[pt] O presente trabalho tem por objetivo implantar um método para calibração de sistema de medição linear por interferometria laser por meio de comparação a um outro sistema laser de referência. O referido método é considerado mais simples que a calibração por componentes realizada atualmente e, conforme demonstrado no trabalho, apresenta confiabilidade metrológica que atende a exatidão necessária para as aplicações dos laseres em metrologia dimensional, vindo suprir uma necessidade metrológica dos laboratórios credenciados pelo Instituto Nacional de Metrologia, Normalização e Qualidade Industrial (Inmetro) e do parque industrial brasileiro, usuários destes sistemas de medição. A implantação do sistema para calibração de lasers de medição foi baseada em normas internacionais de calibração e de cálculo da incerteza de medição e utilizou um sistema laser de referência calibrado no Inmetro, com rastreabilidade a padrões nacionais, com as menores incertezas possíveis. O método de medição implantado realiza a calibração de um sistema laser por comparação a outro utilizando medições feitas a partir do deslocamento da mesa onde é a apoiado o prisma óptico. O que é de fato analisado é a diferença das medições dos dois sistemas laser para um mesmo deslocamento. Foram registradas as diferenças das indicações de 200 mm em 200 mm de deslocamento, em um total de 2000 mm, que variaram de 0,027 µm a 0,690 µm. Foram realizadas três medições para cada deslocamento e quatro repetições completas do procedimento em dias diferentes, com variação do desvio padrão de 0,009 µm a 0,098 µm e incertezas expandidas que variaram de 0,109 µm a 0,306 µm. São apresentadas a metodologia de calibração, cálculos das correções, fontes de erros e cálculos da incerteza de medição para a comparação de sistemas laseres de medição linear. / [en] The present work aims at the implementation of a calibration method for interferometric linear laser measurement systems by comparison to another reference system. The proposed method is considered simpler than the calibration by components that is carried out today at Inmetro (National Institute of Metrology, Standardization and Industrial Quality) and, as demonstrated along this work, presents the metrological reliability and accuracy necessary for several applications of lasers in dimensional metrology. This approach will supply the metrological needs of several laboratories accredited by Inmetro and of the Brazilian industry in general, users of such measurement systems, regarding cost and time of calibration. The method implemented was based on international technical standards related to calibration and uncertainty calculation and used a reference system calibrated at Inmetro, with traceability to national standards, with the lowest uncertainties that could be achieved. The said method performs the calibration of a laser system by comparison to another through measurements of the displacement of the table where the optical prism rests. What is indeed analyzed is the difference of the measurements obtained by the two laser systems for the same table displacement. The differences were recorded for each displacement of 200 mm, in a total of 2,000 mm, their variation being from 0.027 µm to 0.690 µm. The whole procedure was repeated four times, in different days, with three measurements for each displacement. Their standard deviation varied from 0.009 µm to 0.098 µm while their expanded uncertainties varied from 0.109 µm to 0.306 µm depending on the value of the displacement. The calibration methodology, correction calculation, errors sources and measurement uncertainty calculations for the linear measurement laser systems comparison are presented in this dissertation.

