Este trabalho apresenta dois tipos de ensaios não destrutivos para a correlação do módulo dinâmico com a resistência à compressão para elementos de concreto. Os métodos de ensaio são a ultrassonografia e o método de excitação por impulso utilizando o equipamento Sonelastic®. Neste trabalho estão descritos seus funcionamentos, aplicações e limitações. A ultrassonografia, através da propagação de ondas sonoras, fornece, indiretamente, o módulo de elasticidade dinâmico. Com o método de excitação por impulso obtêm-se as frequências naturais e os modos de vibração do elemento estudado, o que permite determinar seu módulo dinâmico. Primeiramente, estes ensaios foram utilizados em corpos-de-prova cilíndricos e lajes alveolares produzidas em laboratório para a obtenção das curvas de correlação e, em seguida, estes mesmos ensaios foram realizados na fábrica de concreto pré-moldado. Para elementos de geometria complexa, como é o caso das lajes alveolares, apresenta-se uma metodologia para a obtenção de uma equação analítica para o cálculo do módulo dinâmico no ensaio de excitação por impulso. Estes métodos tiveram o objetivo final de avaliar a resistência à compressão do concreto na pista de protensão da fábrica, e então determinar o melhor momento para a desforma e corte do cabo de protensão. Com ambos os métodos, obteve-se ótimas correlações do módulo dinâmico com a resistência à compressão dos elementos em laboratório. Na fábrica de concreto pré-moldado não foi possível obter uma curva de correlação representativa de toda a laje na pista de protensão, porém foi possível registrar um bom indicativo de que é possível obter boas correlações para futuras pesquisas no assunto / This work presents two types of non-destructive testing for the correlation of the dynamic elastic modulus with the compressive strength. The test methods are the ultrasonography and the impulse excitation using the Sonelastic® equipment. In this work the equipaments operations, applications and limitations are also described. The ultrasound test indirectly supplies the dynamic elastic modulus through the propagation of sound waves. The natural frequencies and the vibration modes of the studied elements are obtained through impulse excitation method allowing to determine its dynamic modulus. To start, these tests were used in cylindrical specimens and hollow core slabs produced in the laboratory to obtain the correlation curves, and then these same methods were performed in the pre-cast concrete plant. As for complex geometric elements, as in the case of hollow core slabs, a methodology is applied in order to obtain an analytic equation to calculate the dynamic modulus in the impulse excitation test. These methods had the final goal the evaluation of the strength of prestressed concrete lying on track of the plant, so as to determine the best moment to demold and cut the prestressed cable. Excellent correlations of the dynamic modulus with compressive strength of the elements made in laboratory were obtained using both methods. It was not possible to obtain in the precast concrete plant a representative correlation curve of the whole slab on the track, nevertheless, it was possible to record a good indication that it is possible to obtain good correlations for future research.

A análise dinâmica experimental tem sido amplamente pesquisada como uma ferramenta de avaliação de integridade de estruturas de concreto armado. Existem técnicas de identificação de danos baseadas em propriedades modais como frequências de ressonâncias, deformadas modais, curvaturas modais e amortecimento. Há também técnicas baseadas na não linearidade da resposta dinâmica, que apesar do grande potencial na detecção de danos, têm sido pouco exploradas nos últimos anos. Este trabalho tem por objetivo avaliar a integridade estrutural de vigas de concreto armado através do comportamento da resposta dinâmica. Foram realizados ensaios dinâmicos em duas vigas de concreto armado com 3,5 m de comprimento, 25 cm de largura, 35 cm de altura e idênticas taxas de armaduras, mas configuradas com barras de aço de diferentes diâmetros, 2 &#981 16 mm e 8 &#981 8 mm, respectivamente. Tais vigas, inicialmente íntegras, foram submetidas a ciclos de carregamento e descarregamento com intensidades crescentes até atingir a ruptura do elemento. Após cada ciclo, as propriedades dinâmicas foram avaliadas experimentalmente, com o emprego de técnicas de excitação por sinais do tipo aleatório e tipo transiente, respectivamente, visando determinar parâmetros que indiquem a deterioração gradativa do elemento. Nesses ensaios dinâmicos aplicaram-se diferentes amplitudes da força de excitação. Verificou-se que o aumento da amplitude da força dinâmica de excitação provocou reduções nos valores das frequências de ressonância de 1,1% e 2,4%, associadas, respectivamente, às excitações aleatórias e transientes; e um comportamento não linear dos índices de amortecimento, associados às excitações aleatórias, mantendo um crescimento linear com as excitações transientes. Constatou-se, ainda, que os valores das frequências de ressonância decrescem com a redução de rigidez mecânica, diminuída com o aumento do nível de fissuração induzido nos modelos. Já os valores dos índices de amortecimento, após cada ciclo, se comportaram de forma não linear e assumiram diferentes valores, conforme a técnica de excitação empregada. Acredita-se que esta não linearidade está relacionada aos danos provocados no elemento pela solicitação estrutural e, por consequência, ao processo de como a dissipação de energia é empregada no processo de