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Preparação e caracterização de nanoestruturas de carbono contendo nitrogênio / Synthesis and characterization of carbon nanostructires containing nitrogenParedez Angeles, Pablo Jenner 07 October 2007 (has links)
Orientador: Fernando Alvarez / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin / Made available in DSpace on 2018-08-09T10:47:17Z (GMT). No. of bitstreams: 1
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Previous issue date: 2007 / Resumo: Nesta tese são apresentados os efeitos nas propriedades estruturais, eletrônicas e de emissão eletrônica por efeito de campo elétrico induzidos pela incorporação de nitrogênio em nanoestruturas de carbono. As nanoestruturas de carbono contendo nitrogênio foram preparadas por pulverização catódica (sputtering) de um alvo de grafite assistido, ou não, por um feixe iônico. A técnica permite atuar sobre os parâmetros de deposição induzindo mudanças nas propriedades estruturais, eletrônicas e de emissão eletrônica por efeito de campo elétrico. O papel do hélio na formação de nanoes-truturas de carbono contendo nitrogênio foi também explorado, mostrando que o gás nobre promove maior incorporação de nitrogênio. Isto é provavelmente devido à relativa alta condutividade térmica que apresenta o hélio, propriedade que modifica a cinética do crescimento das nanoestruturas. O estudo realizado permitiu entender o mecanismo de formação das nanoestruturas, mostrando que primeiramente o carbono alcança as partículas de Ni por difusão até a saturação do metal, iniciando a formação das camadas grafíticas sobre a partícula de Ni, camadas que foram observadas por microscopia eletrônica de transmissão de alta resolução. O estudo mostra, também, que os parâmetros importantes que controlam a incorporação de nitrogênio no material são a pressão parcial de nitrogênio na câmara de deposição, assim como a energia do feixe de íons assistindo a deposição.Foram estudadas três séries de amostras preparadas em atmosferas controladas.
Na primeira série foi utilizado um feixe de íons de nitrogênio como feixe de assistência, e na segunda, uma mistura composta por duas espécies iônicas, íons de nitrogênio e hidrogênio. Com o auxilio da espectroscopia de elétrons fotoemitidos por raios-X observou-se a incorporação de nitrogênio nos filmes. A microscopia de força atômica revelou a presença de estruturas do tipo domo, distribuídas de maneira uniforme na superfície das amostras, apresentando uma densidade média de ~3×10 9 domos/cm 2as da primeira série, e ~1.4×10 9 domos/cm 2as da segunda série. Tanto a distribuição como a forma seguem o padrão estabelecido pelos precursores utilizados na preparação das nanoestruturas, i.e., ilhas de níquel que agem ao mesmo tempo como catalisadores e como suporte para as nanoestruturas. Na terceira série, as nanoestruturas foram crescidas sobre um filme de nitreto de titânio, depositado sobre substratos de Si, pulverizando um alvo de grafite em atmosferas de nitrogênio e hélio-nitrogênio. A densidade dos domos encontrada para esta série foi de ~5.3×10 10 domos/cm 2 . Os espectros Raman das três séries apresentam as bandas G e D, o que indica a presença estruturas grafíticas com distorções representadas pela banda D. A incorporação de nitrogênio ocasiona o alargamento da banda G e aumento da razão das intensidades das bandas D e G, respectivamente, indicando uma redução da ordem estrutural com a incorporação de Nitrogênio. Finalmente, para as três séries de amostras, fez-se também um estudo das propriedades de emissão eletrônica por efeito de campo elétrico. A emissão é predominantemente por tunelamento quântico (as curvas de densidade de corrente vs campo elétrico seguem o modelo de Fowler-Nordheim) e dependem da concentração de nitrogênio assim como do processo usado na preparação das amostras / Abstract: The subject of this thesis is establishing a link among the synthesis, structures, and field emission properties for nanostructured carbon materials containing nitrogen. The materials were prepared by ion beam assisted deposition and ion beam sputtering. The carbon material was obtained sputtering an ultra pure graphite target by an argon ion beam. The method allows controlling the deposition parameters to induce changes in the structural, electronic, and field emission properties. Also, the role of helium on the carbon containing nitrogen nanostructures was investigated. The remarkable thermal conductance of He modifying the growing kinetics was also studied. An important goal of the work was to elucidate the mechanism of the nanostructures formation. It was found that, at first, the carbon atoms reach the Ni particles saturating the metal particle, and then, the formation of stacked graphene starts on the metal particles. The graphene layers were observed by high resolution transmission electron microscopy. The results show that mainly two parameters control the nitrogen incorporation, namely, the deposition chamber nitrogen partial pressure and the energy of the nitrogen ion beam assisting the growth. Three sample series prepared in controlled atmospheres were studied.