Made available in DSpace on 2016-04-26T20:19:54Z (GMT). No. of bitstreams: 1 Paulo Sergio Feuz.pdf: 806476 bytes, checksum: 7827f776a5a095ac43a83d9587bb7d3a (MD5) Previous issue date: 2010-11-29 / Upon the enactment of the 1988 Federal Constitution, a new stage takes place in Brazil: the democratic rule-of-law state. The grounds of this new politics formula are sovereignty citizenship, the dignity of the human person, and the social values of labor and of free enterprise system, as we]1 as political pluralism. In this context, it defined the protection of the consumers, settled in 1990 with the enactment of Law 8,078/90. The main concern of such legislation, which is presented in its National Policy for Consumption Relations, is to serve the consumers, by respecting their dignity, security and health, by protecting their economic interests and aiming at improving their life quality, thus implementing a National System for Consumer Defense. For this reason, and taking into account the concept of system for Law, the identification of subsystems which are able to meet the grounds of the democratic rule-of-law state, as well as the interests of the National Policy for Consumption Relations are indispensable. To that end, we take metrology as the central point, by analyzing all of the Law subsystem which are linked to it, and finally we discuss the complexity and the regeneration of Law as a whole / Com a chegada da carta Constitucional de 1988, inaugura-se uma nova fase no Brasil: o Estado Democrático de Direito. Essa nova fórmula política determina como fundamentos para sua estrutura a soberania, a cidadania, a dignidade da pessoa humana, os valores sociais do trabalho e da livre iniciativa e o pluralismo político. Nesse contexto, determinou a tutela dos consumidores consagrada em 1990 com a chegada da Lei 8.078/90. Referida legislação tem como preocupação central, exposta em sua Política Nacional das Relações de Consumo atender o consumidor, respeitando sua dignidade, segurança e saúde, protegendo seus interesses econômicos e visando a melhoria de vida, instituindo para isso, um Sistema Nacional de Defesa do Consumidor. Dessa forma, e tomando em conta o conceito de sistema para o direito, é imprescindível a identificação de subsistemas que possam atender os fundamentos do estado Democrático de Direito bem como os reclamos da Política Nacional das Relações de Consumo. Para isso, usamos como ponto central a metrologia analisando todos os subsistemas de direito a ele vinculados, para por fim discorrer sobre a complexidade e autopoiesi do direito como um todo

L’origine et l’évolution des différentes structures qui peuplent l’au-delà de la photosphère du Soleil, ainsi que les processus qui interviennent dans la dynamique et le chauffage de sa couronne demeurent de nos jours assez peu compris. L’inextricable complexité inhérente aux phénomènes physiques qui gouvernent l’atmosphère externe solaire s’accompagne de l’absence de données adaptées au besoin scientifique. En effet, l’interprétation et la modélisation des « mécanismes » qui raccordent les échanges entre la chromosphère et la couronne dépendent de paramètres d’observation critiques. Il est par exemple essentiel de pouvoir mesurer de larges bandes de températures et densités verticales s’adaptant aux multiples échelles spatiales et temporelles caractéristiques des différents évènements qui se déroulent dans le Soleil. La compréhension de la dynamique des plasmas repose aussi sur l’analyse Doppler de la scène observée. Ceci implique notamment la capacité de combiner des techniques de spectroscopie et d’imagerie simultanément dans le temps. Pour la couronne, le passage à l’UV spatial est incontournable, et relève d’un véritable défi technique. Malgré les excellents progrès technologiques, l’étude UV du Soleil est une science relativement récente, et aucune mission spatiale solaire n’a pu fournir jusqu’à présent une spectro-imagerie combinée et simultanée dans le domaine spectral qui nous intéresse. C’est pour répondre à cette attente que l’étude d’un nouveau dispositif appelé IFTSUV (abréviation de Imaging Fourier Transform Spectrometer working in the far UV), est présentée dans cette recherche. Malgré l’absence de missions d’opportunité dans l’horizon proche, les travaux de thèse se sont déroulés suivant le plan de l’action R&T du CNES R-S11/OT-0004-040, concernant la définition d’un spectro-imageur à transformée de Fourier dans l’UV lointain, et la réalisation en laboratoire d’un démonstrateur de métrologie dédié, pierre angulaire de la faisabilité technique de l’instrument. Ainsi, partant de la détermination du besoin scientifique et de la justification du choix technique, le premier objectif de cette étude est de concevoir un modèle instrumental préliminaire complet de l’IFTSUV. La spécification technique est fondée sur le calcul de dimensionnement et l’évaluation théorique des spécifications en termes de précision spectrale, qualité de l’image et rapport signal sur bruit. A travers l’identification des points durs, la réalisation d’une métrologie d’asservissement du miroir d’échantillonnage apparait tout naturellement, comme un besoin intrinsèque de la validation du concept. En effet, l’acquisition de l’interférogramme doit se faire de manière rigoureusement constante et le pas d’échantillonnage doit être connu avec une grande exactitude, car il fixe les nombres d’onde pour lesquels les spectres bruts sont calculés. Le maquettage d’une solution métrologique constitue donc le deuxième objectif de ce travail. L’architecture optique mise en place a été choisie afin de satisfaire les besoins de stabilité angulaire (< 2.5 μrad) et de précision linéaire (< 8 nm) discernés, et testée en laboratoire. Les résultats sur la maquette valident le concept, même si ses performances s’éloignent des prédictions théoriques. L’évaluation expérimentale des performances permet d’établir des solutions aux problèmes rencontrés qui convergent vers l’optimisation et le prototypage d’un système pouvant être intégré dans une application