The methods of analysis with a focused ion beam, commonly termed as nuclear microscopy, include quantitative physical processes like PIXE and RBS. The element concentrations in a sample can be quantitatively mapped with a sub-micron spatial resolution and a sub-ppm sensitivity. Its fully quantitative and non-destructive nature makes it particularly suitable for analysing biological samples. The applications in biomedical research are manifold. The iron overload hypothesis in Parkinson\\\'s disease is investigated by a differential analysis of human substantia nigra. The trace element content is quantified in neuromelanin, in microglia cells, and in extraneuronal environment. A comparison of six Parkinsonian cases with six control cases revealed no significant elevation in iron level bound to neuromelanin. In fact, a decrease in the Fe/S ratio of Parkinsonian neuromelanin was measured, suggesting a modification in its iron binding properties. Drosophila melanogaster, or the fruit fly, is a widely used model organism in neurobiological experiments. The electrolyte elements are quantified in various organs associated with the olfactory signalling, namely the brain, the antenna and its sensilla hairs, the mouth parts, and the compound eye. The determination of spatially resolved element concentrations is useful in preparing the organ specific Ringer\\\'s solution, an artificial lymph that is used in disruptive neurobiological experiments. The role of trace elements in the progression of atherosclerosis is examined in a pilot study. A differential quantification of the element content in an induced murine atherosclerotic lesion reveals elevated S and Ca levels in the artery wall adjacent to the lesion and an increase in iron in the lesion. The 3D quantitative distribution of elements is reconstructed by means of stacking the 2D quantitative maps of consecutive sections of an artery. The feasibility of generating a quantitative elemental rodent brain atlas by Large Area Mapping is investigated by measuring at high beam currents. A whole coronal section of the rat brain was measured in segments in 14 h. Individual quantitative maps of the segments are pieced together to reconstruct a high-definition element distribution map of the whole section with a subcellular spatial resolution. The use of immunohistochemical staining enhanced with single elements helps in determining the cell specific element content. Its concurrent use with Large Area Mapping can give cellular element distribution maps.

A instabilidade térmica do óxido de germânio (GeO2) é um obstáculo à utilização de germânio (Ge) como material semicondutor em dispositivos MOSFET. Essa instabilidade é induzida por vacâncias de oxigênio originadas de uma reação interfacial entre o óxido e o substrato. Essas vacâncias são responsáveis pela dessorção de GeO da superfície do óxido e pela deterioração das propriedades elétricas do transistor. Estudos sugerem que a incorporação de nitrogênio no GeO2 aumenta a sua estabilidade. Nesta dissertação, filmes de oxinitreto de germânio (GeOxNy) foram crescidos termicamente sobre Ge, utilizando gás óxido nítrico (NO), em um forno aquecido resistivamente. Técnicas de análise por feixe de íons, como espectrometria de retroespalhamento Rutherford e análise por reações nucleares, foram utilizadas para investigar o transporte atômico durante o crescimento dos filmes e o papel do nitrogênio na estabilização do óxido. Para a determinação da espessura, da densidade e da rugosidade de alguns filmes, foram realizadas medidas de reflectometria de raios X. Os resultados mostram que a incorporação de uma pequena quantidade de nitrogênio resulta em uma diminuição substancial na dessorção de GeO e na formação de uma barreira eficiente contra a oxidação adicional do substrato. Átomos de nitrogênio incorporados na estrutura do óxido podem reduzir a difusividade das vacâncias de oxigênio, levando ao aumento da estabilidade térmica. / The thermal instability of germanium oxide (GeO2) hinders the use of germanium (Ge) as the semiconductor material in MOSFET devices. This instability is induced by oxygen vacancies originated from the interfacial reaction between the oxide and the substrate. These vacancies are responsible for GeO desorption from the oxide surface and deterioration of the device’s eletrical properties. Previous studies suggest that nitrogen incorporation increases the oxide’s stability. In this dissertation, germanium oxynitride (GeOxNy) films were thermally grown on Ge using nitric oxide (NO) gas, in a conventional resistively heated furnace. Ion beam analysis tecniques, such as Rutherford backscattering spectrometry and nuclear reaction analysis, were used to investigate atomic transport during thermal growth and the role of nitrogen in the improved stability. Film thickness, density and roughness were obtained through X-ray reflectometry. Results show that the incorporation of a small amount of nitrogen yields a substantial decrease in GeO desorption and the formation of a strong barrier against further oxidation of the substrate. Nitrogen atoms incorporated into the oxide structure may decrease oxygen vacancy diffusivity, leading to enhanced thermal stability.