The first series was prepared assisting the growth with a nitrogen ion beam and, the second series by a nitrogen-hydrogen ion beam. The third sample series were prepared by ion beam sputtering on silicon substrate by sequentially depositing titanium nitride thin film, nanometric nickel particles and carbon. The carbon containing nitrogen nanostructures were grown in nitrogen and helium-nitrogen atmospheres. X-ray photoelectron spectroscopy analysis indicates nitrogen incorporation and it depends predominantly on the ion beam energy or on the nitrogen partial pressure. Atomic force microscopy reveals dome-like structures uniformly distributed on the surface of the samples, with ~3×10 9 domes/cm 2 for the first series, ~1.4×10 9 domes/cm 2 for the second, and ~5.3×10 10 domes/cm 2 for the third. Both distribution and shape follow the Ni island pattern, i.e. the Ni islandsact both as a catalytic and uphold. The three samples series were also analyzed by Raman spectros-copy, showing a defined G bands around 1593 cm -1 indicating the presence of graphitic structures. Also, are observed D bands indicating structural disorder. The disorder increases with the augment of the nitrogen content, as is shown by the augment of the D and G intensities ratio.
Finally, the field emission properties of the three series were studied and the electron emission depends on the growing conditions in general, and on the nitrogen content in particular. The results show that the emission is predominantly by quantum tunneling and the current density vs. electric field curves follow the Fowler-Nordheim model / Doutorado / Física / Doutor em Ciências
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Simulação acelerada de baixo custo para aplicações em nanoengenharia de materiais / Low cost accelerated simulation for application in nanoengineering materialsTuratti, Luiz Gustavo, 1977- 23 August 2018 (has links)
Orientadores: Jacobus Willibrordus Swart, Stanislav Moshkalev / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Elétrica e de Computação / Made available in DSpace on 2018-08-23T22:11:44Z (GMT). No. of bitstreams: 1
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Previous issue date: 2013 / Resumo: Este é um trabalho multidisciplinar que aborda questões de química, física, engenharia elétrica (nanoengenharia) e principalmente avanços obtidos com simulações por computador. Os programas comumente utilizados para simulações de fótons/íons focalizados em outro material consomem recursos computacionais por diversas horas ou até dias, para concluir os cálculos de determinado experimento, como a simulação de um processo efetuado com o equipamento FIB/SEM (Focused Ion Beam/Scanning Electron Miscroscopy), por exemplo. Através do uso de ambientes computacionais virtualizados, associados a programação paralela em CPU (Central Processing Unit) e GPGPU (General Purpose Graphics Processing Unit) é possível reduzir significativamente o tempo da simulação de horas para minutos, em situações de interação de partículas, que envolvem aproximação de colisões binárias (BCA, Binary Collision Approximation) e o Método de Monte Carlo (MMC), principalmente. O uso de placas gráficas (comumente utilizadas para jogos) potencializou o poder de processamento numérico para uso acadêmico a baixo custo, reduzindo o tempo para obtenção de resultados que foram comprovados experimentalmente. A utilização de programas análogos que empregam BCA e MMC, tais como TRIM/SRIM (Transport of Ions in Matter, atualizado para Stopping and Range of Ions in Matter), MCML (Monte Carlo for Multi Layered media) e CUDAMCML (Compute Unified Device Architecture, MCML) auxiliam a comparação de ganho de desempenho entre CPU e GPGPU evidenciando o melhor desempenho desta última arquitetura, com CUDA. Em simulações equivalentes com matrizes esparsas executadas em CPU e GPGPU, a redução do tempo de processamento variou entre três e quinze mil vezes, respectivamente. Com o Método de Monte Carlo, a redução foi de até cento e quarenta e uma vezes para melhores resultados. As simulações de alto desempenho e baixo custo computacional permitem antever algumas situações experimentais, diminuindo a necessidade de explorar todas as possibilidades práticas e, dessa forma, reduzindo o custo com laboratório / Abstract: This is a multidisciplinary work that addresses issues of chemistry, physics, electrical engineering (Nanoengineering) and especially advances obtained with computer simulations. Programs commonly used for simulations of photons/ions focused onto other materials consume computational resources for several hours or even days, to complete the simulations of a process performed with the equipment