spatiale. / The origin and evolution of the different structures that inhabit beyond the Sun’s photosphere, as well as the processes involved in the dynamics and the heating of the corona remain quite unknown. The inextricable complexity of the physical phenomena that govern the solar outer atmosphere is accompanied by the lack of suitable data adapted to the scientific need. Indeed, the interpretation and the models of the mechanisms that connect the exchanges between the chromosphere and the corona depend on critical observational parameters. It is for example essential to measure broad bands of vertical temperature and density ranges that fit the multiple spatial and temporal scales that are characteristic of the different events that take place in the Sun. The understanding of the dynamics of the plasma must be also based on the Doppler analysis of the observed scene. That implies the ability to combine time resolved spectroscopic and imaging technologies. Moreover, space is the place to observe the far UV corona and that implies a real technical challenge. Despite excellent advances in technology and instrumentation, the study of the Sun in the far UV is a fairly recent. To date, no solar space mission could provide a combined and simultaneous diagnostic of both observable in the spectral range of interest. It is because of these expectations that the study of a new device called IFTSUV (the acronym of Imaging Fourier Transform Spectrometer working in the far UV) is presented in this research. Despite the lack of opportunity missions on the near horizon, these thesis works have been conducted thanks to the R&D funding R-S11/OT-0004-040 from the CNES, concerning either the definition of an imaging Fourier transform spectrometer in the far UV, or the realization of a laboratory metrology demonstrator that is the cornerstone of the instrument’s feasibility. Thus, starting from the definition of the scientific requirements that lead to the technical choice, the first objective of this study is to develop a preliminary instrumental model of the IFTSUV. The overall technical and design specifications are based in theoreticalcalculations that have been expressed in terms of spectral accuracy, image quality and signal to noise ratio. Throughout the identification of difficult points, the realization of a servo-metrology system dedicated to the sampling mirror appears naturally as an intrinsic need of proof of concept. Indeed, the wavenumbers from the raw spectra are set by the interferogram. That implies that acquisition must be rigorously constant and that the sampling steps must be known with high accuracy. The mockup of a metrological solution is therefore the second objective of this work. The optical breadboard architecture under test has been chosen to meet the needs of angular stability (< 2.5 μrad) and linear accuracy (< 8 nm). The results on the demonstrator validate the concept even if its performances are away from the theoretical predictions. The experimental performance evaluation is used to establish solutions to the instrumental problems encountered. That converge to the optimization and prototyping of a system that could be integrated in a space based application.

Esta dissertação descreve os recentes desenvolvimentos do Chafariz Atômico localizado no Instituto de Física de São Carlos. Ele consiste de um aparato experimental que provê uma referência de freqüência (e tempo) de altíssima precisão. Para conseguir tal qualidade metrológica, esse sistema trava a freqüência de um oscilador eletrônico, baseado em um cristal de quartzo, na freqüência relativa a uma transição atômica, de uma amostra de átomos resfriados. O átomo utilizado é o 133Cs e a transição utilizada corresponde aos dois níveis hiperfínos do seu estado fundamental. O ciclo de funcionamento é composto por uma etapa de aprisionamento a laser dos átomos e bombeamento óptico, para que todos os átomos se encontrem num mesmo e determinado nível de energia. Esses átomos são então lançados opticamente contra a gravidade através de uma cavidade de microondas. Em trajetória balística e livre de interferências externas, o conjunto de átomos sofre uma possível mudança de estado, dependendo das características de potência e freqüência do sinal de microondas injetado na cavidade. Esta probabilidade de transição é o sinal de erro utilizado para travar em malha fechada o gerador de microondas que alimenta a cavidade. Os melhores resultados obtidos neste experimento foram uma estabilidade de 5x10-12&tau;-1/2 resultante de um sinal com 3Hz de largura a meia altura (FWHM) da franja central. Fizemos também uma avaliação preliminar dos principais deslocamentos de freqüência e uma análise de interação espacial dos átomos com o campo de microondas. / This paper describes the recent developments of the Atomic Fountain located at the São Carlos Physics Institute. It provides a very high resolution frequency (and time) reference. This is achieved locking an electronic oscillator, based on a quartz crystal, to an atomic resonance of a cold atomic sample. Our laboratory uses the 133Cs atom, using as the referenced transition that corresponds to the two hyperfine energy levels of the ground state. The operating cycle comprises a stage of laser trapping atoms or optical pumping, so that all atoms are within the same atomic state. These atoms are then launched optically against gravity through a microwave cavity. In ballistic trajectory and free from external interference, the set of atoms undergoes a change of state, depending on the power and frequency of the microwave signal injected into the cavity. This transition probability is the error signal used to lock the microwave generator supplying the cavity in a closed loop. The best result obtained in this experiment was a stability of 5x10-12&tau;-1/2 resulting from signal with a 3 Hz half width (FWHM) of the central fringe. We also provide a preliminary assessment of the main frequency shifts and an analysis of spatial interaction of atoms with the microwave field.

