Les systèmes d'imagerie à rayons X (RX) sont des appareils volumineux et contraignants en termes de contrôle du faisceau. L'industrie des tubes électroniques est donc à la recherche de solutions pour assurer la stabilité du courant tout en permettant la miniaturisation du système.Ce travail opte pour l'amélioration de la source d'électrons, en remplaçant l'émission thermoïonique historique par l'émission de champ. En particulier, les cathodes froides à base de nanotubes de carbone possèdent l'avantage de pouvoir délivrer de forts courants (>1A/cm^2), tout en ayant un faible temps de réponse.A travers le développement d'une structure innovante de cathodes à nanotubes de carbone à grille intégrée, l'objectif de cette étude est de réaliser des sources commutables et régulées, pour des sources de rayons X miniatures, portables ou polyvalentes.La modélisation électrostatique de la nouvelle structure a conduit à la fabrication de cathodes à grille optimisées, sur lesquelles est cru un réseau vertical de nanotubes de carbone. L'analyse de défaillance permet finalement d'obtenir des dispositifs isolés fiables. Leur caractérisation en émission de champ indique des performances de modulation de courant inégalées, de l'ordre de 10^6 pour +/-40V de polarisation de grille. La régulation du courant a également été démontrée avec l'obtention d'une stabilité à 0,02% sur 100 h.Pour pallier les limitations rencontrées (courant de fuite et croissance parasite), une structure de grille enterrée a été proposée avec succès, ainsi qu'une nouvelle méthode de fabrication d'émetteurs courts et fins. Ces cathodes fonctionnelles ont finalement été intégrées en tube à rayons X et ont montré pour la première fois une modulation de courant de 2000 à une haute tension fixe de 60 kV. / This work chooses to improve the electron source by replacing thermionic emission with field emission. More especially, carbon nanotubes based cold cathodes stand out by their ability to supply high currents (>1A/cm^2) while responding fast.Through the development of an innovative structure of in-plane gated carbon nanotube based cathode, this study aims at making switchable and regulated sources for miniature, portable or polyvalent X-rays sources.The electrostatic modelling of the new structure led to the fabrication of optimized gated cathodes, where a vertically aligned array of carbon nanotubes is grown. Default analysis allows to get reliable insulated devices.Field emission characterization shows unprecedented current modulation of 10^6 at +/-40V bias voltage. Current regulation is also achieved with a stability of 0.02% over 100 h.Another structure with a burried gate electrode was designed to successfully cope with leak current and parasitic growth. A new way of growing short and thin nanotubes was tackled.Finally, gated cathodes were integrated in a compact X-ray tube and showed a current modulation of 2000 at a high voltage of 60 kV.

<p>   The arrival of Si transistors and integrated circuit technology more than half a century ago made vacuum electronic technology almost extinct. Today, there are only a few niche applications for vacuum electronics. The main issues with this technology are its high voltage requirement and high-power consumption, difficult and costly fabrication technology, lack of integration capability, and poor reliability characteristics. Some of these issues may be addressed by going to nm scale fabrication that did not exist 60 years ago. Other problems such as reliability and lack of integration capability require alternative solutions to what has been proposed so far. Vacuum is the ultimate conduction media allowing electrons to reach the speed of light without any scattering. Consequently, a vacuum transistor, if designed correctly, can achieve THz frequency performance, while delivering Watt-level powers. No semiconductor technology can compete with vacuum technology to deliver such performance. </p> <p>In this work, novel methods for implementing nanoscale field emitter arrays used in vacuum electronics are proposed. Gated and ungated field emitters are fabricated with self-assembly technology and electron beam lithography. Different anisotropic dry etching recipes are developed to achieve emitters with different sharpness and aspect ratios. Our methods lead to field emitter array operation under low voltages (less than 20 V) and high current densities (around 50 A/cm2) using self-assembly and soft film anode-cathode isolator, and field emitter devices with ~4.5 A/cm2 current density with a turn-on voltage less than 50 V using electron beam lithography and oxide anode-cathode isolator. </p> <p>Making reliable field emitter devices is challenging. Due