FIB/SEM (Focused Ion Beam/Scanning Electron Miscroscopy), for example. Through virtualized computing environments associated with parallel programming on CPU (Central Processing Unit) and GPGPU (General Purpose Graphics Processing Unit) is possible to significantly reduce the simulation total time from hours to minutes in the interactions of particles, involving binary collision approximation (BCA) and Monte Carlo method (MMC), mostly. The use of graphics cards (generaly used for games) enhanced the numerical processing power to be used in academia with low cost and reduced the time to obtain results experimentally verified. The use of similar software using BCA and MMC, such as TRIM/SRIM (Transport of Ions in Matter, upgraded to Stopping and Range of Ions in Matter), MCML (Monte Carlo for Multi Layered media) and CUDAMCML (Compute Unified Device Architecture, MCML) helped us to make a comparison of performance between CPU and GPGPU showing the best performance of the latter architecture, with CUDA. In equivalent simulations using sparse matrices in CPU and GPGPU, the time reduction of processing varied between three and fifteen thousand times, respectively. With the Monte Carlo method, reduction was up to one hundred forty one times for best results. Simulations of high performance and low computational cost allow us to predict some experimental situations, reducing the need to explore all practical possibilities and thus, reducing the lab costs / Doutorado / Eletrônica, Microeletrônica e Optoeletrônica / Doutor em Engenharia Elétrica
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Development of charged particle detection systems for materials analysis with rapid ion beams : large solid angle detectors and numerical nuclear pulse processing / Développement de système de détection de particules pour analyse de matériaux avec faisceau d’ions : détecteur de grande angle solide et traitement numérique des impulsions nucléairesAlarcón Díez, Víctor 14 December 2016 (has links)
Cette thèse présente de nouveaux développements en détection de particules chargées et traitement tout-numérique d'impulsions pour application à l'analyse avec des faisceaux d'ions rapides (IBA). Un ensemble de 16 détecteurs gravés sur une puce de Si est mis en œuvre, ce qui fournit un angle solide de détection environ 100 fois plus grande que celle des détecteurs utilisés auparavant pour l'IBA. Seize chaines d'acquisition sont également mises en œuvre avec une approche 'tout-numérique' pour le traitement des signaux issus des détecteurs. Dans son ensemble, le système ainsi développé a une résolution en énergie équivalent à celle des détecteurs standards. La considérable quantité d'information ainsi générée est traitée de manière cohérente en ajustant des spectres en énergie simulé aux spectres mesurés grâce à un algorithme de recuit simulé, avec le NDF DataFurnace. Les grandes angles solides disponibles sont exploitées pour des études par rétrodiffusion de Rutherford (RBS) et canalisation d'ions de l'isolant topologique Bi2Se3 enrichi en fer en vue d'études de l'effet thermoélectrique, de spintronique ou encore la computation quantique, ainsi que pour des études par RBS et analyse par réactions nucléaires (NRA) de matériaux pour la photovoltaïque organique, basés sur tetraphenyldibenzoperiflanthene (DBP) comme photo-absorbant avec oxydes de métaux de transition pour injection de charge. / This thesis presents new developments in charged particle detection and digital pulse processing for application in analysis with fast ion beams - Ion Beam Analysis (IBA). In particular a charged particle detector array, consisting of 16 independent charged particle detectors on a single silicon chip is implemented giving an overall solid angle of detection around two orders of magnitude greater than the standard charged particle detectors used in IBA. Sixteen parallel data acquisition channels are implemented using a fully digital approach for nuclear pulse processing. The overall system has an energy resolution equivalent to that of standard detectors. The large amount of data generated is handled in a self-consistent way by spectrum fitting with a simulated annealing algorithm via the NDF DataFurnace. The large solid angles thus achieved are exploited in Rutherford Backscattering Spectrometry (RBS) and ion channelling studies of the topological insulator Bi2Se3 enriched in Fe, in view of studies of the thermo-electric effect, spintronics and quantum computing, and in RBS and Nuclear Reaction Analysis (NRA) studies of organic photovoltaic materials based on tetraphenyldibenzoperiflanthene (DBP) as the photo-absorber and transition metal oxide charge injectors.
