We present the development of a far-field magneto-optical Kerr effect microscope. An inverted optical microscope was constructed to accommodate Kerr imaging and atomic force microscopy. In Kerr microscopy, magnetic structure is investigated by measuring the polarization rotation of light reflected from a sample in the presence of a magnetic field. Atomic force microscopy makes use of a probe which is scanned over a sample surface to map the topography. The design was created virtually in SolidWorks, a three-dimensional computer-aided drafting environment, to ensure compatibility and function of the various components, both commercial and custom-machined, required for the operation of this instrument. The various aspects of the microscope are controlled by custom circuitry and a field programmable gate array data acquisition card at the direction of the control code written in National Instrument LabVIEW. The microscope has proven effective for both Kerr and atomic force microscopy. Kerr images are presented which reveal the bit structure of magneto-optical disks, as are atomic force micrographs of an AFM calibration grid. Also discussed is the future direction of this project, which entails improving the resolution of the instrument beyond the diffraction limit through near-field optical techniques. Preliminary work on fiber probe designs is presented along with probe fabrication work and the system modifications necessary to utilize such probes.

With increase in the number of three dimensional (3-D) nanometer-scale objects that are being either fabricated or studied, there is a need to accurately characterize their geometry. While the Atomic force microscope (AFM) is a versatile tool for performing nano-metrology, it suffers from issues of poor accessibility of 3-D features and inability to measure 3-D forces that limit its applicability in 3-D nano-metrology. This thesis investigates the design and development of a novel probing system based on AFM that improves accessibility and enables direct measurement of 3-D forces acting on the AFM tip. Two approaches are investigated to address the issue of poor accessibility. The first is to develop a novel system that enables in-situ replacement and reuse of specialized AFM tips that improve accessibility, and the second is to design a special AFM tip that can actively re-orient about two independent axes. In order to perform in-situ tip replacement, a liquid meniscus based micro-gripper is developed and integrated on to a conventional AFM probe. The stiffness of the gripper is analyzed and shown to be adequately high along all three axes for AFM imaging to be performed. Tip replacement and re-use are both experimentally demonstrated by employing a novel tip-exchange station. The replaced tips are employed to show artifact-free AFM imaging of a standard calibration grating in both tapping-mode and contact-mode. To actively re-orient a conventional tip, a novel magnetically-actuated micro-scale ball-and-socket joint is integrated onto an AFM probe. The quasi-static behavior of the joint is experimentally characterized, and the ability of the tip to independently re-orient about two axes is demonstrated. The achieved range is about +/- 90 degrees about both X- and Y-axes. In order to realize the potential of the proposed probes for 3-D nano-metrology, an AFM is developed in-house that possesses the capability to make direct measurement of 3-D forces. Optimization of the measurement system to achieve identical sensitivities and resolution along all three axes is studied. Subsequently, the necessary electronics for measurement, actuation and control are developed. All the subsystems are experimentally calibrated and integrated. The overall AFM is shown to have a resolution of about 0.2 nm when operated in tapping-mode. The developed AFM is employed to showcase the following applications: characterization of the coefficient of kinetic friction of Muscovite mica, force controlled nano-scribing on polymethyl methacrylate (PMMA) and tapping-mode imaging of a calibration grating with the developed re-orientable AFM probe. Finally, the unique ability of the re-orientable AFM probe to control its tip-orientation is employed to develop a nanometer-scale coordinate measurement machine (CMM). The developed nano-CMM is shown to access the vertical wall of a sample and obtain its topography.

