Este estudo se propõe a analisar a resposta pulpar de dentes humanos a preparos cavitários de classe V, em função de duas diferentes técnicas de instrumentação e de duas diferentes técnicas de restauração. Para tal, cavidades classe V, nas superfícies vestibulares de 48 pré-molares hígidos de pacientes entre 11 e 25 anos, que estavam em tratamento ortodôntico, foram preparadas e restauradas de acordo com os seguintes grupos experimentais: G 1 (n=24) - preparos cavitários realizados com ponta diamantada em alta rotação, restaurados com guta-percha plastificada, cimento ionômero de vidro e verniz cavitário (G 1A; n=12) ou com técnicas adesivas (sistema restaurador adesivo aplicando-se o condicionamento ácido total) e cimento ionômero de vidro (G 1B; n=12); G 2 (n=24) - preparos cavitários com ponta CVD ativada por ultrassom, restaurados com gutapercha plastificada, cimento ionômero de vidro e verniz cavitário (G 2A; n=12) ou com técnicas adesivas (sistema restaurador adesivo aplicando-se o condicionamento ácido total) e cimento ionômero de vidro (G 2B; n=12); e G 3 (controle; n=4) - dentes que foram extraídos sem a realização de qualquer procedimento. Os preparos cavitários foram realizados mantendo o assoalho da cavidade o mais próximo possível da polpa, no entanto, sem provocar exposição pulpar. Os dentes foram extraídos após três períodos experimentais (imediato, sete e trinta dias após o preparo cavitário), fixados, descalcificados, e processados histologicamente. Cortes teciduais longitudinais seriados de 5 m foram obtidos, corados pelas técnicas de H & E e de Brown & Brenn, e examinados em microscopia ótica. As avaliações morfométricas e por escores foram realizadas e os resultados das mesmas, submetidos, respectivamente, aos testes estatísticos de Mann-Whitney e de Kruskal-Wallis/Dunn, adotando-se um nível de significância de 5%. No período inicial, todos os grupos experimentais (1A, 1B, 2A e 2B) exibiram ligeiro desarranjo da camada odontoblástica vacuolizada e leve invasão da zona acelular de Weil. Não houve diferença entre os grupos experimentais iniciais e o grupo controle. No intervalo de sete dias, pôde-se observar redução da camada odontoblástica, muitos núcleos de odontoblastos aspirados nos túbulos dentinários, alguns espécimes com ausência de pré-dentina e resposta inflamatória aguda com hemorragia. Trinta dias depois, cinco espécimes do total avaliado apresentaram dentina terciária; dois espécimes do grupo 1B apresentaram necrose relacionada com a presença de bactérias nos túbulos dentinários; e os demais mostraram graus variados de inflamação crônica, associados a restaurações adesivas ou a processos de reparo, com proliferação de vasos e persistência de focos de hemorragia. Portanto, os dois tipos de instrumentação cavitária promovem respostas pulpares similares entre si, mas as diferentes técnicas restauradoras promovem efeitos significativamente diferentes sobre o complexo dentinopulpar. / The aim of this study is to analyze the pulp response of human teeth to class V cavity preparation, in function of two different instrumentation and restorative techniques. Class V cavities were made on the buccal surfaces of 48 sound human pre-molars from orthodontic patients from 11 to 25 years, and were divided as follows: G1 (n=24) cavity preparations were made with diamond bur under high speed, restored with either plasticized gutta-percha, glass ionomer cement and surface coated with varnish (G1A) or adhesive protocol (total etch technique and adhesive system application) with glass ionomer filling (G1B); G2 (n=24) cavity preparations were made with diamond CVD point and ultrasonic device, restored with either plasticized gutta-percha, glass ionomer cement and surface coated with varnish (G2A) or adhesive protocol (total etch technique and adhesive system application) with glass ionomer filling (G2B); and control group G3 (n=4) extracted teeth with no previous cavity preparation. All avities were prepared with the cavity floor as close to the pulp as possible, without causing pulp exposure. Teeth extractions were made in three experimental periods (immediate, 7 and 30 days after cavity preparation) and right after extraction they were submitted to histological procedures. Longitudinal tissue serial sections of 5 mm were obtained, H&E and Brown&Brenn stained, and analyzed under optical microscope. Morphometric and score evaluations were carried out and data from both were, respectively, submitted to Mann-Whitney and Kruskal-Wallis/Dunn tests, with 5% significance. Immediately, all experimental groups (1A, 1B, 2A and 2B) exhibited a discrete disorganization of the odontoblastic layer and invasion of the Weil zone. There was no difference between experimental and control groups. At 7-day interval, a decrease of the odontoblastic layer was observed. Many odontoblasts nucleus were seen displaced into the dentinal tubules. Some specimens showed absence of pre-dentine and inflammatory pulp response with hemorrhage. Thirty days later, five specimens presented tertiary dentin formation; two specimens from group 1B presented necrosis coincident with bacteria inside the dentinal tubules; the other specimens showed various degrees of chronic inflammation, associated to adhesive restorations or repair processes, with blood vessels proliferation and persistent hemorrhagic areas. Therefore, both instrumentation techniques promoted similar pulp response, but different restoration procedures elicited significantly different responses of the dentinpulp complex.