instauração, configuração e propagação das fissuras nos elementos de concreto armado. / The experimental dynamic analysis has been widely investigated as a tool to assess integrity of reinforced concrete structures. State-of-the-art modal-based techniques for structural damage analysis use resonance frequencies, modal deformed, curvature and modal damping analysis. There are also techniques based on nonlinear dynamic response that despite the large potential for damage detection, have not been considered in recent years. This work aims to evaluate the structural integrity of reinforced concrete beams through the dynamic response behavior. Dynamic tests were performed on two reinforced concrete beams with 3.5 meters of length, 250 mm of width, 350 mm of height and identical reinforcement rates, but different steel bars diameters, 2 &#981 16 mm e 8 &#981 8 mm, respectively. Beams were initially intact and were subjected to loading and unloading cycles with increasing intensity until the rupture of the concrete beam. After each cycle, the dynamic properties were evaluated experimentally with random and transient excitation signals to determine parameters that indicate gradual deterioration of the beam. Different amplitudes of the excitation force were applied during dynamic testing of concrete beams. These results indicated that an increase in amplitude of dynamic excitation force caused reductions in frequency resonances by 1.1% and 2.4%, associated with the random and transient excitations, respectively. Furthermore, a non-linear behavior of the damping ratios related to random excitations was observed while a linear relationship with transient excitation was found. Moreover, it was found that the resonance frequency decreased with the cracking-related reduction of beam stiffness, caused by increasing level of loading. Additionally, the values of the damping ratios after each cycle behaved non-linearly assuming different values according to the used excitation technique. It is believed that this non-linearity can be related to the loading-related structural damage of the reinforced concrete beam. Therefore, the energy dissipation related to cracking initiation, configuration and propagation in reinforced concrete elements played an important role in the damping ratios of concrete beams.

La thèse s’inscrit dans les travaux du CEA LIST pour développer dans la plate-forme CIVA un module simulant le contrôle non-destructif (CND) par ondes ultrasonores guidées ; elle est dédiée au développement et à la validation de modèles simulant l’inspection de canalisations et se focalise sur le cas de canalisations comportant un ou plusieurs coudes. Pour prédire l’effet de la courbure sur les ondes guidées, une extension en coordonnées curvilignes de la méthode des éléments finis semi-analytiques est réalisée pour calculer les modes se propageant dans un coude, par résolution d’un système d’équations aux valeurs propres restreint à la section du guide. Ce développement a aidé à comprendre les effets de distorsion des champs ultrasonores et de décalage des fréquences de coupures dus à la courbure. La diffraction des ondes à la jonction entre un tube droit et un coude est ensuite calculée par raccordement modal donnant la matrice de diffraction de la jonction ; les éléments de la matrice s’obtiennent par évaluation numérique d’intégrales à la surface de la jonction. Les matrices de diffractions locales sont enfin combinées à des matrices de propagation pour rendre compte de la présence de plusieurs diffracteurs sur la canalisation, sous forme d’une matrice globale de diffraction. Le coût minimal de son calcul permet d’étudier l’influence des paramètres de contrôle et de les optimiser. Les modèles sont validés en comparant leurs prédictions avec des résultats numériques et expérimentaux de la littérature et des mesures faites au CETIM sur maquettes industrielles. Intégrés à la plate-forme CIVA, ils étendent les possibilités du module de simulation du CND par ondes guidées. / The thesis is in the framework of developments made at CEA LIST of a module of the CIVA platform to simulate nondestructive testing (NDT) by ultrasonic guided waves; it is dedicated to the development and the validation of models simulating the examination of pipelines and is focussed on the case of pipeline comprising one or several elbows. To predict effects due to the curvature on guided waves, an extension in curvilinear coordinates of the semi-analytic finite element method is worked out to compute modes propagating in an elbow, by solving an eigen system restricted to the guide section. This development allows us to better understand effects due to the curvature such as displacement field distortions or cut-off frequencies splits. The scattering of waves at the junction between a straight tube and an elbow is then computed by means of the mode-matching method, leading to the modal scattering matrix of the junction; matrix elements are obtained by numerical evaluation of integrals over the junction surface. Local scattering matrices are finally combined to propagation matrices to account for the presence of several scatterers in the pipeline, to form a global scattering matrix. Its minimal computation cost allows us to study the influence of the parameters of the testing configuration and to optimize them. Models are validated by comparing their predictions to numerical and experimental results of the literature and to measurements made at CETIM on industrial mock-ups. Integrated in the platform CIVA, the developed models extend the capabilities of the guided wave NDT module.