This thesis addresses particular topics in the field of the length metrology for nanometrology. Nanometrology deals with dimensional measurements of micro- and nanostructures with a high spatial resolution. It typically combines a microscope imaging with a precise coordinate measurement, usually capable of nanometre resolution using the state-of-art laser interferometry techniques. The development in this field is driven, among others, by emerging advanced nanotechnologies that demand to push further the capabilities and limits of the interferometric techniques to make the nanometre-level dimensional measurement of nanostructures possible. The principal limitations of current systems are the environmental conditions and especially the fluctuations in the refractive index of air. The theoretical part of this thesis aim at analysis of individual parts of laser interferometer. I oriented myself on the study of their advantages/disadvantages and further also the possibilities of their industrial applications. The second part of the thesis presents my work that focused on the influence of the refractive index of air (RIA) on the measurement uncertainty. I experimentally demonstrated an interferometric system with a self-cancellation RIA fluctuations: a transparent photodetector is used for the measurement of the standing wave along the axis of a passive resonator, where the resonator also serves as a reference for the laser wavelength stabilisation. Another optical arrangement, based on a setup of several Michelson interferometers, represents a combination of an interferometer and a refractometer into a single system. This setup was used to study the behaviour of the ambient airflow with respect to the optical path difference and physical separation of the interferometer’s and refractometer’s path. Based on the experimental results I proposed new arrangements for shape measuring interferometers, which combine length interferometry and a tracking refractometer for the direct compensation of RIA fluctuations with geometrically adjacent optical beams. The results indicate an improvement in RIA fluctuation induced uncertainty by a factor of 100. Third part describes the design and implementation of interferometric systems for specific applications. For the industrial environment I developed a compact interferometric displacement gauge which is designed to allow nanometre level measurement using a simplified interferometer construction. For coordinate measurement of the position of the sample up to six degrees of freedom, I realised a compact modular interferometric system, which represents a unique setup together with a stabilised laser source. To measure the position of the sample in an electron beam writer chamber, I designed and implemented a differential interferometer that works in the near infrared domain and uses a new detection method developed for this system. In the fourth part I describe the realisation of a high-speed interferometer with a differential arrangement, which allows evaluation of high-cycle fatigue in material engineering. This method of studying high-cycle fatigue should be beneficial for both the basic research and the engineering practice.

À l'heure où les nanotechnologies sont en plein essor, la précision des mesures réalisées à l'échelle nanométrique devient un défi essentiel pour améliorer les performances et la qualité des produits intégrant des nano. Pour répondre aux besoins sous-jacents en nanométrologie dimensionnelle, le Laboratoire National de métrologie et d'Essais (LNE) a conçu intégralement un Microscope à Force Atomique métrologique (mAFM). Son objectif principal est d'assurer la traçabilité au mètre défini par le Système International d'unités (SI) pour les mesures à l'échelle nanométrique. Pour cela, le mAFM utilise quatre interféromètres différentiels qui mesurent en temps réel le déplacement relatif de la pointe par rapport à l'échantillon. Cet instrument de référence est destiné à l'étalonnage d'étalons de transfert couramment utilisés en microscopie à champ proche (SPM) et en microscopie électronique à balayage (SEM). Lors de ce processus, une incertitude de mesure est évaluée. Elle détermine un niveau de confiance de l'étalonnage réalisé par le mAFM. Cette incertitude est généralement évaluée grâce à des mesures expérimentales permettant de déterminer l'impact de certaines sources d'erreur qui dégradent les mesures à l'échelle du nanomètre. Pour d'autres sources d'erreur, leur évaluation reste complexe ou expérimentalement impossible. Pour surmonter cette difficulté, le travail de thèse a consisté à mettre en place un modèle numérique de l'instrument nommé " AFM virtuel ". Il permet de prévoir l'incertitude de mesure du mAFM du LNE en ciblant les sources critiques d'erreur grâce à l'utilisation d'outils statistiques tels que la Méthode de Monte Carlo (MCM), les plans de Morris et les indices de Sobol. Le modèle utilise essentiellement la programmation orientée objet afin de prendre en compte un maximum d'interactions parmi les 140 paramètres d'entrée, en intégrant des sources jusqu'ici négligées ou surestimées par manque d'informations. / At present where nanotechnology applications are growing fast and nano products spreading worldwide, measurement accuracy at nanometer scale becomes an essential challenge to improve the performance and the quality of products integrating nano. To meet the specific needs in the field of dimensional nanometrology, LNE (French metrology institute) integrally designed a metrological Atomic Force Microscope (mAFM). Its main objective is to ensure the traceability of nanoscale measurements to the meter as defined by the International System of Units (SI). The mAFM uses four differential interferometers which measure the tip to sample relative position. This instrument will be devoted to the calibration of transfer standards commonly used in scanning probe microscopy (SPM) and scanning electron microscopy (SEM). During this process, a measurement uncertainty is evaluated to determine a confidence level of the calibration realized by the mAFM. This uncertainty is usually evaluated thanks to experimental measurements which determine the impact of some error sources which degrade measurements at the nanoscale. For other components, their evaluation can be more complex and sometimes impossible to estimate experimentally. To overcome this difficulty, the thesis work consisted in the development of a numerical model called "Virtual AFM". It allows producting the measurement uncertainty of the LNE's mAFM and to identify the critical components by using statistic tools such as Monte Carlo Method (MCM), Morris' design and Sobol' indices. The model uses essentially oriented-object programming to take into account a maximum of interactions from about 140 input quantities. It allowed integrating components previously neglected or overestimated due to a lack of information.