Le travail présenté dans ce manuscrit de thèse s’inscrit dans le cadre d’une coopération scientifique notamment à travers le projet Région Centre « Connectic » en partenariat avec la société STMicroelectronics de Tours, les laboratoires LMR et CEMHTI. Il concerne les interconnexions des générations futures de circuits intégrés. Par rapport aux technologies d’interconnexion à base d’alliage métallique l’intégration de nanotubes de carbone (NTC) comme connecteur en microélectronique de puissance limiterait les effets d’échauffement dans les empilements de puces grâce à leurs propriétés de transport intéressantes. Les NTC peuvent assurer simultanément une bonne conduction électrique et un maintien mécanique des assemblages de puces. Les objectifs de ce travail étaient d’établir dans un premier temps un procédé reproductible d’élaboration de NTC verticalement alignés sur des substrats de nature multiple, et de réaliser dans un deuxième temps un véhicule test qui permet de caractériser leurs propriétés électrique, thermique et mécanique. Le dispositif expérimental d’élaboration présenté dans cette étude utilise le dépôt de catalyseur (Ni, Fe), la structuration par plasma d’hydrogène simultanément à un recuit thermique, ainsi que la méthode de CVD assistée par plasma radiofréquence d’éthylène et d’hydrogène pour la croissance des NTC. Des conditions optimales reproductibles d’obtention des NTC ont été établies à la suite d’une étude paramétrée utilisant notamment un diagnostic original de suivi in situ par spectroscopie Raman développé en collaboration avec le CEMHTI. Dans le cas d’un tapis de NTC de 10 µm de haut, des performances électrique (⍴ = 10⁻⁵ Ω.m), thermique (λth = 40-60 W.m⁻¹.K⁻¹), et mécanique (E = 480 GPa) comparables aux alliages métalliques ont été établies. Enfin, nous avons été capables d’assembler les substrats de la microélectronique et les NTC par un procédé de thermocompression. / The work presented in this thesis was a scientific cooperation between the society ST Microelectronics in Tours, the laboratories of LMR and CEMHTI within the framework of the project Région Centre “ConnectiC”. The main issue of that project concerns the interconnections for the future generation of integrated circuits. In comparison with the current interconnection technologies on metallic alloys as connectors; the integration of carbon nanotubes (CNT) as connector in power microelectronics would limit effects of overheating in the chip-structure due to their interesting transport properties. CNT can provide at the same time good electrical, thermal conduction characteristics and can be a mechanical support of chip packages. The aims of this work were: firstly, obtain a reproducible growth process of vertically aligned CNT on different kinds of substrate; secondly: to elaborate a test vehicle with CNT interconnects allowing the electrical, thermal and mechanical characterization. The experimental method used herein for synthesis of CNT interconnects combines the catalyst deposition (Ni, Fe), the structuration by both means of hydrogen plasma treatment and thermal annealing, and a RF PECVD method using ethylene and hydrogen for the CNT growth. Optimal reproducible conditions were found using a novel in situ Raman spectroscopy diagnostic developed in collaboration with the CEMHTI. The carpet of CNT (height of 10 µm) produced presents the electrical (⍴ = 10⁻⁵ Ω.m), thermal (λth = 40-60 W.m⁻¹.K⁻¹), and mechanical (E = 480 GPa) performances comparable with the metallic. Finally, by means of thermocompression, we assembled CNT on substrates from the microelectronics.

