Tore Supra and TEXTOR was found, pointing out the importance of small pits and local fibre structure in understanding fuel retention. At deeper depths into the CFC limiter tiles from Tore Supra, deuterium rich bands were observed confirming the correlation between the internal material structure and fuel storage in the bulk. Sample cross sections from thick deposits on the JET divertor showed elemental distributions that were dominantly laminar although more complex structures also were observed. Depth profiles of this kind elucidate the plasma-wall interaction and material erosion/deposition processes in the reactor vessel. The information gained in this thesis will improve the knowledge of first wall material for the next generation fusion reactors, concerning the fuel retention and the lifetime of the plasma facing materials which is important for safety as well as economical reasons.

Eine der drei Säulen der Krebsbehandlung ist die Strahlentherapie. Einer der neuesten Ansätze hierbei ist die Bestrahlung mit Ionen, zurzeit insbesondere Protonen und Kohlenstoffionen. Diese Hochpräzisionstherapie erfordert ein hohes Maß an Kontrolle, da die applizierte Dosisverteilung sehr empfindlich von Dichteveränderungen im durchstrahlten Gewebe abhängt. Das bisher einzige klinisch eingesetzte Verfahren zur in vivo Überwachung der Dosisapplikation bei Ionenbestrahlungen ist die Positronen-Emissions-Tomographie (PET). Sie ermöglicht eine Verifikation der Teilchenreichweite sowie der Lage des Bestrahlungsfeldes. Die mit der PET-Methode gemessene Aktivitätsverteilung lässt sich jedoch nicht direkt mit der geplanten Dosisverteilung vergleichen. Daher ist eine Vorherberechnung der erwarteten Aktivitätsverteilung auf der Grundlage des Bestrahlungsplanes notwendig, welche dann mit der Messung verglichen wird und eine qualitative Beurteilung der Bestrahlung ermöglicht. Die Vorherberechnung der erwarteten Aktivitätsverteilung erfordert bislang die Kenntnis einer Vielzahl von Wirkungsquerschnitten. Nur für wenige dieser Wirkungsquerschnitte liegen jedoch Messdaten im benötigten Energiebereich und mit ausreichender Genauigkeit vor. Daher verwenden viele Monte-Carlo-Simulationen intrinsische Kernmodelle oder semi-empirische Modellierungen, die häufig eine unzureichende Genauigkeit aufweisen. In Fachkreisen ist bisher noch nicht geklärt, welches die optimale Ionensorte für die Tumortherapie ist. Insbesondere Lithiumionen weisen aufgrund ihrer physikalischen und radiobiologischen Eigenschaften ein großes Potenzial auf. Auch für Bestrahlungen mit diesen Ionen ist ein PET-Monitoring der Therapie erstrebenswert. In der vorliegenden Arbeit wird zunächst die Anwendbarkeit der Reichweite-Verifikation mittels PET bei Bestrahlung mit Lithiumionen gezeigt. Des Weiteren wird ein Konzept zur Modellierung der Positronenemitter-Verteilung ohne Kenntnis der Wirkungsquerschnitte entwickelt. Diese Vorhersage beruht auf in Referenzmaterialien (Wasser, Graphit und Polyethylen) gemessenen tiefenabhängigen Positronenemitter-Yields, mit welchen durch geeignete Linearkombination die Verteilung der Positronenemitter in beliebigen Materialien bekannter Stöchiometrie vorausberechnet werden kann. Die Anwendbarkeit des Yield-Konzeptes wird gezeigt für Lithium- und Kohlenstoffbestrahlungen homogener Polymethylmethacrylat (PMMA) Targets sowie verschiedener inhomogener Targets.

Eine ortsauflösende Spannungs- und Dehnungssensortechnik soll durch die Nutzung magnetostriktiver Materialien auf der Oberfläche von Kohlenstoffeinzelfasern (C-Fasern) und Mikrofeinstrukturierung dieser Schichten erzeugt und zur elektronischen Überwachung des Belastungszustandes von sicherheits- oder servicerelevanten Faserverbundbauteilen eingesetzt werden. Eine auf lokaler Gasphasenabscheidung und Mikrostrukturierung mittels der Focused Ion Beam (FIB)-Technik beruhende Sensorfabrikationsmethode wurde gemeinsam mit dem Institut für Mikrotechnologie Hannover (imt) entwickelt. Mehrschichtig mittels CVD und PVD bedampfte und zusätzlich galvanisch beschichtete C-Fasern weisen neuartige Eigenschaften auf, die im vorgestellten Vorhaben am Lehrstuhl für Verbundwerkstoffe (LVW) charakterisiert wurden. Insbesondere die Untersuchung der verschiedenen Schichten sowie deren Interfaces nehmen eine bedeutende Rolle ein.