Os ensaios de proficiência têm sido utilizados, por laboratórios de ensaio e calibração acreditados sob a norma ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories), como principal mecanismo para garantia da qualidade de seus resultados. Além de atender a um requisito normativo, a participação satisfatória neste tipo de atividade é utilizada, por organismos acreditadores, como condição à obtenção e manutenção da acreditação. Entretanto, existe uma carência por provedores de ensaios de proficiência acreditados de acordo com a norma ISO/IEC 17043 (Conformity assessment — General requirements for proficiency testing), o que causa dificuldades aos laboratórios. Esta dissertação teve como objetivo analisar a viabilidade de que laboratórios acreditados à ISO/IEC 17025 atuem, simultaneamente, como provedores de ensaios de proficiência, acreditados à ISO/IEC 17043. Para isso, foram estabelecidas as relações entre os itens das normas, identificadas e analisadas as exigências adicionais e adaptações necessárias no sistema de gestão, identificados os potenciais conflitos de interesses e estabelecidas propostas de atendimento para cada item normativo afetado. Os artigos que constituem esta pesquisa foram validados por um grupo de especialistas na área da metrologia, sendo as suas opiniões consideradas nos estudos realizados. Conclui-se, ao final, que a atuação simultânea proposta é viável, exigindo adaptações no sistema de gestão e procedimentos complementares referentes à confidencialidade e à imparcialidade. Como resultado prático, espera-se minimizar a carência por este serviço, sem comprometer sua confiabilidade. / Proficiency tests have been used by testing and calibration laboratories accredited to the ISO/IEC 17025 standard (General requirements for the competence of testing and calibration laboratories) as the main mechanism for assuring the quality of their results. Besides attending to a normative requirement, the satisfactory participation in this kind of activity is used by accreditation bodies as a condition to obtaining and maintaining the accreditation. However, there is a lack of proficiency testing providers accredited according to the ISO/IEC 17043 standard (Conformity assessment — General requirements for proficiency testing), which causes laboratories to have difficulties. This thesis had as its goal to analyze the viability of laboratories accredited to the ISO/IEC 17025 acting simultaneously as proficiency testing providers, accredited to the ISO/IEC 17043. For that, relations between the items of both standards have been established, additional requirements and necessary adaptations in the management system have been identified and analyzed, potential conflicts of interest have been identified and solutions have been proposed for each normative item. A group of experts in the field of metrology validated the articles that constitute this research and their opinions have been considered in the studies. At the end, the conclusion was that the proposed simultaneous acting is viable, requiring adaptations in the management system and complementary procedures referring to confidentiality and impartiality. As a practical result, it is hoped to minimize the shortage for this kind of service, without compromising its reliability.