Croissance catalytique et étude de nanotubes de carbone multi-feuillets produits en masse et de nanotubes de carbone ultra-long individuels à quelques feuillets Résumé: Ce travail expérimental traite de la croissance catalytique à partir d'une phase vapeur (CCVD) de nanotubes de carbone multi-feuillets (MWCNT) et de nanotubes de carbone (CNT) ultralongs ainsi que de l'étude de leurs propriétés physiques. Dans la première partie du manuscrit est décrite l'optimisation des paramètres pour la croissance CCVD de MWNT en masse et à faible coût. Avec l'acétylène comme source de carbone, Fe(NO3)3.9H2O comme précurseur de catalyseur et CaCO3 comme support, nous rapportons les conditions optimales pour la production de 525 g de MWCNT par jour à un coût estimé de 0.6$/g. La purification des MWCNT ainsi produits par un traitement à l'oxygène ou au dioxyde de carbone est également présentée. La seconde partie est consacrée à la synthèse de CNT ultralongs. L'influence des paramètres de synthèse est étudiée et, à partir de ces observations, les mécanismes de croissance possibles sont discutés. La dernière partie de la thèse est dédiée à la fabrication et à l'étude des propriétés physiques de nanotubes individuels ultralongs. Sur la base du savoir-faire développé précédemment, nous avons réalisé des CNT ultralongs alignés, des jonctions de CNT (suspendus ou supportés) ainsi que des CNT suspendus au-dessus de différents supports. Les propriétés électroniques et de transport des CNT individuels ultralongs sur substrat de silicium ont été étudiées par microscopie à force atomique, spectroscopie Raman et mesures de transport. Enfin, les modes de phonons actifs en Raman sont étudiés par des expériences combinant microscopie électronique à transmission, diffraction électronique et spectroscopie Raman.Mots clés: Nanotubes de carbone multi-feuillets, nanotubes de carbone ultralongs, croissance catalytique à partir d'une phase vapeur, mécanisme de croissance, lithographie, spectroscopie Raman de résonance, transport électronique. / Catalytic growth and study of mass-produced multi-walled carbon nanotubes and ultralong individual few-walled carbon nanotubesAbstract: This experimental work deals with the growth of multi-walled carbon nanotubes (MWCNTs) and ultralong carbon nanotubes (CNTs) by catalytic chemical vapor deposition (CCVD), and the study of their physical properties. In the first part of the manuscript is described the parameter optimization of the CCVD growth of MWCNTs for a large-scale production at low cost. By using acetylene as a carbon source, Fe(NO3)3.9H2O as a precursor catalyst and CaCO3 as a catalyst support, we report on optimized growth conditions allowing the production of 525 g of MWCNTs per day at an estimated cost of 0.6 $ per gramme. The purification of the as-grown MWCNTs by oxygen or carbon dioxide treatments is also presented. In the second part is presented the synthesis of ultralong individual CNTs. The influence of the growth parameters is investigated and based on the experimental observations, the possible growth mechanisms are discussed. Finally, the last part of the thesis is dedicated to the preparation and to the study of the physical properties of ultralong individual carbon nanotubes. From the know-how developed in the previous part, we prepared well-aligned ultralong CNTs, cross junction of CNTs (on a substrate or suspended) and suspended CNTs over different supports. Electronic and electron transport properties of the individual ultralong CNTs on silicon substrate are then studied by atomic force microscopy, Raman spectroscopy and transport measurements. Finally, the Raman-active phonons of suspended individual CNTs were investigated in combined experiments by transmission electron microscopy, electron diffraction and Raman spectroscopy. Keywords: Multi-walled carbon nanotubes, ultralong carbon nanotubes, catalytic chemical vapor deposition, growth mechanism, lithography, resonant Raman spectroscopy, electronic transport.

The master’s thesis deals with the theory of thin film technology, especially creating these layers. The work includes the distribution of vacuum deposition techniques for physical (PVD) and chemical (CVD). The main aim is to create a theme in different ways of implementation by using magnetron sputtering device, and these motives evaluated in terms of the quality of sputtering.

The aim of the thesis is to design, conduct and assess an experiment seeking to look into the utility properties of recent tools manufactured by HAM-FINAL. The tools include polycrystalline diamond (PCD) and CVD diamond cutting edges. In the theoretical part, the attention is devoted to cutting materials with an emphasis on diamond materials, as well as to issues associated with the wearing of the cutting tools, requirements specified for precision of bores and tools used in the manufacture of precision bores. The paper further provides an overview of a selection of world’s leading manufacturers of PCD blanks, CVD diamond coatings, CVD diamond layers and reamers with PCD cutting edges.