to Joule heating, ion bombardment, and geometrical variations for each tip in the field emitter arrays, emission current becomes nonuniform across the array. Sharper tips emit at a higher rate and eventually, the heat generated at the tip deforms the tips leading to electron emission at a lower rate. With ultra-low doped emitters, the current of each tip is limited to a few nano-amperes leading to a negligible current fluctuation at the tips. </p> <p>Our fabricated ultra-low doped devices with both self-assembly and electron beam lithography techniques presented constant emission current with almost no change over 24 hours of continuous operation. Such excellent reliability characteristics in vacuum field emitter devices have not been demonstrated to date.</p> <p>The screening effect in close-packed field emitter arrays which occurs by nearby conductive or semiconductive objects is thoroughly investigated and different solutions are proposed to reduce this effect between the emitters. Simulation studies using Sentaurus TCAD, MATLAB, and COMSOL Multiphysics simulators facilitated the design and optimization of gated and ungated field emitter arrays. These studies included the effect of sharpness, the distance between neighboring emitters, enclosing the emitters by a Si block around the emitters as well as anode-cathode separation on the electrical characterization of field emitter arrays. </p> <p>The optimum location and operating voltages which lead to a maximum gate control and emitter current density are also studied for gated field emitter arrays. Instead of individually gating each field emitter, it was found that controlling the emission of a sub-array with a metallic all-around gate is more efficient and it leads to higher current densities. Guided by simulations, gated field emitter arrays with 5×5 and 2×2 sub-arrays are developed. In terms of strength of the grid control (transconductance), turn-on voltage, maximum emission current, and field intensification factor, the device with the 2×2 sub-array was superior to the one with the 5×5 sub-array. The VFET with 5×5 sub-arrays achieved a higher current density due to a larger number of field emitters packed per active emission area. Finally, plans to further improve the technology and transitioning into the fabrication of vacuum integrated circuits are discussed.</p> <p>  </p>

This thesis describes utilization of a nanotechnology in new pressure sensors. Detailed analysis of individual principles are carrying on. And simulations and experimental models of sensors are developed. More detailed description is provided for new capacitive pressure sensor, which is manufactured using nanotechnology, including its model and analysis in order to improve its properties. The work deals with the emission pressure sensor which uses the principle of cold emissions, including analysis comparison of the measured values of the emission current from the applied nanotubes field and analysis to improve emissions performance.

Ce travail de thèse porte sur l’étude de nouveaux phénomènes vibratoires dans les systèmes Nano-électromécaniques (NEMS) conçus à partir de nanofils (NFs) SiC ou de nanotubes de carbone (NCs) résonants. La configuration encastré-libre permet d'effectuer l'émission de champ (EC) pour caractériser nos échantillons et notamment mesurer le module de Young et le facteur de qualité (Q) de nos NEMS. Le chauffage du résonateur permet d'accroître fortement la valeur de Q des nanofils SiC (Qmax = 159 000). Les auto-oscillations observées sous EC sont obtenues seulement par l'application d'une tension continue et permettent un taux de conversion AC/DC de l'ordre de 50%. L'utilisation de NFs très résistifs couplée au courant d'EC est indispensable pour engendrer ces oscillations spontanées. La réalisation d'une nanoradio sous EC permet la démodulation d'un signal AM ou FM grâce à la résonance d'un NC. Nous décrivons une méthode originale pour exciter les vibrations d'un NF à partir du faisceau d'électrons d'un microscope électronique. L'évolution de la charge au bout du NF est la principale cause de ces auto-oscillations. La configuration encastré-encastré consiste à obtenir un transistor à base de NCs suspendus. Les composants sont caractérisés électriquement et mécaniquement dans un testeur sous pointe sous ultra vide à partir de techniques dites de mixing. La fréquence de résonance de ces échantillons est de l'ordre de 100 MHz et la démodulation d'un signal FM est réalisée pour la première fois dans cette configuration de NEMS. Pour l'ensemble des phénomènes découverts et traités dans ce manuscrit, un modèle et les simulations qui en découlent sont présentés et commentés / This thesis