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Intercalation d'alliages or-potassium et calcium-lithium dans des structures carbonées de basse dimensionnalité / Intercalation of gold-potassium and calcium-lithium alloys into low-dimensional carbon-based structuresFauchard, Mélissa 10 October 2014 (has links)
L’intercalation de métaux dans le graphite a été réalisée pour la première fois en 1926. Depuis cette découverte, de nombreux composés binaires et ternaires ont été synthétisés. Au cours de ce travail, la méthode solide-liquide en milieu alliage fondu à base d’alcalin a d’abord été utilisée afin d’intercaler l’or dans le graphite à l’aide du potassium. Puis, l’intercalation du calcium dans des matériaux B-C-N de structure graphitique a été réalisée par le biais du lithium. La diffraction des rayons X, l’analyse par faisceau d’ions, la microscopie électronique ainsi que les techniques spectroscopiques associées ont été mises en œuvre pour caractériser ces nouveaux composés. Dans le cas du système graphite-potassium-or, trois nouveaux composés ternaires de premier stade et de distances interplanaires très différentes (1311, 953 et 500 pm) ont pu être synthétisés. Le composé K1,3Au1,5C4 a été isolé de façon reproductible et présente selon l’axe c une séquence d’empilement K-Au-Au-Au-K pour l’insérat. L’étude du mécanisme d’intercalation menant à ce composé a mis en évidence un intermédiaire réactionnel de formule K1,6Au0,7C4 dont le feuillet inséré est tricouche. Le troisième composé, KAu0,7C4, constitué de deux couches mixtes or-potassium, s’est quant à lui révélé métastable. Parallèlement, l’intercalation d’un alliage Li-Ca dans le matériau B-C-N a été réalisée avec succès. L’analyse par faisceau d’ions de l’hôte a permis de doser sur un même échantillon la teneur en bore, carbone et azote, conduisant à une formule B2C5N. Les mesures effectuées sur le matériau intercalé montrent la préservation du réseau hôte et l’insertion de 0,6 atome de lithium par atome de calcium / Since the discovery in 1926 of the first graphite intercalation compounds containing alkali metals, numerous binary and ternary compounds have been synthesized. In this work, solid-liquid method in alkali metal based molten alloys has been employed to intercalate gold into graphite using potassium as an intercalation vector for opening the van der Waals’s gaps and decreasing the reaction temperature. Then, lithium has been used to assist the intercalation of calcium into B-C-N compounds. X-ray diffraction, ion beam analysis, electron microscopy and associated spectroscopy techniques have been performed to characterize the as-prepared compounds. In the case of graphite-potassium-gold system, three novel ternary first stage intercalation compounds with very different repeat distances (1311, 953 and 500 pm) have been synthesized. The K1.3Au1.5C4 compound, isolated in a reproducible fashion, presents a K-Au-Au-Au-K c-axis stacking sequence for the intercalated sheets. The study of its intercalation mechanism evidenced an intermediate product which chemical formula is K1.6Au0.7C4, with three-layered intercalated sheets. The third compound KAu0.7C4 is metastable and contains in each van der Waals‘s gap two successive layers containing a mixture of gold and potassium. Elsewhere, the intercalation of a Li-Ca alloy into B-C-N host material has been successfully carried out. The ion beam analysis of the pristine B-C-N lead to determine on a same sample the amount of boron, carbon and nitrogen with the corresponding B2C5N formula. The experiments realized on the intercalated compound showed the preservation of the host lattice and the intercalation of 0.6 lithium per calcium atom
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Fabrication and electrical characterisation of quantum dots : uniform size distributions and the observation of unusual electrical characteristics and metastabilityJames, Daniel January 2010 (has links)
Quantum dots (QDs) are a semiconductor nanostructure in which a small island of one type of semiconductor material is contained within a larger bulk of a different one. These structure are interesting for a wide range of applications, including highly efficient LASERs, high-density novel memory devices, quantum computing and more. In order to understand the nature of QDs, electrical characterisation techniques such as capacitance-voltage (CV) profiling and deep-level transient spectroscopy (DLTS) are used to probe the nature of the carrier capture and emission processes. This is limited, however, by the nature of QD formation which results in a spread of sizes which directly affects the energy structure of the QDs. In this work, I sought to overcome this by using Si substrates patterned with a focused ion beam (FIB) to grow an array of identically-sized Ge dots. Although I was ultimately unsuccessful, I feel this approach has great merit for future applications.In addition, this thesis describes several unusual characteristics observed in InAs QDs in a GaAs bulk (grown by molecular beam epitaxy-MBE). Using conventional and Laplace DLTS, I have been able to isolate a single emission transient. I further show an inverted relation between the emission rate and the temperature under high field (emissions increase at lower temperatures). I attribute this to a rapid capture to and emission from excited states in the QD. In addition, I examine a metastable charging effect that results from the application of a sustained reverse bias and decreases the apparent emission rate from the dots. I believe this to be the result of a GaAs defect with a metastable state which acts as a screen, inhibiting emission from the dots due to an accumulation of charge in the metastable state. These unusual characteristics of QDs require further intensive work to fully understand. In this work I have sought to describe the phenomena fully and to provide hypotheses as to their origin.