Ce travail rentre dans le cadre de la caractérisation des couches minces, de revêtements et de surfaces fonctionnelles (épaisseur, constantes élastiques,…). Parmi les méthodes de caractérisation potentielles, les méthodes ultrasonores employant des ondes de surface sont particulièrement intéressantes. Pour ce faire, nous avons choisi d’exploiter la dispersion des ondes de surface de type Rayleigh. En effet, les ondes acoustiques de surface (SAW) de type Rayleigh se propagent à la surface d’un matériau et l’énergie véhiculée par ces ondes est confinée sous la surface dans une couche d’épaisseur de l’ordre d’une longueur d’onde. Afin de caractériser ces revêtements, il est nécessaire de travailler sur une large gamme de fréquences. D’autre part, ces couches peuvent être fragiles et transparentes, c’est pourquoi, des transducteurs interdigités (IDT) sont envisagés. Pour optimiser ce type de capteurs, et en particulier leur bande passante, il est nécessaire d’étudier différentes configurations sachant qu’il est notamment possible de faire varier le nombre d’électrodes, les dimensions des électrodes, leurs formes et leurs espacements. Enfin, pour exciter ces ondes de surface dans une large gamme de fréquence avec des niveaux de déplacement suffisants pour la caractérisation des couches minces et revêtements, la technique à double Chirp spatio-temporel basée sur des transducteurs SAW-IDT a été privilégiée. Nous avons montré les potentialités de cette approche en caractérisant premièrement des structures à couche mince métalliques d’épaisseurs de 100 nm et plus, et deuxièmement des revêtements transparents de type sol-gel. / This work is within the scope of characterization of thin layers, coatings and functional surfaces (thickness, elastic constants,…). Among the characterization methods, the ultrasonic methods using surface acoustic waves are particularly interesting. In order to do this, we chose to make use the dispersion phenomenon of Rayleigh-like surface acoustic waves. Indeed, the propagation of these waves is close to the surface of material and the energy is concentrated within a layer under the surface of about one wavelength thick. In order to characterize these coatings and structures, it is necessary to perform measurements in high frequencies. On the other hand, these coatings can be fragile and transparent, this is why in this study, SAW-IDT sensors are achieved for surface acoustic wave generation. For optimization of these SAW-IDT sensors, particularly their band-width, it is necessary to study various IDT configurations by varying the number of electrodes, dimensions of the electrodes, their shapes and spacings. Finally, to generate the surface acoustic waves over a wide frequency range with sufficient displacement amplitude for the characterization of thin films and coatings, a time-space chirp technique with SAW-IDT sensors was selected. We have shown the potential of this approach by characterizing firstly thin metallic layers, and secondly transparent coatings obtained by the sol-gel process.