Hintergrund: Die Entwicklung von Nanotechnologien und insbesondere integrierten Schaltkreisen beruht auf dem Verständnis von Struktur und Funktion auf der Nanoskala, wofür exakte Messungen erforderlich sind. Kleinwinkel-Röntgenstreuung unter streifendem Einfall (GISAXS) ist eine Methode zur schnellen, berührungs- und zerstörungsfreien dimensionellen Messung von nanostrukturierten Oberflächen. Ziele: Es soll die Möglichkeit untersucht werden, die zunehmend komplexeren Proben aus Wissenschaft und Industrie mit Hilfe von GISAXS präzise zu vermessen. Ein weiteres Ziel ist es, Messtargets aus der Halbleiter-Qualitätskontrolle mit einer Größe von ca. 40x40 µm² zu messen, deren Signal typischerweise nicht zugänglich ist, weil ein Bereich von ca. 1x20 mm² auf einmal beleuchtet wird. Methoden: Synchrotron-basierte GISAXS-Messungen verschiedener Proben werden mit Hilfe einer Fourier-Konstruktion, der "distorted wave Born approximation" und einem Maxwell-Gleichungs-Löser basierend auf finiten Elementen analysiert. Ergebnisse: Aus GISAXS-Messungen kann die Linienform von Gittern mit einer Periode von 32 nm rekonstruiert werden und sie weicht weniger als 2 nm von Referenzmessungen ab. Eine sorgfältige Bayes'sche Unsicherheitsanalyse zeigt jedoch, dass wichtige dimensionelle Parameter innerhalb der Unsicherheiten nicht übereinstimmen. Für die Messung von kleinen Gittertargets entwerfe ich ein neuartiges Probendesign, bei dem das Target in Bezug auf die umgebenden Strukturen gedreht wird, und stelle fest, dass dadurch parasitäre Streuung effizient unterdrückt wird. Fazit: GISAXS-Messungen von komplexen Nanostrukturen und kleinen Targets sind möglich, jedoch würde GISAXS enorm von effizienteren Simulationsmethoden profitieren, die alle relevanten Effekte wie Rauhigkeit und Randeffekte einbeziehen. Hier gibt es vielversprechende theoretische Ansätze, so dass GISAXS eine zusätzliche Methode für die Halbleiter-Qualitätskontrolle werden könnte. / Background. The development of nanotechnology such as integrated circuits relies on an understanding of structure and function at the nanoscale, for which reliable and exact measurements are needed. Grazing-incidence small angle X-ray scattering (GISAXS) is a versatile method for the fast, contactless and destruction-free measurement of sizes and shapes of nanostructures on surfaces. Aims. A goal of this work is to investigate the possibility of precisely measuring the increasingly complex samples produced in science and industry using GISAXS. A second objective is to measure targets used in semiconductor quality control with a size of approx. 40x40 µm², whose signal is typically not accessible because an area of approx. 1x20 mm² is illuminated at once. Methods. I take synchrotron-based GISAXS measurements and analyze them using reciprocal space construction, the distorted wave born approximation, and a solver for Maxwell's equations based on finite elements. Results. I find that the line shape of gratings with a period of 32 nm can be reconstructed from GISAXS measurements and the results deviate less than 2 nm from reference measurements; however, a careful Bayesian uncertainty analysis shows that key dimensional parameters do not agree within the uncertainties. For the measurement of small grating targets, I create a novel sample design where the target is rotated with respect to the surrounding structures and find that this efficiently suppresses parasitic scattering. Conclusions. I show that GISAXS measurements of complex nanostructures and small targets are possible, and I highlight that further development of GISAXS would benefit tremendously from efficient simulation methods which describe all relevant effects such as roughness and edge effects. Promising theoretical approaches exist, so that GISAXS has the potential to become an additional method in the toolkit of semiconductor quality control.