La thématique abordée porte sur la métrologie virtuelle (VM) pour estimer les données manquantes durant les processus de fabrications des semi-conducteurs. L'utilisation de la métrologie virtuelle permet également de fournir les mesures logicielles (estimations) des sorties pour alimenter les régulateurs run-to-run (R2R) mis en place pour le contrôle de la qualité des produits fabriqués. Pour remédier aux problèmes liés au retard de mesures causé par l'échantillonnage statique imposé par la stratégie et les équipements mis en place, notre contribution dans cette thèse est d'introduire la notion de l'échantillonnage dynamique intelligent. Cette stratégie est basée sur un algorithme qui prend en compte la condition de voisinage permettant d'éviter la mesure réelle même si l'échantillonnage statique l'exige. Cela permet de réduire le nombre de mesures réelles, le temps du cycle et le coût de production. Cette approche est assurée par un module de métrologie virtuelle (VM) que nous avons développé et qui peut être intégré dans une boucle de régulation R2R. Les résultats obtenus ont été validés sur des exemples académiques et sur des données réelles fournies par notre partenaire STMicroelectronics de Rousset concernant un processus chemical mechanical planarization (CMP). Ces données réelles ont permis également de valider les résultats obtenus de la métrologie virtuelle pour les fournir ensuite aux régulateurs R2R (ayant besoin de l'estimation de ces données). / The addressed work is about the virtual metrology (VM) for estimating missing data during semiconductor manufacturing processes. The use of virtual metrology tool also makes it possible to provide the software measurements (estimations) of the outputs to feed the run-to-run (R2R) controllers set up for the quality control of the manufactured products.To address these issues related to the delay of measurements caused by the static sampling imposed by the strategy and the equipments put in place, our contribution in this thesis is to introduce the notion of the dynamic dynamic sampling. This strategy is based on an algorithm that considers the neighborhood condition to avoid the actual measurement even if the static sampling requires it. This reduces the number of actual measurements, the cycle time and the cost of production. This approach is provided by a virtual metrology module (VM) that we have developed and which can be integrated into an R2R control loop. The obtained results were validated on academic examples and on real data provided by our partner STMicroelectronics of Rousset from a chemical mechanical planarization (CMP) process. This real data also enabled the results obtained from the virtual metrology to be validated and then supplied to the R2R regulators (who need the estimation of these data).

A padronização para a fabricação de instrumentos endodônticos em aço inoxidável contribuiu para o desenvolvimento de novos aspectos geométricos. Surgiram propostas de alterações no desenho da haste helicoidal, da seção reta transversal, da ponta, da conicidade e do diâmetro na extremidade (D0). Concomitantemente, o emprego de ligas em Níquel-Titânio possibilitou a produção de instrumentos acionados a motor, largamente empregados hoje. A cada ano a indústria lança instrumentos com diversas modificações, sem, contudo, disponibilizar informações suficientes quanto às implicações clínicas destas modificações. Existe um crescente interesse no estudo dos diferentes aspectos geométricos e sua precisa metrologia. Tradicionalmente, a aferição de aspectos geométricos de instrumentos endodônticos é realizada visualmente através de microscopia ótica. Entretanto, esse procedimento visual é lento e subjetivo. Este trabalho propõe um novo método para a metrologia de instrumentos endodônticos baseado no microscópio eletrônico de varredura e na análise digital das imagens. A profundidade de campo do MEV permite obter a imagem de todo o relevo do instrumento endodôntico a uma distância de trabalho constante. Além disso, as imagens obtidas pelo detector de elétrons retro-espalhados possuem menos artefatos e sombras, tornando a obtenção e análise das imagens mais fáceis. Adicionalmente a análise das imagens permite formas de mensuração mais eficientes, com maior velocidade e qualidade. Um porta-amostras específico foi adaptado para obtenção das imagens dos instrumentos endodônticos. Ele é composto de um conector elétrico múltiplo com terminais parafusados de 12 pólos com 4 mm de diâmetro, numa base de alumínio coberta por discos de ouro. Os nichos do conector (terminais fêmeas) têm diâmetro apropriado (2,5 mm) para o encaixe dos instrumentos endodônticos. Outrossim, o posicionamento ordenado dos referidos instrumentos no conector elétrico permite a aquisição automatizada das imagens no MEV. Os alvos de ouro produzem, nas imagens de elétrons retro-espalhados, melhor contraste de número atômico entre o fundo em ouro e os instrumentos. No porta-amostras desenvolvido, os discos que compõem o fundo em ouro são na verdade, alvos do aparelho metalizador, comumente encontrados em laboratórios de MEV. Para cada instrumento, imagens de quatro a seis campos adjacentes de 100X de aumento são automaticamente obtidas para cobrir todo o comprimento do instrumento com a magnificação e resolução requeridas (3,12 m/pixel). As imagens obtidas são processadas e analisadas pelos programas Axiovision e KS400. Primeiro elas são dispostas num campo único estendido de cada instrumento por um procedimento de alinhamento semi-automático baseado na inter-relação com o Axiovision. Então a imagem de cada instrumento passa por uma rotina automatizada de análise de imagens no KS400. A rotina segue uma sequência padrão: pré-processamento, segmentação, pós-processamento e mensuração dos aspectos geométricos. / The standardization of stainless steel endodontic instruments has contributed to the development of new geometric features. Many design changes in tip shape, cross section, tapering and diameters have come out. At the same