Les structures mécaniques utilisées de nos jours ne cessent d’évoluer en utilisant des matériaux composites ou à gradient fonctionnel afin de répondre aux enjeux de résistance accrue, allégement de la structure et amélioration des performances. Ceux-ci nécessitent un contrôle adéquat de leur état de santé afin de s’assurer de l’intégrité de la structure. L’utilisation des ondes guidées ultrasonores fournit un moyen efficace et rapide d’inspection sur de longues distances. Néanmoins, ces ondes présentent certaines caractéristiques complexes qui rendent la tâche très difficile. L’utilisation d’outils d’analyse tels que les modèles numériques constitue un grand atout pour ce type d’application. Dans ce contexte, l’objectif de cette de thèse est le développement d’un outil de modélisation performant, permettant d’étudier la propagation des ondes guidées ultrasonores avec une grande précision et une faible consommation de ressources et de temps de calculs. De ce fait, l’intérêt est porté sur des méthodes numériques d’ordres élevés dont les propriétés de convergence sont beaucoup améliorées que les méthodes classiques. En particulier, la méthode semi-analytique éléments finis de Galerkin discontinue pour la détermination des courbes de dispersion des ondes guidées est développée. La méthode est applicable aux structures planes et cylindriques fabriquées de matériaux isotropes, anisotropes et hétérogènes (à gradient fonctionnel de propriétés). Une étude comparative sur l’analyse des performances de ces méthodes est effectuée. Celle-ci a démontré la capacité de la méthode à modéliser la propagation des ondes guidées ultrasonores dans des guides d’ondes à section arbitraire avec des performances prometteuses par rapport à la méthode des éléments finis classique. / The mechanical structures used today are constantly evolving using composite or functionally gradient materials to meet the challenges of increased strength, lightening the structure and improving performance. These require adequate control of their state of health to ensure the integrity of the structure. The use of Ultrasound Guided Waves (UGW) provides an efficient and fast way of inspection over long distances. Nevertheless, these waves have some complex features that make the task very difficult. The use of analysis tools such as numerical models is a great asset for this type of application. In this context, the objective of this thesis is the development of a powerful modeling tool, allowing to study the propagation of UGWs with a great precision, less computational time and consumption of resources. Accordingly, we are interested in higher order numerical methods whose convergence properties are much improved than the classical methods. In particular, a semi-analytical discontinuous Galerkin finite element method (SADG-FE) is developped for the determination of the dispersion properties of guided waves in arbitrary cross-section waveguides. The method is applicable to plates and cylindrical structures made of isotropic, anisotropic heterogeneous (functionally graded) materials. The performance analysis of these methods and their comparisons are performed with respect to the models based on the classical finite element method. The results demonstrated the ability of the proposed method to model the propagation of ultrasounic guided waves in arbitrary section waveguides with promising performance over the conventional finite element method.

North American civil infrastructures are aging. According to recent (2016) Canadian infrastructure report card, 33% of the Canadian municipal infrastructures are either in fair or below fair condition. The current deficit of replacing fair and poor municipal bridges (covers 26% of bridges) is 13 billion dollars. According to the latest report (2017) by American Society of Civil Engineers, the entire American infrastructure have been given a D+ condition rating. This includes some of the structural elements of infrastructures that pose a significant risk and there is an urgent need for frequent and effective inspection to ensure the safety of people. Visual inspection is a commonly used technique to detect and identify surface defects in bridge structures as it has been considered the most feasible method for decades. However, this currently used methodology is inadequate and unreliable as it is highly dependent on subjective human judgment. This labor-intensive approach for inspection requires huge investment in terms of an arrangement of temporary scaffoldings/permanent platforms, ladders, snooper trucks, and sometimes helicopters. To address these issues associated with visual inspection, the completed research suggests three innovative methods; 1) Combined use of Fuzzy logic and Image Processing Algorithm to quantify surface defects, 2) Unmanned Aerial Vehicle (UAV)-assisted American Association of State Highway and Transportation Officials (AASHTO) guideline-based damage assessment technique, and 3) Patent-pending multi-device robotics-based sensor data acquisition system for mapping and assessing defects in civil structures. To detect and quantify subsurface defects such as voids and delamination using a UAV system, another patent-pending UAV-based acoustic method is developed. It is a novel inspection apparatus that comprises of an acoustic signal generator coupled to a UAV. The acoustic signal generator includes a hammer to produce an acoustic signal in a structure using a UAV. An outcome of this innovative research is the development of a model to refine multiple commercially available NDT techniques’ data to detect and quantify subsurface defects. To achieve this, a total of nine 1800 mm × 460 mm reinforced concrete slabs with varying thicknesses of 100 mm, 150 mm and 200 mm are prepared. These slabs are designed to have artificially simulated defects like voids, debonding, honeycombing, and corrosion. To determine the performance of five NDT techniques, more than 300 data points are considered for each test. The experimental research shows that utilizing multiple techniques on a single structure to evaluate the defects, significantly lowers error and increases accuracy compared to that from a standalone test. To visualize the NDT data, two-dimensional NDT data maps are developed. This work presents an innovative method to interpret NDT data correctly as it compares the individual data points of slabs with no defects to slabs with simulated damage. For the refinement of NDT data, significance factor and logical sequential determination factor are proposed. / Graduate / 2020-09-06