focuses on new phenomena in the mechanical resonances of SiC nanowires (NWs) and carbon nanotubes (CNs) of interest for the emerging field of nano-electro-mechanical systems (NEMS). The clamped-free confiuration allowed the study of our nanowire and nanotube samples by field emission (FE), including measuring the Young's modulus and the quality factor (Q). Heating NW resonators significantly increased their Q factor (Qmax = 159 000). Self-oscillations were observed during FE where only a DC voltage was applied, thus allowing DC/AC conversion with a rate of up to » 50%. Using highly resistive NWs coupled with FE current was required to generate these spontaneous oscillations. Achieving a nanoradio under FE allowed the demodulation of AM or FM signals through the mechanical resonance of CNs. We describe a new method to excite vibrations of a NW from the electron beam of an electron microscope. The evolution of the charge at the end of NW is the main source of these self-oscillations. The clamped-clamped configuration consists of a transistor based on suspended CNs. The devices are characterized electrically and mechanically in a probe station under ultrahigh vacuum with mixing techniques. The resonance frequencies of these samples was around 100 MHz. The demodulation of an FM signal was achieved for the first time in this NEMS configuration. For all the phenomena discovered and treated in this manuscript, a model and derived simulations are described and discussed

No description available.

L'étape clé pour intégrer des nanotubes de carbone à une échelle industrielle demeure un meilleur contrôle de leur croissance et notamment le contrôle sélectif de leurs chiralités en lien avec leurs propriétés électroniques. Ce travail a pour but de s'intéresser à la synthèse in-situ et à la caractérisation de nanotubes de carbone individuels par émission de champ pour mieux comprendre les mécanismes de nucléation et de croissance qui conditionnent sa chiralité. Nous avons développé un microscope à émission de champ couplé à un réacteur CVD (Chemical Vapor Deposition) pour observer directement la croissance catalytique de nanotubes de carbone individuels sur des pointes émettrices. Nous avons ainsi découvert que les nanotubes tournent souvent axialement pendant leur croissance, soutenant ainsi un modèle de « dislocation de vis ». L’analyse détaillée des résultats obtenus montre que nous observons directement la croissance atome par atome d'un nanotube monofeuillet individuel avec ajout d’un dimère de carbone à la fois à sa base. Parallèlement, des échantillons ont été caractérisés en détail sous émission de champ. Nous avons établi un protocole de collage de nanotubes individuels à l’apex d’une pointe métallique sous microscopies optique et électronique à balayage à l’aide d’un nanomanipulateur. Leur dépendance en température à très bas courant a été mise en évidence avec un compteur d’électrons afin d'identifier les différents domaines d'émission électronique. L'analyse des distributions énergétiques a fait apparaître un phénomène de chauffage induit qui peut mener à des températures de l’ordre de 2000 K à l’extrémité du nanotube lorsqu’il est soumis à un fort champ. / The key issue for realizing the potential of carbon nanotubes has always been, and still remains, a better control of their growth and in particular the selective control of their chirality related to their electronic properties. This work aims to address the in-situ synthesis and characterization of individual carbon nanotubes by field emission to better understand the mechanisms of nucleation and growth that determine their chirality. We have developed a field emission microscope coupled to a CVD reactor (Chemical Vapor Deposition) to observe directly the catalytic growth of individual carbon nanotubes on metallic tips. We found that nanotubes often turn axially during growth, thereby supporting a model of "screw dislocation". Detailed analysis of results shows that we directly observe the atom by atom growth of one individual single wall nanotube with addition of a carbon dimer to the base. In parallel, certain samples were characterized by in-depth field emission studies. For this we established a protocol of bonding individual nanotubes at the apexes of metal tips under optical and scanning electron microscopies using a nanomanipulator. Their temperature dependence at very low current has been demonstrated with an electron counter to identify the various fields of electron emission. Analysis of energy distributions revealed an induced heating phenomenon that can lead to temperatures of about 2000 K at the end of the nanotube subjected to strong fields that create high current emission.