Tato diplomová práce se zabývá problematikou PVD povlakování střižných nástrojů ze slinutých karbidů, se zaměřením na zvýšení životnosti postupových nástrojů. Především poukazuje na využití povlakovaných nástrojů v praxi a procesních kroků před a po procesu povlakování. V teoretické části jsou popsány obě základní metody povlakování, tj. fyzikální metoda PVD a metoda CVD, založena na chemickém procesu. Dále jsou představeny jednotlivé způsoby vlastních procesů povlakování se stručným popisem výhod i nevýhod jejich využití. Praktická část je zaměřena na testování, jehož podstatou byl nejen vhodný výběr samotného povlaku pro daný materiál, ale i úpravy před a po povlakování, které jsou často opomínány. Ty jsou však nezbytnou součástí a mají výrazný vliv nejen na výsledný povlak, ale i na kvalitu pracovního procesu. Vyhodnocením experimentu je souhra určení nejproduktivnějšího povlaku v závislosti na dané úpravě.

Machining of Aluminum can be complicated due to large amounts of adhesion and diffusion of the aluminum onto the cutting tool, causing effects such as built-up layers and built-up edges. This leads to poor surface finishes and can significantly affect the tool life. CVD diamond coated tools have shown to be a potential solution to this problem and is tested and analyzed as such in this thesis. CVD diamond coated inserts are tested and compared to uncoated cemented carbide inserts and Polycrystalline diamond tipped inserts, in milling, turning and in refined tribological methods. The workpiece material in both the machine tests and the tribological tests is a high strength aluminum of the name Alumec 89. The machine tests were performed for 5 and 60 seconds at three cutting speeds, 600, 900 and 1200 m/min, keeping other parameters constant. The cutting inserts, the chips and the generated workpiece surface are examined using LOM, SEM and EDS. In the refined tribological testing, a pin-turning tribometer is used, with pins of uncoated and coated (CVD diamond) cemented carbide pins. These are tested at 5 and 30 seconds at 600 and 1200 m/min, applying a constant force of 10 N. In addition, a friction test was performed to measure the friction of the uncoated and the CVD diamond coated cemented carbide. Like the cutting inserts, the used pins were examined in LOM and SEM. The results show that while a large amount of built-up layer and built-up edges gather when using uncoated cemented carbide tools, only minimal amounts can be detected on CVD diamond and PCD. It has also been shown that the reason for the reduced adhesion in the case of diamond tooling materials is most likely due to the lack of chemical interactions between the diamond and the aluminum. The friction of the CVD diamond material was shown to be lower compared to the cemented carbide. The surface finish generated by the different materials, was the best in the case of PCD while the CVD generated multiple small scratches that severely reduced the surface roughness. This thesis provides some initial basic understanding of the interaction of CVD diamond coated inserts with high strength aluminum alloys.

The thesis describes the construction of a CVD system, the deposition of thin molybdenum disulphide layers using this system and the analysis of the samples produced. The deposition of thin molybdenum disulphide layers and an intercalation of the silicon carbide substrate used were demonstrated and the measurement results obtained by atomic force microscopy, Raman spectroscopy and photoelectron spectroscopy were further discussed.:1. Introduction: Two-Dimensional Materials 2. Experimental Methods 2.1. Atomic Force Microscopy 2.2. Photoelectron Spectroscopy 2.2.1. Layer Thickness Determination 2.2.2. Quantitative Surface Analysis 3. Structure, Properties and Synthesis of the Used Materials 3.1. Transition Metal Dichalcogenides 3.1.1. Molybdenum Disulfide 3.1.2. Synthesis of Thin MoS Films-State of the Art 3.2. Substrate-Graphene on SiC 3.2.1. Graphene 3.2.2. Epitaxial Graphene on Silicon Carbide 4. Development of a CVD System for the Growth of MoS2 films 4.1. Basic Principles of Chemical Vapor Deposition 4.2. Construction of the CVD System 4.3. Temperature Measurements 4.4. Preliminary Considerations for the CVD Process 5. Growth Characteristics 5.1. Chemical Composition of the Substrate 5.2. Chemical Composition of the Grown MoS Films 5.3. Layer Thickness of the Grown MoS Films 5.3.1. Determination with XPS 5.3.2. Determination with Raman 5.4. AFM Measurements 6. Conclusion