A instabilidade térmica do óxido de germânio (GeO2) é um obstáculo à utilização de germânio (Ge) como material semicondutor em dispositivos MOSFET. Essa instabilidade é induzida por vacâncias de oxigênio originadas de uma reação interfacial entre o óxido e o substrato. Essas vacâncias são responsáveis pela dessorção de GeO da superfície do óxido e pela deterioração das propriedades elétricas do transistor. Estudos sugerem que a incorporação de nitrogênio no GeO2 aumenta a sua estabilidade. Nesta dissertação, filmes de oxinitreto de germânio (GeOxNy) foram crescidos termicamente sobre Ge, utilizando gás óxido nítrico (NO), em um forno aquecido resistivamente. Técnicas de análise por feixe de íons, como espectrometria de retroespalhamento Rutherford e análise por reações nucleares, foram utilizadas para investigar o transporte atômico durante o crescimento dos filmes e o papel do nitrogênio na estabilização do óxido. Para a determinação da espessura, da densidade e da rugosidade de alguns filmes, foram realizadas medidas de reflectometria de raios X. Os resultados mostram que a incorporação de uma pequena quantidade de nitrogênio resulta em uma diminuição substancial na dessorção de GeO e na formação de uma barreira eficiente contra a oxidação adicional do substrato. Átomos de nitrogênio incorporados na estrutura do óxido podem reduzir a difusividade das vacâncias de oxigênio, levando ao aumento da estabilidade térmica. / The thermal instability of germanium oxide (GeO2) hinders the use of germanium (Ge) as the semiconductor material in MOSFET devices. This instability is induced by oxygen vacancies originated from the interfacial reaction between the oxide and the substrate. These vacancies are responsible for GeO desorption from the oxide surface and deterioration of the device’s eletrical properties. Previous studies suggest that nitrogen incorporation increases the oxide’s stability. In this dissertation, germanium oxynitride (GeOxNy) films were thermally grown on Ge using nitric oxide (NO) gas, in a conventional resistively heated furnace. Ion beam analysis tecniques, such as Rutherford backscattering spectrometry and nuclear reaction analysis, were used to investigate atomic transport during thermal growth and the role of nitrogen in the improved stability. Film thickness, density and roughness were obtained through X-ray reflectometry. Results show that the incorporation of a small amount of nitrogen yields a substantial decrease in GeO desorption and the formation of a strong barrier against further oxidation of the substrate. Nitrogen atoms incorporated into the oxide structure may decrease oxygen vacancy diffusivity, leading to enhanced thermal stability.