Made available in DSpace on 2014-10-09T12:42:01Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:04:33Z (GMT). No. of bitstreams: 1 19174.pdf: 31751 bytes, checksum: 7f1e1ac2bd5fcea7b8edbb1e6ba7a12b (MD5) / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Made available in DSpace on 2014-10-09T12:42:01Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:04:33Z (GMT). No. of bitstreams: 1 19174.pdf: 31751 bytes, checksum: 7f1e1ac2bd5fcea7b8edbb1e6ba7a12b (MD5) / A Terapia de Captura de Nêutron por Boro (BNCT) é uma terapia de combate ao câncer bimodal, na qual a energia útil da terapia vem da reação nuclear que ocorre pelo Boro quando irradiado com nêutrons térmicos. No IPEN há uma instalação de pesquisas em BNCT, na qual o feixe de radiação contendo nêutrons é proveniente do reator IEA-R1. Como condição desta terapia é necessário realizar a dosimetria do feixe de radiação, que atualmente é feito com o uso de folhas de ativação, para cálculo do fluxo de nêutrons, e do dosímetro TLD 400, para estimativa da dose gama. Para campos mistos de nêutrons e gamas, a Comissão Internacional de Unidades e Medidas (ICRU) recomenda o uso de dosímetros com sensibilidades distintas para as componentes do feixe, como o caso do par TLD 600 e TLD 700 que apresentam sensibilidades distintas a nêutrons térmicos, devido à diferente quantidade do isótopo 6Li em sua composição, o qual apresenta uma alta seção de choque para nêutrons térmicos. Este trabalho constou da realização de simulações e experimentos visando a implementação da metodologia de dosimetria utilizando o par TLD 600 e TLD 700 e sua comparação com a metodologia atualmente utilizada pelo grupo de pesquisa em BNCT, que utiliza o TLD 400. Portanto, foi realizado um estudo das respostas de cada um destes TLDs a partir de irradiações em diferentes campos e sempre utilizando simulações com o MCNP para fornecer a discriminalização das componentes de dose depositadas em cada TLD. Foram realizadas varias irradiações em campo de gama puro e em campo misto de nêutrons e gamas para o estudo da reprodutibilidade destes TLDs. Este estudo mostrou que mesmo TLDs do mesmo tipo têm sensibilidades distintas, e assim foi criado um Fator de Normalização para cada um dos TLDs, eliminando assim a necessidade de selecionamento. Foi realizado um estudo sobre a diferença das respostas destes TLDs devido à diferentes campos. Este estudo mostrou ser possível estimar o fluxo relativo entre gamas e nêutrons a partir da relação existente entre as duas regiões de interesse dos TLDs 600 e 700. Também foi possível observar que o TLD 700 apresenta resposta para nêutrons, e se a recomendação da ICRU for seguida, a resposta devido à radiação gama será superestimada. Foram obtidas as curvas de calibração dose resposta destes TLDs para campos de gamas puro e campos mistos. Este trabalho propõe o uso desta metodologia com o uso do par TLD 600 e TLD 700, por apresentar maior precisão de resposta frente a atual metodologia que utiliza o TLD 400, porém precauções devem ser tomadas para evitar que a dose gama seja superestimada. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Le travail de thèse propose d’éclaircir les dynamiques qui régissent les réactions d’hydrogénation du dioxyde d’azote (NO2) se déroulant à la surface de catalyseurs modèles de platine, de rhodium et de leur alliage Pt-Rh. Une meilleure compréhension de la réaction catalytique en conditions réactionnelles permettrait, à terme, un meilleur contrôle de la réaction. De manière similaire, le comportement du catalyseur permettrait d’orienter la synthèse de catalyseurs afin d’en augmenter la sélectivité et/ou activité. La structure de ces catalyseurs ainsi que l’analyse des processus sont effectuées à l’échelle nanométrique grâce à l’utilisation de microscopies à effet de champ :la microscopie ionique à effet de champ (FIM) et la microscopie d’émission d’électrons par effet de champ (FEM). La réaction NO2+H2 étudiée à 390 K sur le platine permet de mettre en évidence la présence de différents domaines réactionnels :dynamique monostable, oscillations périodiques auto-entretenues, oscillations périodiques bimodales, ainsi que des oscillations bruitées. Malgré la présence importante de fluctuations à l’échelle du nanomètre, les traitements de signaux mettent en évidence une importante robustesse qui se traduit par