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Fabrication and characterization of sige-based core-shell nanostructures / Fabrication et caractérisation de nanostructures Coeur-Coquille à base de silicium germaniumBenkouider, Abdelmalek 23 October 2015 (has links)
Du fait de leur facilité de fabrication et de leurs propriétés physiques uniques, les nanofils (NFs) de semi-conducteurs présentent des potentialités d’application importantes elles pouvaient être comme briques élémentaires de nombreux dispositifs nano- et opto-électroniques. Différents procédés de fabrication ont été développés pour fabriquer et organiser ces nanofils en épitaxie sur silicium. Cependant, un des principaux problèmes réside dans le manque de reproductibilité des NFs produits naturellement. Pour obtenir un meilleur contrôle de leur périodicité, localisation, forme et taille, différents types de gravure ont été mis au point. Aujourd’hui, des incertitudes importantes persistent quant à leurs propriétés fondamentales, en raison d’un manque de corrélation entre les propriétés électroniques et optiques et les détails microscopiques (composition, structure, chimie ...etc.). L’objectif de ce travail est de développer deux types de procédés de fabrication : le premier "top-down" est basé sur la nanogravure directe par faisceau d’ions focalisés (FIB)de couches bi-dimonsionnelles de SiGe. Ce procédé permet de contrôler la taille des NFs, les déformations, et leur localisation précise. Il permet de fabriquer des réseaux de larges piliers. Les NFs réalisés par cette technique sont peu denses et de diamètre important. Le second procédé est de type "Bottom-Up" ; il s’appuie sur la croissance VLS à partir de catalyseurs métalliques (AuSi). Les NFs réalisés ont étudiés à l’échelle locale afin de mesurer la taille moyenne de contrainte ainsi que leur effet sur le confinement quantique et sur la structure de bande des NFs. / SiGe/Si core/shell nanowires (NWs) and nanodots (NDs) are promising candidates for the future generation of optoelectronic devices. It was demonstrated that the SiGe/Si heterostructure composition, interface geometry, size and aspect ratios can be used to tune the electronic properties of the nanowires. Compared to pure Si or Ge nanowires, the core-shell structures and exhibit extended number of potential configurations to modulate the band gap by the intrinsic strain. Moreover, the epitaxial strain and the band-offsets produce a better conductance and higher mobility of charge carriers. Recent calculations reported that by varying the core-shell aspect ratio could induce an indirect to direct band gap transition. One of the best configurations giving direct allowed transitions consists of a thin Si core embedded within wide Ge shell. The Germanium condensation technique is able to provide high Ge content (> 50%) shell with Si core whom thickness of core and shell can be accurately tuned. The aim of this work is to develop two types of synthesis processes: the first "top-down" will be based on direct nanoetching by focused ion beam (FIB) of 2D SiGe layer. This process allows the control of the size of NWs, and their precise location. The NWs achieved by this technique are not very dense and have a large diameter. The second processes called "bottom-up"; are based on the VLS growth of NWs from metal catalysts (AuSi). Grown NWs have been studied locally in order to measure the mean size and the strain and their effects on the quantum confinement and band structure of NWs.
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Studium vlastností povrchových plazmonových polaritonů na magnetických materiálech / Study of Properties of Surface Plasmon Polaritons on Magnetic MaterialsDvořák, Petr January 2011 (has links)
The diploma thesis deals with the experimental study of surface plasmon polaritons (SPPs) on nano-structures with the Au/Co/Au multilayer. Plasmonic structures were prepared by the electron beam lithography and by the focused ion beam. A Scanning optical near-field microscope was used for detection of surface plasmon polaritons. SPPs were confirmed by the experiment with different polarizations of the illuminating light. Furthermore, differences in plasmon interference wavelengths was measured for different surface dielectric functions. Finally, the decantation of the SPPs interference image was measured in dependence on the external magnetic field.