time, the use of Ni-Ti alloys enabled the production of rotary instruments, which are widely employed nowadays. In fact, the industry continuously releases novel instruments with different designs. Nevertheless, not enough information is provided about these modifications and their clinical impacts. Thus, there is a growing interest in the study of these different geometric features and their accurate metrology. Traditionally, the measurement of geometric aspects in endodontic instruments is made visually under an optical microscope. However, this visual procedure is subjective and slow. This work proposes a new method for the metrology of endodontic instruments based on scanning electron microscope (SEM) and digital image analysis. The superior depth of field of the SEM allows the whole relief of an endodontic instrument to be imaged at a constant working distance. Moreover, the images from the back-scattered electrons (BSE) detector have less artifacts and shadows, making the image analysis task easier. In addition, image analysis provides efficient ways of measuring with greater speed and statistical quality. A specific sample holder was adapted for the task of imaging endodontic files. It is composed of a multiple electrical connector, a 12 pole screw terminal strip (4 mm), on an aluminum base covered by gold plates. The holes (female terminals) in the electrical connector have an appropriate diameter (2.5 mm) to fix the endodontic instruments. Besides, the ordered placement of endodontic instruments on the electrical connector allows automating image acquisition in the SEM. The gold plates produce, in BSE images, greater atomic number contrast between the gold background and the instruments. In the built sample holder, the gold plates are in fact gold targets of a sputter coater, because it is a material commonly present in SEM labs. For each file, 4 to 6 adjacent fields at 100X are automatically imaged, to cover its entire length with the required magnification and resolution (3.12 m/pixel). These acquired images are processed and analyzed by AxioVision and KS400 softwares. First, they are assembled in a single extended field image of each instrument by a semi-automated alignment procedure based on cross-correlation in AxioVision. Then, the image of each entire instrument passes through a fully automated image analysis routine in KS400. This routine follows the image analysis standard sequence: pre-processing, segmentation, post-processing and measurement of geometric aspects. The obtained results are consistent with manual measurements but the proposed method is faster. Since assembling 4 to 6 BSE images in an extended field image is the only step that is not fully automated, the proposed method depends much less on the subjectivity of the human operator.

Este trabalho descreve a preparação, caracterização e certificação de um conjunto de materiais de referência isotópicos de urânio na faixa de 0,5 a 20,0 % de 235U em massa. Os principais conceitos da metrologia em medições químicas foram aplicados para que as propriedades certificadas nos materiais pudessem ser rastreáveis diretamente ao Sistema Internacional de Unidades (SI). Em conseqüência desta abordagem, estes materiais poderão ser utilizados na calibração de instrumentos de medição, avaliação da incerteza de medição, validação de métodos analíticos, avaliação da performance de analistas, rotinas de controle de qualidade e em programas de intercomparação de resultados de medição. As mais avançadas técnicas e métodos de espectrometria de massas, a saber, espectrometria de massas com fonte de gás (GSMS), espectrometria de massas por termoionizacão (TIMS) e espectrometria de massas com fonte de plasma induzido (ICPMS) foram investigadas para identificar quais são os componentes dominantes na incerteza e quantificar a sua contribuição no valor final da incerteza de medição da razão isotópica. Os resultados obtidos foram comparados entre si, para verificar quais técnicas e métodos estão associados aos menores valores de incerteza de medição. A razão isotópica n(235U)/n(238U) nos materiais produzidos foi certificada com incertezas de medição expandidas na faixa de 0,02 a 0,10 % e as razões n(234U)/n(238U) e n(236U)/n(238U), com incertezas na faixa de 0,03 a 2,20 %. Estes valores atendem plenamente aos requisitos da caracterização isotópica do combustível nuclear, bem como aos requisitos das análises de amostras ambientais para fins de salvaguardas nucleares. / This work describes the preparation, characterization and certification of a set of uranium isotope reference materials ranging from 0.5 to 20.0 % of 235U in mass. The most important concepts of metrology in chemical measurements were applied so that the certified quantities in these materials could be directly traceable to the International System of Units (SI). As a consequence of this approach, these materials can be used in the instruments calibration, estimation of measurement uncertainty, method validation, assessment of performance of analysts, quality control routines and interlaboratory comparison programmes. The most advanced methods and techniques in mass spectrometry, that is, gas source mass spectrometry (GSMS), thermal ionisation mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICPMS) were investigated to identify which are the dominant components in the uncertainty and to quantify its contribution to the final value of the measurement uncertainty of the isotopic ratio. The results obtained were then compared to verify which are the methods and techniques associated to the lowest measurement uncertainty values. The isotope amount ratio n(235U)/n(238U) was certified in the materials produced to expanded uncertainties ranging from 0.02 to 0.10 % and the ratios n(234U)/n(238U) and n(236U)/n(238U), to uncertainties ranging from 0.03 to 2.20 %. These values fully comply to the requirements of the isotopic characterization of nuclear fuel as well as the analysis of environmental samples for nuclear safeguards.