Este trabalho tem por objetivo a caracterização de filmes finos de óxido de alumínio produzidos por deposição assistida por feixe de íons Ar+. Tal caracterização consiste em estabelecer a relação entre os parâmetros de produção (energia do feixe e uxo relativo de Ar), a composição e a estrutura dos lmes. Para tanto, utiliza-se técnicas de microscopia de força atômica, difração de raios-x, reetividade de raios-x e análise por feixe iônico. Resultados mostram que amostras produzidas à temperatura ambiente e à 450 oC são amorfas independentemente da energia do feixe iônico. Filmes formados com assistência de feixe possuem qualidade superior àqueles formados por deposição física de vapor. O bombardeamento de íons Ar+ mostra-se capaz de controlar a concentração de hidrogênio, a estequiometria, a rugosidade, o tamanho dos grãos e a densidade dos lmes nos. Amostras com excelente qualidade baixa rugosidade, estequiometria próxima da ideal e boa densidade foram produzidas utilizando íons com energia dentre 300 eV e 600 eV. / The scope of this work is the characterization of aluminum oxide thin films produced by Ar+ ion beam assisted deposition. This characterization consists in establishing the relationship between production parameters (ion beam energy and argon relative ux), structure and composition of these lms. In order to undertake this task, the following techniques were used: atomic force microscopy, x-ray diraction, x-ray reectivity and ion beam analysis. Results show that samples produced at room temperature and at 450 oC are amorphous regardless the ion beam energy. Films grown under ion assistance have better characteristics than the ones deposited by physical vapor deposition. The ion beam bombardment is capable of controlling hydrogen concentration, stoichiometry, roughness, grain size and density of alumina samples. High quality lms at surface and increased density lms with near ideal stoichiometry were produced with 300 eV and 600 eV ion beam energy.

A instabilidade térmica do óxido de germânio (GeO2) é um obstáculo à utilização de germânio (Ge) como material semicondutor em dispositivos MOSFET. Essa instabilidade é induzida por vacâncias de oxigênio originadas de uma reação interfacial entre o óxido e o substrato. Essas vacâncias são responsáveis pela dessorção de GeO da superfície do óxido e pela deterioração das propriedades elétricas do transistor. Estudos sugerem que a incorporação de nitrogênio no GeO2 aumenta a sua estabilidade. Nesta dissertação, filmes de oxinitreto de germânio (GeOxNy) foram crescidos termicamente sobre Ge, utilizando gás óxido nítrico (NO), em um forno aquecido resistivamente. Técnicas de análise por feixe de íons, como espectrometria de retroespalhamento Rutherford e análise por reações nucleares, foram utilizadas para investigar o transporte atômico durante o crescimento dos filmes e o papel do nitrogênio na estabilização do óxido. Para a determinação da espessura, da densidade e da rugosidade de alguns filmes, foram realizadas medidas de reflectometria de raios X. Os resultados mostram que a incorporação de uma pequena quantidade de nitrogênio resulta em uma diminuição substancial na dessorção de GeO e na formação de uma barreira eficiente contra a oxidação adicional do substrato. Átomos de nitrogênio incorporados na estrutura do óxido podem reduzir a difusividade das vacâncias de oxigênio, levando ao aumento da estabilidade térmica. / The thermal instability of germanium oxide (GeO2) hinders the use of germanium (Ge) as the semiconductor material in MOSFET devices. This instability is induced by oxygen vacancies originated from the interfacial reaction between the oxide and the substrate. These vacancies are responsible for GeO desorption from the oxide surface and deterioration of the device’s eletrical properties. Previous studies suggest that nitrogen incorporation increases the oxide’s stability. In this dissertation, germanium oxynitride (GeOxNy) films were thermally grown on Ge using nitric oxide (NO) gas, in a conventional resistively heated furnace. Ion beam analysis tecniques, such as Rutherford backscattering spectrometry and nuclear reaction analysis, were used to investigate atomic transport during thermal growth and the role of nitrogen in the improved stability. Film thickness, density and roughness were obtained through X-ray reflectometry. Results show that the incorporation of a small amount of nitrogen yields a substantial decrease in GeO desorption and the formation of a strong barrier against further oxidation of the substrate. Nitrogen atoms incorporated into the oxide structure may decrease oxygen vacancy diffusivity, leading to enhanced thermal stability.