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Magnetická transformace metastabilních vrstev fcc Fe/Cu(100) pomocí fokusovaného iontového svazku / Magnetic transformation of metastable fcc Fe/Cu(100) films by focused ion beamGloss, Jonáš January 2014 (has links)
Metastable paramagnetic face-centered cubic (fcc) Fe thin films deposited on a Cu(100) single-crystal are good candidates for focused ion-beam magnetic patterning, due to their structural and magnetic phase transformation to ferromagnetic body-centered cubic (bcc) Fe upon ion-beam irradiation. However, pure fcc Fe films undergo spontaneous transformation when their thickness exceeds 10 ML. This limit can be extended to approximately 22 ML by deposition of Fe at increased CO background pressures. We show that much thicker films can be grown by alloying with Ni, that stabilizes the fcc phase. The amount of Ni necessary to stabilize non-magnetic, metastable fcc Fe films in dependence on the residual background pressure during the deposition is determined and a phase diagram revealing the metastable region is presented. It is also shown that the stabilizing effect of CO can be removed by artificial O saturation of the surface and thus the Ni-stabilized films can be grown also in systems with lower vacuum. Finally, we present fabrication of micro- and nanostructures in 44 ML thick films of Fe alloyed with Ni on Cu(100) by focused ion beam.
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Development of a Versatile High-Brightness Electron Impact Ion Source for Nano-Machining, Nano-Imaging and Nano-Analysis / Développement d'une source d'ions polyvalente à haute brillance basée sur l'impact électronique pour la nano-fabrication, la nano-imagerie et la nano-analyseCastro, Olivier de 07 December 2016 (has links)
Les nano-applications utilisant des faisceaux d'ions focalisés nécessitent des sources d'ions à haute brillance avec une faible dispersion en énergie (ΔE) ce qui permet une excellente résolution latérale et un courant d'ions suffisamment élevé pour induire des vitesses d'érosion raisonnables et des rendements élevés d'émission électronique et ionique. Les objectifs de cette thèse sont le développement d'une source d'ions basée sur l'impact électronique ayant une brillance réduite Br de 10³ – 10⁴ A m⁻² sr ⁻ ¹ V⁻ ¹, une dispersion en énergie ΔE ≲ 1 eV et un choix polyvalent d'ions. Le premier concept évalué consiste à focaliser un faisceau d'électrons à une énergie de 1 keV entre deux électrodes parallèles distant de moins d'un millimètre. Le volume d'ionisation « micrométrique » est formé au-dessus d'une ouverture d'extraction de quelques dizaines de µm. En utilisant un émetteur d'électrons LaB₆ et une pression de 0.1 mbar dans la région d'ionisation, Br est proche de 2.10² A m⁻² sr ⁻ ¹ V ⁻ ¹ avec des tailles de source de quelques µm, des courants de quelques nA pour Ar⁺/Xe⁺/O₂ ⁺ et une dispersion en énergie ΔE < 0.5 eV. La brillance réduite Br est encore en dessous de la valeur minimum de notre objectif et la pression de fonctionnement très faible nécessaire pour l'émetteur LaB₆ ne peut être obtenue avec une colonne d'électrons compacte, donc ce prototype n'a pas été construit.Le deuxième concept de source d'ions évalué est basé sur l’idée d’obtenir un faisceau ionique à fort courant avec une taille de source et un demi-angle d’ouverture similaire aux résultats du premier concept de source, mais en changeant l’interaction électron-gaz et la collection des ions. Des études théoriques et expérimentales sont utilisées pour l’évaluation de la performance de ce deuxième concept et de son utilité pour les nano-applications basées sur des faisceaux d'ions focalisés. / High brightness low energy spread (ΔE) ion sources are needed for focused ion beam nano-applications in order to get a high lateral resolution while having sufficiently high ion beam currents to obtain reasonable erosion rates and large secondary electron/ion yields. The objectives of this thesis are: the design of an electron impact ion source, a reduced brightness Br of 10³ – 10⁴ A m⁻² sr⁻ ¹ V⁻ ¹ with an energy distribution spread ΔE ≲ 1 eV and a versatile ion species choice. In a first evaluated concept an electron beam is focussed in between two parallel plates spaced by ≲1 mm. A micron sized ionisation volume is created above an extraction aperture of a few tens of µm. By using a LaB₆ electron emitter and the ionisation region with a pressure around 0.1 mbar, Br is close to 2.10² A m⁻² sr ⁻ ¹ V ⁻ ¹ with source sizes of a few µm, ionic currents of a few nA for Ar⁺/Xe⁺/O₂ ⁺ and the energy spread being ΔE < 0.5 eV. The determined Br value is still below the minimum targeted value and furthermore the main difficulty is that the needed operation pressure for the LaB₆ emitter cannot be achieved across the compact electron column and therefore a prototype has not been constructed. The second evaluated source concept is based on the idea to obtain a high current ion beam having a source size and half-opening beam angle similar to the first concept, but changing the electron gas interaction and the ion collection. Theoretical and experimental studies are used to evaluate the performance of this second source concept and its usefulness for focused ion beam nano-applications.