Aujourd'hui, il n'existe pas d'étalon de référence pour la grandeur physique des pressions dynamiques infrasonores. La demande d'étalonnage d'une telle grandeur est apparue récemment, en réponse à des problématiques du domaine de la géophysique, étudiant la propagation d'ondes acoustiques dans l'atmosphère entre 20 Hz et 0,001 Hz, soutenue par la surveillance du respect du Traité d'Interdiction Complète des Essais Nucléaires (TICE). Dans le but de répondre à cet enjeu, cette thèse a pour objectif la réalisation d'un étalon primaire pour cette grandeur. Le contexte métrologique et quelques bancs d'étalonnage existants, utilisant des générateurs de pression dynamique infrasonore, sont présentés. Afin de concevoir le banc d'étalonnage primaire, les réponses en amplitude et en phase du générateur d'infrasons du CEA sont caractérisées analytiquement et expérimentalement. Par ailleurs, le principe de l'étalon primaire basé sur le pistonphone calculable utilise les mêmes modèles d'admittance acoustique de transfert des cavités cylindriques que ceux préconisés pour l'étalonnage primaire des microphones étalons par la méthode de la réciprocité en pression. Les limites des formulations normalisées sont identifiées pour les fréquences inférieures à 100 Hz. Deux solutions alternatives sont proposées, permettant de généraliser la gamme de fréquences au domaine des infrasons. La validité de ces formulations est démontrée expérimentalement. Enfin, à partir de ces travaux, le développement du banc primaire est détaillé, avec son modèle analytique et les choix mécaniques associés. / Currently, there is no reference standard for the dynamic infrasonic pressures physical quantity. The request for calibration of such a quantity has recently appeared, in response to geophysical issues, studying the propagation of acoustic waves in the atmosphere between 20 Hz and 0.001 Hz, supported by the monitoring of the respect of the Comprehensive Nuclear-Test-Ban Treaty (CTBT). In order to meet this challenge, the aim of this thesis is to realize a primary standard for this quantity. The metrological context and some existing calibration benches, using infrasonic dynamic pressure generators, are presented. To design the primary calibration bench, the amplitude and phase responses of the CEA infrasound generator are characterized analytically and experimentally. In addition, the definition of the standard model is based on the primary method models for pressure calibration of standard microphones in the acoustic pressure range, using cylindrical cavities. The limits of the acoustic transfer admittance standard formulations for these cavities are identified for frequencies below 100 Hz. Two alternative solutions are proposed, allowing the frequency range to be extended to the infrasound domain. The validity of these formulations is demonstrated experimentally. Finally, based on this work, the development of the primary bench is detailed, with its analytical model and the associated mechanical choices.