Controlled thermonuclear fusion may become an attractive future electrical power source. The most promising of all fusion machine concepts is called a tokamak. The fuel, a plasma made of deuterium and tritium, must be confined to enable the fusion process. It is also necessary to protect the wall of tokamaks from erosion by the hot plasma. To increase wall lifetime, the high-Z metal tungsten is foreseen as wall material in future fusion devices due to its very high melting point. This thesis focuses on the following consequences of plasma impact on a high-Z wall: (i) erosion, transport and deposition of high-Z wall materials; (ii) fuel retention in tokamak walls; (iii) long term effects of plasma impact on structural machine parts; (iv) dust production in tokamaks. An extensive study of wall components has been conducted with ion beam analysis after the final shutdown of the TEXTOR tokamak. This unique possibility offered by the shutdown combined with a tracer experiment led to the largest study of high-Z metal migration and fuel retention ever conducted. The most important results are:   - transport is greatly affected by drifts and flows in the plasma edge; - stepwise transport along wall surfaces takes place mainly in the toroidal direction; - fuel retention is highest on slightly retracted wall elements; - fuel retention is highly inhomogeneous.   A broad study on structural parts of a tokamak has been conducted on the TEXTOR liner. The plasma impact does neither degrade mechanical properties nor lead to fuel diffusion into the bulk after 26 years of duty time. Peeling deposition layers on the liner retain fuel in the order of 1g and represent a dust source. Only small amounts of dust are found in TEXTOR with overall low deuterium content. Security risks in future fusion devices due to dust explosions or fuel retention in dust are hence of lesser concern. / <p>QC 20170630</p>

Obwohl Wasserstoff omnipräsent ist, ist seine Analytik anspruchsvoll und es stehen nur wenige analytische Verfahren zur Auswahl. Unter diesen nimmt die auf einer Kernreaktion von Wasserstoff und Stickstoff basierende N-15-Methode einen herausragenden Platz ein. Sie liefert eine ortsaufgelöste Wasserstoffkonzentration bis in den ppm-Bereich in oberflächennahen Schichten (kleiner 2 µm). Gegenstand der Arbeit sind die Darstellung der Theorie der N-15-Kernreaktionsanalyse (NRA), des experimentellen Aufbaus des entsprechenden Strahlrohrs am Ionenbeschleuniger der BAM und der Auswertung der Messergebnisse. Ziel ist die erstmalige Charakterisierung eines Referenzmaterials für die H-Analytik auf Basis von amorphen Silizium (aSi) auf einem Si[100]-Substrat. International wird von den metrologischen Instituten NIST [REE90] und IRMM [VAN87] je ein Referenzmaterial für die Heißextraktion in Form von Titanplättchen angeboten. Diese sind aber für die oberflächennahen Verfahren (NRA, ERDA, GDOES, SIMS) nicht nutzbar, da die oberflächennahe Konzentration von Wasserstoff in Titan nicht konstant ist. Die Homogenität der mittels CVD abgeschiedenen aSi:H-Schichten wurde untersucht. Dazu wurden pro Substrat für ca. 30 Proben die Wasserstofftiefenprofile gemessen, mittels eines innerhalb der Arbeit entstandenen Programms entfaltet und der statischen Auswertung unterzogen. Das Ergebnis waren Mittelwert und Standardabweichung der Wasserstoffkonzentration, sowie ein Schätzer für den Beitrag der Inhomogenität zur Meßunsicherheit. Die Stabilität des potentiellen Referenzmaterials wurde durch die Konstanz der Ergebnisse von Wiederholtungsmessungen der Wasserstoffkonzentrtion während der Applikation einer hohen Dosis von N-15 Ionen bewiesen. In einem internationalen Ringversuch wurde die Rückführbarkeit der Messergebnisse nachgewiesen. Teilnehmer waren 13 Labore aus 7 Ländern. Eingesetzt wurden N-15 und F-19 NRA, ERDA und SIMS. Besonderer Beachtung wurde der Bestimmung der Messunsicherheiten gewidmet. Für die Charakterisierung der aSi:H-Schichten wurden neben der NRA die Weißlichtinterferometrie, Ellipsometrie, Profilometrie und Röngenreflektometrie, sowie die IR- und Ramanspektroskopie genutzt. Die Stöchiometrie des eingesetzten Standardmaterials Kapton wurde mittels NMR-Spekroskopie und CHN-Analyse überprüft. [VAN87] Vandendriessche, S., Marchandise, H., Vandecasteele, C., The certification of hydrogen in titanium CRM No318, Brüssel-Luxembourg,1987 [REE90] Reed, W.P., Certificate of Analysis SRM 352c, Gaithersburg, NIST, 1990