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Nachweis und Quantifizierung von NanopartikelnDorn, Marco 20 February 2015 (has links)
Die Nanotechnologie spielt eine Schlüsselrolle bei der technologischen Entwicklung. Jedoch stellen Nanopartikel ein potentielles Gesundheitsrisiko dar. Durch ihre große Oberfläche zeigen Nanopartikel eine hohe Reaktivität und die geringe Größe trägt zu einer erhöhten Beweglichkeit und Bioverfügbarkeit bei. Beispielsweise können Nanopartikel Entzündungen auslösen oder die Produktion von freien Radikalen fördern. Insbesondere Lungenepithelzellen stellen die wichtigste Barriere zur Aufnahme von industriell relevanten Nanopartikeln im Alltag dar, denn durch ihre geringe Größe können Nanopartikel bis in einzelne Alveolen vordringen und in die Blutbahn gelangen. Aus diesen Gründen ist es notwendig das Risikopotential, was von Nanopartikeln ausgeht zu bewerten. In dieser Dissertation wurden die Metalloxid-Nanopartikel Al2O3, TiO2, Fe2O3, ZnO und CeO2 in einzelnen Lungenzellen erstmals mit Hilfe der Ionenstrahlmikroskopie quantifiziert. Darüber hinaus erfolgte die Quantifizierung von ausgewählten Metalloxid-Nanopartikeln in gedehnten primären Typ 2 Pneumozyten sowie in den Alveolen des Lungengewebes. Außerdem wurden Gold und Silber als Markierungspartikel eingesetzt, um die Aufnahme der organischen Nanopartikel Graphen zu untersuchen. Die Ionenstrahlmikroskopie ist eine hochempfindliche Methode, welche durch die charakteristische Röntgenstrahlung den zellulären Elementgehalt innerhalb einer Zelle visualisieren kann. Dies ist, je nach Element, bis zu einer unteren Konzentrationsgrenze von 5 – 20 ppm möglich. Die Ionenstrahlmikroskopie erlaubt, im Vergleich zur Elektronenstrahlmikroanalyse, biologische Proben bis zu einer Tiefe von ca. 80 µm zu untersuchen. Durch das zelluläre Rückstreusignal konnte bei Kulturzellen entschieden werden, ob die Nanopartikel internalisiert wurden oder auf der Zelloberfläche assoziiert sind. Da biologische Proben eine relativ geringe Dichte und Dicke aufweisen, ist die Signalausbeute und damit die Messzeit ein limitierender Faktor bei der ionenstrahlanalytischen Quantifizierung des Elementgehalts. Durch das Aufziehen der Probe auf einen Aluminiumrahmen, konnte der Abstand zwischen Röntgendetektor und Probe reduziert werden, was zu einer höheren Signalausbeute führte und damit eine schnellere Analyse der Präparate ermöglichte. Die Art und Weise der Probenpräparation kann einen Einfluss auf den zellulären Elementgehalt haben, indem Ionen aus dem Medium an die Zellaußenseite binden oder durch die Waschlösung ein Verlust von intrazellulär lokalisierten organischen und anorganischen Molekülen entsteht. Durch den Vergleich zwischen einer ionenfreien Polyethylenglycol-Lösung mit dem üblicherweise verwendeten Waschpuffer konnte gezeigt werden, dass sich bei der Verwendung des Waschpuffers der zelluläre Elementgehalt von Kalium, Kalzium und insbesondere Chlor erhöht. Allerdings bleiben Phosphor und Schwefel als wichtige zelluläre Strukturelemente und die biologisch relevanten Spurenelemente Eisen und Zink davon unbeeinflusst. Die ionenstrahlmikroskopische Analyse von Lungengewebe erfordert eine Einbettung der Präparate. Dabei erwies sich DePeX, was als Material routinemäßig zur Einbettung verwendet wird, als ungeeignet, da eine inhomogene Zink-Kontamination vorhanden war, welche eine intrazelluläre Zink-Messung verhinderte. Durch die Entwicklung eines neuen zinkfreien Einbettmaterials auf Limonen-Basis, konnte jetzt auch die Zinkkonzentration in Alveolen gemessen werden. Im biologischen Millieu können Proteine und Ionen auf der Oberfläche der Nanopartikel adsorbieren und dadurch deren Aufnahme in die Zelle beeinflussen. Deshalb wurde