Heteroepitaxial SiGe(C) layers have attracted immense attention as a material for performance boost in state of the art electronic devices during recent years. Alloying silicon with germanium and carbon add exclusive opportunities for strain and bandgap engineering. This work presents details of epitaxial growth using chemical vapor deposition (CVD), material characterization and integration of SiGeC layers in MOS devices. Non-selective and selective epitaxial growth of Si1-x-yGexCy (0≤x≤0.30, 0≤y≤0.02) layers have been performed and optimized aimed for various metal oxide semiconductor field effect transistor (MOSFET) applications. A comprehensive experimental study was performed to investigate the growth of SiGeC layers. The incorporation of C into the SiGe matrix was shown to be strongly sensitive to the growth parameters. As a consequence, a much smaller epitaxial process window compared to SiGe epitaxy was obtained. Incorporation of high boron concentrations (up to 1×1021 atoms/cm3) in SiGe layers aimed for recessed and/or elevated source/drain (S/D) junctions in pMOSFETs was also studied. HCl was used as Si etchant in the CVD reactor to create the recesses which was followed (in a single run) by selective epitaxy of B-doped SiGe. The issue of pattern dependency behavior of selective epitaxial growth was studied in detail. It was shown that a complete removal of pattern dependency in selective SiGe growth using reduced pressure CVD is not likely. However, it was shown that the pattern dependency can be predicted since it is highly dependent on the local Si coverage of the substrate. The pattern dependency was most sensitive for Si coverage in the range 1-10%. In this range drastic changes in growth rate and composition was observed. The pattern dependency was explained by gas depletion inside the low velocity boundary layer. Ni silicide is commonly used to reduce access resistance in S/D and gate areas of MOSFET devices. Therefore, the effect of carbon and germanium on the formation of NiSiGe(C) was studied. An improved thermal stability of Ni silicide was obtained when C is present in the SiGe layer. Integration of SiGe(C) layers in various MOSFET devices was performed. In order to perform a relevant device research the dimensions of the investigated devices have to be in-line with the current technology nodes. A robust spacer gate technology was developed which enabled stable processing of transistors with gate lengths down to 45 nm. SiGe(C) channels in ultra thin body (UTB) silicon on insulator (SOI) MOSFETs, with excellent performance down to 100 nm gate length was demonstrated. The integration of C in the channel of a MOSFET is interesting for future generations of ultra scaled devices where issues such as short channel effects (SCE), temperature budget, dopant diffusion and mobility will be extremely critical. A clear performance enhancement was obtained for both SiGe and SiGeC channels, which point out the potential of SiGe or SiGeC materials for UTB SOI devices. Biaxially strained-Si (sSi) on SiGe virtual substrates (VS) as mobility boosters in nMOSFETs with gate length down to 80 nm was demonstrated. This concept was thoroughly investigated in terms of performance and leakage of the devices. In-situ doping of the relaxed SiGe was shown to be superior over implantation to suppress the junction leakage. A high channel doping could effectively suppress the source to drain leakage. / <p>QC 20100715</p>

This thesis is devoted to the development of nano-focusing refractive optics for high energy X-rays using planar microelectronic technology. The availability of such optics is the key for the exploitation of high brilliance third and fourth generation X-ray sources. Advancements in the quality of optics available are commensurate with advancements in the fabrication technology. The fabrication process directly influences the quality and performance, so must be understood and controlled. In the first part of this thesis, the development of high aspect ratio Si kinoform lenses is examined. It is shown that control of the re-entrance angle is critical for successful fabrication; in fact, a large re-entrance angle can destroy the lens during the fabrication process. Through an etch study, it was found that as aspect ratio increases, control of the re-entrance angle becomes harder. To control the re-entrance angle for very high aspect ratios, a novel approach based on sacrificial structures was proposed and initial results presented. The second part is dedicated to an experimental study of refractive lenses made from diamond. Due to its low atomic number, relatively high density and very high thermal conductivity, diamond is one of the most desirable lens materials for refractive X-ray optics. However, due to its extreme hardness, it is very difficult to structure into a form suitable for X-ray lenses. To overcome this difficulty a Si moulding technique was used and focusing down to a 400 nm wide spot was achieved. Several obstacles were encountered and successfully overcome. The hardest obstacle was to obtain selective void-free filling in the Si moulds. Several methods were investigated. A method based on a sacrificial oxide layer and an Electrostatic Self-Assembly process was found to be the most useful. The approach discovered in this thesis is not limited to X-ray lenses, but can be applied to a wide variety of high aspect ratio MEMS requiring void-free diamond filling and smooth sidewalls.