In the nanoscale metrology industry, there is a need for low-cost instruments, which have the ability to probe the structrure and elemental composition of thin films. This dissertation, describes the research performed to design and simulate a miniature Cylindrical Mirror Analyzer, (CMA), and Auger Electron Spectrometer, (AES). The CMA includes an integrated coaxial thermionic electron source. Electron optics simulations were performed using the Finite Element Method, (FEM), software COMSOL. To address the large Secondary Electron, (SE), noise, inherent in AES spectra, this research also included experiments to create structures in materials, which were intended to suppress SE backgound noise in the CMA. Laser Beam Machining, (LBM), of copper substrates was used to create copper pillars with very high surface areas, which were designed to supress SE’s. The LBM was performed with a Lumera SUPER RAPID‐HE model Neodymium Vanadate laser. The laser has a peak output power of 30 megawatts, has a 5x lens and a spot size of 16 μm. The laser wavelength is in the infrared at 1064 nm, a pulse width of 15 picoseconds, and pulse repetition rate up to 100 kHz. The spectrometer used in this research is intended for use when performing chemical analysis of the surface of bulk materials and thin films. It is applicable for metrology of thin films, as low as 0.4 nm in thickness, without the need to perform destructive sample thinning, which is required in Scanning Tranmission Electron Microscopy, (STEM). The spectrometer design is based on the well known and widely used coaxial cylinder capacitor design known as the Cylindrical Mirror Analyzer, (CMA). The coaxial tube arrangement of the CMA allows for placing an electron source,which is mounted in the center of the inner cylinder of the spectrometer. Simulation of the electron source with an Einzel Lens was also performed. In addtion, experiments with thin film coatings and Laser Beam Machining to supress Secondary Electron emission noise within the Auger electron spectrum were completed. Design geometry for the miniature CMA were modeled using Computer Aided Design, (CAD). Fixed Boundary Conditions, (BC), were applied and the geometry was then meshed for FEM. The electrostatic potential was then solved using the Poisson equation at each point. Having found the solution to the electrostatic potentials, electron flight simulations were performed and compared with the analytical solution. From several commercially available FEM modeling packages, COMSOL Multiphysics was chosen as the research platform for modeling of the spectrometer design. The CMA in this design was reduced in size by a factor of 4 to 5. This enabled mounting the CMA on a 2 ¾ in flange compared to the commercial PHI model 660 CMA which mounts onto a 10 in flange. Results from the Scanning Electron Microscopy measurements of the Secondary Electron emission characteristics of the LBM electron suppressor will also be presented.

La compréhension du comportement d'un composite à matrice céramique (CMC) lorsqu'il est sollicité en fatigue est l'un des points clés pour permettre son utilisation dans un cadre industriel. Il est en effet nécessaire de déterminer la chronologie des différents mécanismes d'endommagement ainsi que d'estimer la durée de vie en conditions d'utilisation. Il est alors nécessaire de réaliser une caractérisation mécanique mais aussi de définir des indicateurs d'endommagement permettant la prévision de durée de vie. Dans ce but, il est intéressant de coupler l'analyse des paramètres mécaniques et les observations microstructurales à des techniques de suivi en temps réel de l'endommagement. L'émission acoustique (EA) est une méthode de suivi non destructive qui permet de répondre à cette problématique. Elle permet notamment de quantifier et de localiser l'endommagement. Dans ce travail, de nouveaux indicateurs d'endommagement sont mis en place tels la "Sévérité" des signaux définie à partir de l'énergie acoustique ainsi que la "Sentry function" définie à partir de l'énergie acoustique et de l'énergie mécanique. Ce travail s'articule autour de deux principaux axes. Dans un premier temps il s'agit de caractériser les effets de la sollicitation cyclique sur ce type de matériau, ceci notamment en comparant l'évolution des paramètres mécaniques, les observations microstructurales ainsi que l’analyse de l'évolution globale de l'émission acoustique (EA) lorsque le matériau est soumis à un chargement statique et à un chargement cyclique. La seconde partie consiste à déterminer un scenario d'endommagement. Dans un premier temps, les signaux d’EA sont analysés en fonction de leur détection dans le cycle (charge/décharge). Ensuite la détermination de la signature acoustique des différents mécanismes d'endommagement par application de techniques de reconnaissance de formes supervisées a permis d'évaluer leur chronologie d'activation durant les essais de fatigue cyclique. Cette étude a permis de mettre en évidence un ensemble de mécanismes propres à la sollicitation cyclique, composé principalement de décohésion et de frottement aux interfaces fibre/matrice et matrice/matrice. De