The methods of analysis with a focused ion beam, commonly termed as nuclear microscopy, include quantitative physical processes like PIXE and RBS. The element concentrations in a sample can be quantitatively mapped with a sub-micron spatial resolution and a sub-ppm sensitivity. Its fully quantitative and non-destructive nature makes it particularly suitable for analysing biological samples. The applications in biomedical research are manifold. The iron overload hypothesis in Parkinson\\\''s disease is investigated by a differential analysis of human substantia nigra. The trace element content is quantified in neuromelanin, in microglia cells, and in extraneuronal environment. A comparison of six Parkinsonian cases with six control cases revealed no significant elevation in iron level bound to neuromelanin. In fact, a decrease in the Fe/S ratio of Parkinsonian neuromelanin was measured, suggesting a modification in its iron binding properties. Drosophila melanogaster, or the fruit fly, is a widely used model organism in neurobiological experiments. The electrolyte elements are quantified in various organs associated with the olfactory signalling, namely the brain, the antenna and its sensilla hairs, the mouth parts, and the compound eye. The determination of spatially resolved element concentrations is useful in preparing the organ specific Ringer\\\''s solution, an artificial lymph that is used in disruptive neurobiological experiments. The role of trace elements in the progression of atherosclerosis is examined in a pilot study. A differential quantification of the element content in an induced murine atherosclerotic lesion reveals elevated S and Ca levels in the artery wall adjacent to the lesion and an increase in iron in the lesion. The 3D quantitative distribution of elements is reconstructed by means of stacking the 2D quantitative maps of consecutive sections of an artery. The feasibility of generating a quantitative elemental rodent brain atlas by Large Area Mapping is investigated by measuring at high beam currents. A whole coronal section of the rat brain was measured in segments in 14 h. Individual quantitative maps of the segments are pieced together to reconstruct a high-definition element distribution map of the whole section with a subcellular spatial resolution. The use of immunohistochemical staining enhanced with single elements helps in determining the cell specific element content. Its concurrent use with Large Area Mapping can give cellular element distribution maps.

Neste trabalho, estudamos e aplicamos técnicas analíticas com feixes iônicos para a identificação e quantificação do elemento químico Boro em amostras de Boro depositado sobre Níquel 11B/Ni, sobre Silício B/Si e em amostras de Silício Grau Metalúrgico - SiGM. Estas últimas foram fornecidas pelo grupo de metalurgia do Instituto de Pesquisas Tecnológicas (IPT). Especificamente, as seguintes técnicas analíticas foram utilizadas: Nuclear Reaction Analysis - NRA, Elastic Recoil Detection Analysis - ERDA e Secondary Ion Mass Spectrometry - SIMS. Nas amostras de B/Ni e B/Si, as concentrações foram obtidas com medidas de NRA, ERDA e SIMS. Também foi abordado quais dentre essas três técnicas apresentam menor limite de deteção e menor incerteza para a quantificação de Boro. Usando a reação nuclear 11B(p,a0)8Be, foi possível calcular a sua seção de choque diferencial para ângulo de espalhamento theta=170, cujo resultado, para este ângulo específico, é inédito na literatura. As amostras de SiGM foram analisadas com a técnica SIMS e comparadas com medidas de Inductively Coupled Plasma - ICP realizadas pelo grupo do IPT. Uma vez que técnicas nucleares podem ser consideradas