L’effet Hall quantique (EHQ) apparaissant dans des gaz bidimentionnels d’électrons places à basse température et sous fort champ magnétique a révolutionné la métrologie des résistances depuis sa découverte en 1980 par Klaus von Klitzing. Cet effet apporte une représentation de l’ohm uniquement basé sur la constante de Planck et la charge de l’électron. En 2004, le graphène, un arrangement purement bi-dimensionnel d’atomes de carbone en nid d’abeille, dans lequel les porteurs de charge se comportent comme des fermions de Dirac, a permis de mettre à jour une nouvel effet Hall quantique. Du point de vue de la métrologie des résistances l’EHQ dans le graphène est très prometteur car plus robuste que celui apparaissant dans les hétérostructures semi-conductrices. Ceci pourrait mener à la création d’un étalon de résistance plus pratique, fonctionnant à plus haute température et plus faible champ magnétique ce qui serait un avantage notable pour une dissémination accrue d’un étalon de résistance précis vers les acteurs industriels. Dans ce manuscrit une étude complète de l’impact des défauts linéaires, omniprésent dans le graphène crû par dépôt chimique en phase vapeur sur métal, dans le régime d’effet Hall quantique est menée. Nous avons montré que ces défauts linéaires mènent à des processus de dissipation non-conventionnels qui viennent altérer la quantification de la résistance de Hall. Cette étude pointe vers l’utilisation de monocristaux pour les prochaines investigations du graphène CVD pour une application en métrologie des résistances. La deuxième partie de ce manuscrit est dédiée à l’étude du graphène crû par dépôt chimique en phase vapeur sur carbure de silicium. Nous avons comparé précisément la résistance de Hall d’un échantillon de graphène entre 10 et 19 T à la température de 1.4 K avec celle donnée par un étalon de résistance en GaAs/AlGaAs avec une incertitude relative de ( -2 ± 4 ) × 10⁻¹⁰. Pour la première fois un étalon de résistance en graphène a pu fonctionner dans les mêmes conditions de température et de champs magnétique que celui fabriqué en GaAs/AlGaAs et de plus sur un intervalle de champ magnétique plus de dix fois plus grand. Nous avons également étudié les processus de dissipation apparaissant dans cet échantillon de graphène. Cette étude montre que la longueur de localisation des porteurs de charge sature à une valeur proche de l’extension de la fonction d’onde et ce sur une grande plage de champs magnétique, ce qui soulève des questions intéressantes concernant le désordre présent dans ce type de graphène. Finalement dans un second échantillon provenant de la même technique de fabrication nous avons comparé précisément la résistance de Hall de l’échantillon de graphène avec celle d’un étalon de résistance en GaAs/AlGaAs. Il apparait que la résistance de Hall dans l’échantillon de graphène est quantifié avec une précision métrologique pour des champs magnétiques allant jusqu’à 3.5 T, des températures atteignant 9 K et reste dans un état non dissipatif jusqu’à des courants de 500 µA. Ceci ouvre une voie directe à la réalisation d’étalons quantiques de résistance réalisés en graphène. / The quantum Hall effect (QHE) observed in two dimensional electron gas placed at low temperature and under a strong perpendicular magnetic field, has revolutionized the resistance metrology since its discovery in 1980 by Klaus von Klitzing. It provides a representation of the ohm based on the Planck constant and the electron charge only. In 2004, graphene, a purely two dimensional arrangement of carbon atoms in an honeycomb lattice, where the charge carriers behave as Dirac fermions, has revealed a new flavor of the QHE. From the metrological point of view the QHE in graphene is very promising since it is much more robust than the effect appearing in conventional semiconductors and it could lead to a more convenient resistance standard operating at higher temperature and lower magnetic induction which is an advantage for a broader dissemination of a precise standard towards industrial end-users. In this manuscript, a complete study about the impact in the QHE regime of line defects such as wrinkles or grain boundaries, ubiquitous in graphene grown by chemical vapor deposition on metal is treated. We show that these line defects lead to a non conventional dissipation mechanism that jeopardize the quantum Hall effect accuracy pointing to the use of wrinkle-free monocrystals for further metrological studies. The second part of my manuscript is focused on monolayer graphene grown by chemical vapor deposition on silicon carbide. We precisely compared the Hall resistance of the graphene sample from 10 T to 19 T at the temperature of 1.4 K with a GaAs/AlGaAs resistance standard with a relative uncertainty of ( -2 ± 4 ) × 10⁻¹⁰. For the first time a graphene-based standard was able to operate in the same temperature and magnetic field conditions as semiconductor-based one, furthermore, on a magnetic range more than ten times larger. We thus made a careful study of the dissipation mechanisms taking place in this sample and measured precisely the magnitude of the localization length in the QHE regime that saturate interestingly at the extension of the charge carrier wavefunction itself, opening interesting questions about the close link between Hall quantization and localization physics in graphene grown on SiC. Finally in a second sample grown using the same technique we precisely compared the Hall resistance of the graphene sample and a GaAs/AlGaAs resistance standard that turned out to be in agreement at the metrological level for magnetic fields as low as 3.5 T current as high as 500 µA and temperature as high 9 K. This paves the way for the realization of easy to use quantum Hall resistance standards made out of graphene.