plus, l'utilisation de l'émission acoustique a permis de définir des temps caractéristiques ou critiques pouvant être utilisés dans un objectif de prévision de la durée de vie. En effet, par exemple la sévérité des signaux a permis de mettre en évidence un temps caractéristique situé entre 25 et 45% de la durée de vie du matériau. La détection en temps réel de ce temps caractéristique permet d'estimer la durée de vie restante. / The full understanding of a ceramic matrix composite under fatigue loading is needed in view of industrial applications. It is necessary to determine the damage mechanisms chronology and to be able to forecast the lifetime of the material in the conditions of use. To reach these purposes, a mechanical characterisation has to be done as well as the definition of damage indicators. It is then interesting to link the analysis of mechanical parameters and microscope observations with a non-destructive monitoring technique. Acoustic emission (AE) appears to be a good candidate to monitor material damage under loading. It makes the quantification and the material damage localisation possible. In this study, indicators based on released acoustic energy are used as "Severity" of signals or "Sentry function" which depends on both acoustic and mechanical energies. This work is organised in two parts. First, the analysis of mechanical parameters behaviour, material microstructure and global evolution of acoustic emission under static and cyclic loading makes the characterisation of the effects of cyclic fatigue on the material possible. The second part consists in determining a damage scenario. First acoustic emission signals are analysed depending on their acquisition during a cycle (loading or unloading). Then the connection between the acoustic emission signals and the different damage mechanisms, using a supervised clustering method, facilitated the estimation of the activation of these different damage mechanisms during cyclic fatigue tests. This study pointed out different damage mechanisms generated by cyclic loading, which are mainly debonding and friction at matrix/fibre and matrix/matrix interfaces. In addition, damage indicators based on acoustic emission enabled to determine characteristic times which can be used for lifetime forecast. For example, signal severity shows a characteristic time between 25% and 45% of the time to ultimate failure. Detection of this time in real-time during a test can be used to estimate the time of the ultimate failure of the material.

L’hydroxyapatite est l'un des matériaux les plus fréquemment utilisés pour le traitement des maladies des tissus durs. Le zinc est impliqué dans chaque étape du métabolisme du tissu osseux et une carence en zinc peut déterminer l'apparition de l'ostéoporose. Le dopage de l'hydroxyapatite par des ions de zinc peut créer un meilleur matériau, avec des propriétés physico-chimiques supérieures. L'objectif de cette thèse est de créer de nouveaux matériaux biocéramiques avec des propriétés spécifiques qui pourraient permettre le développement de nouvelles applications dans le domaine médical. Une attention particulière a été portée à la caractérisation des propriétés biologiques et physico-chimiques. Dans cette thèse, une nouvelle méthode non destructive de caractérisation de nanoparticules de céramique a été développée. La thèse se compose de six chapitres. Les deux premiers décrivent les biomatériaux et les techniques de caractérisation physico-chimique et ultrasonore utilisées, les trois chapitres suivants présentent des résultats expérimentaux originaux et le dernier chapitre des conclusions générales. La nouveauté de cette étude réside dans la caractérisation de matériaux biocéramiques à base d'hydroxyapatite pour de possibles applications biomédicales. Une nouvelle méthode non destructive de caractérisation par ultrasons est présentée. Ces résultats pourraient contribuer à développer une technique rapide et efficace pour la caractérisation de matériaux céramiques, qui pourrait être utilisée dans le futur en complément des techniques communément utilisées dans le domaine médical, notamment dans le domaine orthopédique. / Hydroxyapatite is one of the most commonly used material used for treating hard tissue diseases. Zinc is involved in each stage of bone tissue metabolism and a lack of it may determine the onset of osteoporosis. Doping hydroxyapatite with Zn ions may cause an improvement of the hydroxyapatite properties, thus resulting a better material, with enhanced physico-chemical properties. Devices based on collagen and hydroxyapatite inhibit the development of bacterial pathogens, reducing the risk of post-surgical infections. The goal of this thesis was to create new bioceramic materials with specific properties which could allow development of new applications in the medical field. Special attention was paid to the characterization of the physico-chemical and biological properties. In this thesis are reported for the first time non-destructive, ultrasonic spectroscopy studies performed on ceramic solutions. The thesis consists of six chapters, the first two comprised of general aspects, the following three chapters present original experimental results and the last chapter presents general conclusions. The novelty of this study lies in the method of synthesis and characterization of bioceramic materials based on hydroxyapatite for possible biomedical applications. Furthermore, a new non-destructive method of characterization techniques based on ultrasounds is presented. The results presented in this study could create a premises of developing a rapid and effective technique for characterization of ceramic materials, which could be used in the future as a complementary technique widely used on different materials used in the medical field, especially in the orthopedic field.