absolutas, concluímos que as medidas de ICP apresentaram dados compatíveis com as medidas SIMS, e que o grupo de metalurgia do IPT está medindo as concentrações de Boro em suas amostras de SiGM corretamente por meio de ICP. Uma reta de calibração entre medidas SIMSxICP foi construída, que poderá servir como um guia para futuras quantificações de Boro com ICP feitas pelo grupo de metalurgia do IPT. / In this work we investigated the use of analytical techniques based on ion beams in the quantification of Boron in many kinds of samples. Specifically, we applied techniques such Nuclear Reaction Analysis (NRA), Elastic Recoil Detection Analysis (ERDA) and Secondary Ion Mass Spectrometry (SIMS) to 11B/Ni and B/Si samples to measure the boron concentration. We also discuss and show what technique has a better detection limit and lower uncertainty. For the first time in the literature, we obtained the cross section for the $^{11}B(p,\\alpha_0){^8}Be$ nuclear reaction in the energy range from 1.6 up to 2.0 MeV in theta = 170 scattering angle. The SIMS technique was applied to analise samples of metallurgical grade silicon (SiGM) from Metallurgy Group of Instituto de Pesquisas Tecnologicas (IPT) to check the Inductively Coupled Plasma (ICP) measurements carried out by the IPT. Moreover, it was possible to build a calibration curve between SIMS and ICP measurements, that can be used to help of Metallurgy Group with futures ICP\'s measurements.

Neste trabalho, estudamos e aplicamos técnicas analíticas com feixes iônicos para a identificação e quantificação do elemento químico Boro em amostras de Boro depositado sobre Níquel 11B/Ni, sobre Silício B/Si e em amostras de Silício Grau Metalúrgico - SiGM. Estas últimas foram fornecidas pelo grupo de metalurgia do Instituto de Pesquisas Tecnológicas (IPT). Especificamente, as seguintes técnicas analíticas foram utilizadas: Nuclear Reaction Analysis - NRA, Elastic Recoil Detection Analysis - ERDA e Secondary Ion Mass Spectrometry - SIMS. Nas amostras de B/Ni e B/Si, as concentrações foram obtidas com medidas de NRA, ERDA e SIMS. Também foi abordado quais dentre essas três técnicas apresentam menor limite de deteção e menor incerteza para a quantificação de Boro. Usando a reação nuclear 11B(p,a0)8Be, foi possível calcular a sua seção de choque diferencial para ângulo de espalhamento theta=170, cujo resultado, para este ângulo específico, é inédito na literatura. As amostras de SiGM foram analisadas com a técnica SIMS e comparadas com medidas de Inductively Coupled Plasma - ICP realizadas pelo grupo do IPT. Uma vez que técnicas nucleares podem ser consideradas absolutas, concluímos que as medidas de ICP apresentaram dados compatíveis com as medidas SIMS, e que o grupo de metalurgia do IPT está medindo as concentrações de Boro em suas amostras de SiGM corretamente por meio de ICP. Uma reta de calibração entre medidas SIMSxICP foi construída, que poderá servir como um guia para futuras quantificações de Boro com ICP feitas pelo grupo de metalurgia do IPT. / In this work we investigated the use of analytical techniques based on ion beams in the quantification of Boron in many kinds of samples. Specifically, we applied techniques such Nuclear Reaction Analysis (NRA), Elastic Recoil Detection Analysis (ERDA) and Secondary Ion Mass Spectrometry (SIMS) to 11B/Ni and B/Si samples to measure the boron concentration. We also discuss and show what technique has a better detection limit and lower uncertainty. For the first time in the literature, we obtained the cross section for the $^{11}B(p,\\alpha_0){^8}Be$ nuclear reaction in the energy range from 1.6 up to 2.0 MeV in theta = 170 scattering angle. The SIMS technique was applied to analise samples of metallurgical grade silicon (SiGM) from Metallurgy Group of Instituto de Pesquisas Tecnologicas (IPT) to check the Inductively Coupled Plasma (ICP) measurements carried out by the IPT. Moreover, it was possible to build a calibration curve between SIMS and ICP measurements, that can be used to help of Metallurgy Group with futures ICP\'s measurements.