die zelluläre Aufnahme in Abhängigkeit der Proteinhülle (Korona) bei in vitro Bedingungen untersucht. Tragen die Partikel eine Korona, ist bei allen untersuchten Metalloxid-Nanopartikeln eine geringere zelluläre Konzentration zu beobachten und gleichzeitig sind weniger Nanopartikel auf der Zelloberfläche adsorbiert. Die Aufnahme von CeO2 und ZnO wurde näher untersucht, da ZnO als einziger untersuchter Nanopartikel einen deutlichen toxischen Effekt hervorruft und CeO2 durch die hohe Ausbeute des Rückstreusignals und die starke zelluläre Aufnahme zum näheren Studium der Aufnahme besonders geeignet ist. Es wurde beobachtet, dass CeO2 und ZnO im extrazellulären Raum mit Phosphat und Kalzium aus dem Kulturmedium kolokalisiert sind. Da Kalziumphosphat als Transfektionsagenz bekannt ist, kann diese Modifikation der Partikeloberfläche die Aufnahme der Partikel begünstigen. Im Vergleich zu CeO2, ist bei ZnO auf Grund der erhöhten Toxizität keine Sättigung der zellulären Konzentration zu erkennen. Daneben lässt die die Halbierung der zellulären CeO2-Konzentration nach 72 Stunden Applikationszeit darauf schließen, dass die Zellen in der Lage sind die Nanopartikel durch Exozytose wieder abzugeben. Mit Hilfe von Inhibitoren wurde der Aufnahmemechanismus von CeO2-NP untersucht. Dabei zeigte sich, dass CeO2 Nanopartikel durch Caveolae- bzw. Clathrin-vermittelte Endozytose und Makropinozytose aufgenommen werden. Die Internalisierung von CeO2 und ZnO Nanopartikeln wurde mit Hilfe des zellulären Protonen-Rückstreusignals untersucht. Internalisierte Nanopartikel liefern im Vergleich zu extrazellulär assoziierten Nanopartikeln ein Rückstreusignal bei niedrigeren Energien, da die zurückgestreuten Protonen durch die Passage des Zellmaterials zusätzlich Energie verlieren. Bei diesen Untersuchungen wurde festgestellt dass, ZnO und CeO2-Nanopartikel ohne Proteinhülle häufiger an der Zelloberfläche lokalisiert sind und zu einer höheren zellulären Konzentration führen. Sowohl im Lungengewebe als auch bei gedehnten primären Typ 2 Pneumozyten und kultivierten Lungenepithelzellen zeigte sich eine sehr inhomogene zelluläre Konzentrationsverteilung der Nanopartikel. Hier liegt die Stärke der Ionenstrahlmikroskopie darin, die Konzentration in einzelnen Zellen bzw. Alveolen erfassen zu können. Dadurch erlaubt es diese Methode, das Risiko abzuschätzen, was durch die Extrembelastung in einzelnen Zellen entstehen könnte. Da Lungengewebe aus Typ I und Typ II Pneumozyten besteht und Makrophagen in das Gewebe einwandern können, ist es in zukünftigen Experimenten notwendig die einzelnen Zelltypen zu markieren, um die Nanopartikel-Aufnahme im Lungengewebe mit den Ergebnissen der Zellkultur besser vergleichen zu können. Durch eine Markierung mit Gold-konjugierten Antikörpern, kann erreicht werden, die einzelnen Zelltypen mittels Ionenstrahlmikroskopie zu identifizieren. Durch verschiedene Applikationsformen bei in vitro und in vivo Untersuchungen ist die Wirkung der Nanopartikel nur schwer vergleichbar. Aus diesem Grund wurde in dieser Arbeit das Konzept der effektiv wirksamen zellulären Dosis eingeführt. Dieses erlaubt es, der Dosis, welche tatsächlich zellulär oder im Gewebe vorhanden ist, einen toxischen Effekt der Nanopartikel zuzuordnen. Dadurch kann die effektive Dosis als wichtige Größe zum systematischen Vergleich von toxikologischen Studien auf in vitro und in vivo Basis eingesetzt werden. Die Ionenstrahlmikroskopie ist zur Zeit die einzige Methode, welche für die intrazelluläre Quantifizierung von unmarkierten Nanopartikeln auf Einzelzellebene in Frage kommt. Deshalb ist sie als zukünftige Referenzmethode für die Dosimetrie von Nanopartikeln sehr gut geeignet.
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