The presented doctoral thesis deals with measurements of extremely small sizes in nanometrology using a touch probe, which constitutes a part of a three-coordinate measuring system. It addresses a newly developed method of exact measurements in nanometrology by touch probes. The aim of this work was to expand the measurement options of this device and design a methodology proposal for the measurement of small parts, including the determination of accuracy of measurement of this device when used in nanometrology. The work includes the new methodology for the calculation of uncertainty of measurement, which constitutes a keystone in determining the accuracy of measurement of a accuracy three coordinate measuring system (hereinafter only nano-CMM). The first part of the doctoral thesis analyzes the present situation in the area of evaluation of accuracy of measurement in very accurate length measurements. It defines and describes individual methods implemented in the determination of accuracy of measurement on the instrument nano-CMM. A great emphasis is placed on the methodology of the measurement uncertainty, which draws from the author’s experience as a metrologist working in the laboratories of the Department of Primary nanometrology and technical length, Czech Metrology Institute Brno (hereinafter only CMI Brno). The second part of the doctoral thesis focuses on the determination of accuracy of length measurement in nanometrology, using a large set of measurements that were carried out under the reproducibility and repeatability conditions. There is also described and tested a model procedure utilizing the Monte Carlo method to simulate the measuring system nano-CMM in order to extent the newly created methodology of the measurement of uncertainty using a touch probe on the instrument nano-CMM. A substantial part of this doctoral thesis provides a detailed evaluation of results obtained from experiments that were executed under the repeatability and reproducibility conditions, especially for the purposes of the determination of the uncertainty of measurement. In this doctoral thesis, the uncertainty of measurement is chosen to quantify the accuracy of measurement of the instrument nano-CMM. The final part of this thesis summarizes the knowledge obtained during the scientific research and provides its evaluation. For the methodology used to determine the accuracy of measurement in nanometrology, it also outlines the future development in the area of scientific research, including the practical use in metrological traceability and extremely accurate measurements for customers. Furthermore, it deals with the possible use of other scanning systems compatible with the instrument nano-CMM.

The diploma thesis deals with the design of three length standards, which will serve to ensure metrological traceability between Rigaku nano3DX, SIOS NMM-1, Zeiss UPMC Carat 850 and other devices located at ÚVSSR BUT and CEITEC Brno. The first part of the thesis focuses on the theoretical acquaintance with concepts closely related to the issue of ensuring metrological traceability. In addition, this section deals with computed tomography and the description of individual devices. The second part of the thesis is devoted to design, production process and testing of individual standards. The last part describes the ensuring the calibration of the smallest standard, the so-called Nano standard and the calculation of the uncertainty of measuring its calibrated length. At the end of the thesis, the outputs of these activities are evaluated.

Ultraprecision single point diamond turning is required to produce parts with sub-nanometer surface roughness and sub-micrometer surface profiles tolerances. These parts have applications in the optics industry, where tight form accuracy is required while achieving high surface finish quality. Generally, parts can be polished to achieve the desired finish, but then the form accuracy can easily be lost in the process rendering the part unusable. Currently, most mid to low spatial frequency surface finish errors are inspected offline. This is done by physically removing the workpiece from the machining fixture and mounting the part in a laser interferometer. This action introduces errors in itself through minute differences in the support conditions of the over constrained part on a machine as compared to the mounting conditions used for part measurement. Once removed, the fixture induced stresses and the part’s internal residual stresses relax and change the shape of the generally thin parts machined in these applications. Thereby, the offline inspection provides an erroneous description of the performance of the machine. This research explores the use of a single, high resolution, capacitance sensor to quickly and qualitatively measure the low to mid spatial frequencies on the workpiece surface, while it is mounted in a fixture on a standard ultraprecision single point diamond turning machine after a standard facing operation. Following initial testing, a strong qualitative correlation exists between the surface profiling on a standard offline system and this online measuring system. Despite environmental effects and the effects of the machine on the measurement system, the capacitive system with some modifications and awareness of its measurement method is a viable option for measuring mid to low spatial frequencies on a workpiece surface mounted on an ultraprecision machine with a resolution of 1nm with an error band of ±5nm with a 20kHz bandwidth. / Thesis / Master of Applied Science (MASc)