In der gartenbaulichen Forschung gewinnen zerstörungsfreie Produktmonitoringverfahren im Hinblick auf ein verbessertes Prozessmanagement an Bedeutung. Optische Methoden werden bereits in mobilen Systemen und Sortieranlagen zur Produktbewertung in Nachernteprozessen eingesetzt. In der vorliegenden Arbeit wurde ein Beitrag zur quantitativen Bestimmung ernährungsphysiologisch bedeutender Fruchtpolyphenole auf der Basis laser-induzierter Fluoreszenzspektroskopie geleistet. An gelagerten Äpfeln und Möhren wurde die Varianz der Produktfluoreszenz bei verschiedenen Lagerbedingungen mit Hilfe der Hauptkomponentenanalyse ausgewertet, um die Produktentwicklung zerstörungsfrei aufzuzeigen. Für eine angepasste Methode der Datenauswertung wurden hierbei verschiedene Signalvorverarbeitungsmethoden getestet. Die quantitative Bestimmung einzelner Inhaltsstoffe wird in der komplexen pflanzlichen Matrix sowohl beeinflusst durch die Fluoreszenzquantenausbeute als auch Reabsorptions- und Löschungseffekten. Aufbauend auf Untersuchungen an Phenolstandards, Fruchtextrakten und geschnittenem Fruchtgewebe zu Einflussparametern und fluoreszenzspektrokopisch messbaren Konzentrationsbereichen wurden neuere Datenvorverarbeitungsmethoden zur Korrektur angewendet. Kalibriermodelle wurden auf der Basis der fluorimetrisch und chromatographisch ermittelten Werte von Hydroxyzimtsäurederivaten bei Apfel und Erdbeere erarbeitetet und hinsichtlich der Messungenauigkeit in der Kalibrierung und Kreuzvalidierung verglichen. Aufgrund der hohen Variabilität gartenbaulicher Produkte wurden diese Modelle auf einem unabhängigen Datensatz getestet. Mit Hilfe mathematischer orthogonaler Signalkorrektur konnte die für den Polyphenolgehalt nicht relevante Varianz aus den spektralen Daten entfernt und verringerte Kalibrierungs- und Validierungsfehler erzielt werden. Der in der Fluoreszenzanalyse übliche empirische Ansatz mit reflexionskorrigierten Fluoreszenzspektren zu arbeiten führten hingegen zu keiner Fehlerverminderung. / During recent years several research groups focussed on the development of non-destructive product monitoring methods to improve the process management for horticultural products in the entire supply chain. Optical methods have been applied for fruit monitoring in production and postharvest processes using mobile measuring systems or NIR sorting lines. The aim of the present study was to quantitatively determine health promoting native fruit polyphenols by means of laser-induced fluorescence spectroscopy. The variance in the fluorescence signal was detected on apples and carrots stored under different conditions. With the help of principal component analysis the fluorescence spectra were evaluated to visualize senescence effects during storage. Different data pre-processing methods were tested for a descriptive factor analysis regarding the wavelength-dependent intensities as variables. However, in a complex fruit matrix the quantitative determination of fruit compounds is influenced by its fluorescence quantum yield as well as reabsorption and quenching effects. The influence of side-effects was studied in phenol standards, fruit extracts and sliced fruit tissue and spectral data was corrected using new data pre-processing methods.. Calibration models for the polyphenol analyses were built on the fruit fluorescence spectra (apples, strawberries) using the chromatographically analysis of hydroxycinnamic acids as a reference. The uncertainty of the models was evaluated by their root mean squares errors of calibration and cross-validation. The feasibility of the non-destructive analysis in practice is influenced by the high variability of horticultural products. Therefore, the models were validated on an independent test set. The mathematical data pre-processing method of direct orthogonal signal correction removed the non relevant information in the spectral data and resulted in the lowest errors. In comparison, the often applied empirical approach in fluorescence spectroscopy to correct with simultaneously recorded reflectance spectra did not improve the calibration models.