un temps de corrélation qui s’étend sur plusieurs centaines de périodes. Les données donnent matière à la reconstruction de l’attracteur dynamique consistant en un cycle limite. La pression d’hydrogène est le paramètre de contrôle qui est varié de sorte à provoquer l’apparition d’oscillations selon une bifurcation de type homocline dans ce cas-ci. Des mesures à haute-vitesse d’acquisition démontrent que l’ignition des différentes faces réactives s’effectue de manière désynchronisée, et la vitesse de propagation est de l’ordre de ~2 μm/s. Au sein d’une seule face, à l’échelle du nanomètre, des propagations de fronts d’ondes chimiques peuvent également être observées à une vitesse de ~2 μm/s, en accord avec les vitesses analysées lors d’expériences menées à l’échelle du micromètre et du millimètre. Sur base des observations, un mécanisme réactionnel de production d’H2O a été proposé. La réaction sur le rhodium à 450 K engendre également des oscillations périodiques qui diffèrent par une robustesse plus faible et par l’apparition d’un cycle limite selon une bifurcation de Hopf. Des mesures exploratoires à 500 K font ressortir la présence de chaos dans le système. Finalement, l’alliage Pt-Rh utilisé comme catalyseur permet d’obtenir des oscillations à 425 K de période comprise entre celles observées sur les deux métaux purs. L’ensemble des expériences et des résultats obtenus à l’échelle du nanomètre permet pour la première fois de valider la théorie des systèmes dynamiques à une telle échelle. / Doctorat en Sciences / info:eu-repo/semantics/nonPublished

Zinc oxide (ZnO) is perhaps one of the most widely studied material in the last two decades. It has received so much of attention because of its incredible potential for wide ranging applications. ZnO is a wide band gap semiconductor (Eg = 3.37 eV at 300 K) with a rather large excitonic binding energy (~60 meV). This combination of properties makes it an ideal choice for several optoelectronic devices that can easily work at room temperature. ZnO is a truly multifunctional material possessing several desirable electrical, optical, optoelectronic, and piezoelectric properties. In addition, it is highly amenable to production of various kinds of nanostructures such as nanorods, nanotubes, nanoribbons, nanoneedles, etc., which makes it even more desirable for nanoscale devices. Examples of ZnO based nanodevices could include photodiodes, photodetectors, nano-lasers, field-emission devices and memristors. In order to make such devices, one could need device quality nanostructures that must be reproducible and cost effective. Naturally, one has to look for a synthesis process that has great controls and is relatively inexpensive. The study provided here shows that among the various methods available for ZnO synthesis, the microwave-assisted chemical synthesis offers outstanding advantages in terms of rapid growth of nanostructures, economical use of energy and excellent controls of process parameters. In order to produce device quality ZnO nanostructures using microwave-assisted synthesis, one has to study the effect of various process parameters and optimise them for the desired growth. Therefore, in the current study, first, a systematic study was undertaken to synthesize ZnO nanostructures both in a aqueous and non-aqueous medium and their characterization was carried out in order to understand the effect of microwave power, time of irradiation, pressure, solvent and salt concentration, etc. The goal was to develop synthesis protocols for various kinds of nanostructures that could guarantee reproducibility, good yield, and device quality structures. This study has led to successful growth of ZnO nanostructures on various substrates, vertically aligned ZnO nanorods and templated arrays of desired structures, all with outstanding properties of the structures as confirmed by XRD, MicroRaman, photoluminescence, cathodoluminescence, FESEM, TEM, PFM studies and pole figure analysis. Piezoelectric force microscopy (PFM) and physical property measurement system (PPMS, Quantum Design), have been used to study the multifunctional properties of ZnO nanostructures. The PFM is a powerful technique to measure the local piezoelectric coefficient of nanostructures and nanoscale thin films. PFM works on the converse piezoelectric effect in which electric potential is applied and mechanical strain is measured using a cantilever deflection. The PFM (Brucker’s AFM dimension Scan Assist) was used to characterize individual ZnO nanorods. Extensive studies were carried out with PFM measurements and it was observed that the nanorods consistently showed high piezoelectric coupling coefficients (d33~50-154 pm/V). It was also found that the variation in d33 depended on morphology and size of nanostructure. The multifunctional properties were observed in small ZnO nanocrystals (NCs). Such high values of piezoelectric coupling coefficients open the door for novel ZnO based nanoscale sensors and actuators. The synthesized ZnO nanostructures were further optimized and characterized keeping in view three device applications namely Field emission, Memristors and Gas Sensors. The fabrication and characterization of these three devices with ZnO nanostructure was carried out using electron beam lithography and direct laser writing micromachining. Device fabrication using lithography involved several steps such as substrate cleaning, photoresist spin coating, pre-baking, post-baking, pattern writing, developing, sputtering/deposition of material for lift-off, ZnO growth, and overlay lithography. For field emission devices, high quality, well aligned, c-axis oriented ZnO nano-needles were grown on sputter coated Ti/Pt (20nm/100nm) on SiO2/Si substrate by rapid microwave-assisted method in aqueous medium. The diameter of the tip was found to be 1~2 nm and the length of the rod was approximately 3~5μm. For a particular batch the tip size, morphology, and lengths were found to be the same and highly repeatable. Pole figure analysis revealed that nanorods were highly oriented towards <002> direction. Field-emission measurements using the ZnO nanoneedles arrays as cathode showed very low turn-on electric field of 0.9 V/μm and a very high field enhancement factor ~ 20200. Such a high emission current density, low turn-on electric field, and high field enhancement factor are attributed to the high aspect ratio, narrow tip size, high quality and single crystallinity of the nanoneedles. The high emission current density, high stability, low threshold electric field (0.95 V/μm) and low turn-on field make the ZnO nanoneedle arrays one of the ideal candidates for field-emission displays and field emission sensors. In the suitability of ZnO nanostructures for memristor application it was found that the single crystalline ZnO nanorods were not suitable as they did not show memristive behaviour but the ZnO nanorods with native defects exhibited considerable memristive behaviour. Therefore the microwave-assisted grown ZnO nanorods with defects were used to fabricate memristive devices. Single and multiple ZnO nanorods based memristors were fabricated using electron beam lithography. These devices were characterized electrically by measuring the hysteresis in the I/V characteristics. A high degree of repeatability has been established in terms of growth, device fabrication, and measurements. The switching in single nanorod based devices was found to have “ON-to- OFF” resistance ratio of approximately 104 and current switching ratio (ION/IOFF) of 106. Gas sensing based on electrical resistance change depends on absorption and desorption rate of gases on the analyte which is governed by surface properties, morphologies and activation energy. Therefore, various morphologies of nanostructure were grown for gas sensing application. Through experimentation, the emphasis shifted to c-axis oriented ZnO nanostructures on SiO2 substrate for gas sensing. The c-axis orientation of ZnO nanostructures was preferred mainly due to its huge surface area. The measurements showed that the c-axis oriented ZnO nanorods were excellent hydrogen sensors, able to detect H2 as low concentration as 2 ppm, even when the sensing temperature is as low as 200 ˚C. However, oxygen sensing was achieved at a higher temperature (300 ˚C). Thus, the study undertaken in this thesis presents a microwave based rapid and economical method for synthesizing high quality, device grade ZnO nanostructures, their extensive characterization that shows the multifunctional properties of these structures, and there examples of varied device applications of the synthesized nanostructures as field emitters, memristors, and gas sensors.