Geochemistry and stratigraphy on sediment cores from Leg198 and Leg 208

The first complete cyclic sedimentary successions for the early Paleogene from drilling multiple holes have been retrieved during two ODP expeditions: Leg 198 (Shatsky Rise, NW Pacific Ocean) and Leg 208 (Walvis Ridge, SE Atlantic Ocean). These new records allow us to construct a comprehensive astronomically calibrated stratigraphic framework with an unprecedented accuracy for both the Atlantic and the Pacific Oceans covering the entire Paleocene epoch based on the identification of the stable long-eccentricity cycle (405-kyr). High resolution X-ray fluorescence (XRF) core scanner and non-destructive core logging data from Sites 1209 through1211 (Leg 198) and Sites 1262, 1267 (Leg 208) are the basis for such a robust chronostratigraphy. Former investigated marine (ODP Sites 1001 and 1051) and land-based (e.g., Zumaia) sections have been integrated as well. The high-fidelity chronology is the prerequisite for deciphering mechanisms in relation to prominent transient climatic events as well as completely new insights into Greenhouse climate variability in the early Paleogene. We demonstrate that the Paleocene epoch covers 24 long eccentricity cycles. We also show that no definite absolute age datums for the K/Pg boundary or the Paleocene - Eocene Thermal Maximum (PETM) can be provided by now, because of still existing uncertainties in orbital solutions and radiometric dating. However, we provide two options for tuning of the Paleocene which are only offset by 405-kyr. Our orbitally calibrated integrated Leg 208 magnetostratigraphy is used to revise the Geomagnetic Polarity Time Scale (GPTS) for Chron C29 to C25. We established a high-resolution calcareous nannofossil biostratigraphy for the South Atlantic which allows a much more detailed relative scaling of stages with biozones. The re-evaluation of the South Atlantic spreading rate model features higher frequent oscillations in spreading rates for magnetochron C28r, C27n, and C26n.

Susceptibility, density, iron and calcium concentrations of ODP holes 165-999B and 165-1001A

Pelagic sediments recording an extreme and short-lived global warming event, the Late Paleocene Thermal Maximum (LPTM), were recovered from Hole 999B (Colombian Basin) and Holes 1001A and 1001B (lower Nicaraguan Rise) in the Caribbean Sea during Ocean Drilling Program Leg 165. The LPTM consists of a 0.3-0.97 m calcareous claystone to claystone horizon. High-resolution downhole logging (Formation MicroScanner [FMS]), standard downhole logs (resistivity, velocity, density, natural gamma ray, and geochemical log), and non-destructive chemical and physical property (multisensor core logger [MSCL] and X-ray fluorescence [XRF] core scanner) data were used to identify composite sections from parallel holes and to record sedimentological and environmental changes associated with the LPTM. Downhole logging data indicate an abrupt and distinct difference in physical and chemical properties that extend for tens of meters above and below the LPTM. These observations indicate a rapid environmental change at the LPTM, which persists beyond the LPTM anomaly. Comparisons of gamma-ray attenuation porosity evaluator (GRAPE) densities from MSCL logging on split cores with FMS resistivity values allows core-to-log correlation with a high degree of accuracy. High-resolution magnetic susceptibility measurements of the cores are compared with elemental concentrations (e.g., Fe, Ca) analyzed by high-resolution XRF scanning. The high-resolution data obtained from several detailed core and downhole logging methods are the key to the construction of composite sections, the correlation of both adjacent holes and distant sites, and core-log integration. These continuous-depth series reveal the LPTM as a multiphase event with a nearly instantaneous onset, followed by a much different set of physical and chemical conditions of short duration, succeeded by a longer transition to a new, more permanent set of environmental circumstances. The estimated duration of these 'phases' are consistent with paleontological and isotopic studies of the LPTM

Density of 9 sediment cores from the Weddell Sea

The wet bulk density is one of the most important parameters of the physical and geological properties of marine sediments. The density is connected directly with sedimentation history and a few sedirnent properties. Knowledge of the fine scale density-depth structure is the base for many model calculations, for both sedimentological and palaeoclimatic research. A density measurement system was designed and built at the Alfred Wegener Institute in Bremerhaven for measuring the wet buk density of sediment cores with high resolution in a non-destructive way. The density is deterrnined by measuring the absorption of Gamma-rays in the sediment. This principle has been used since the 50's in materials research and in the geosciences. In the present case, Cs137 is used as the radioactive source and the intensity is measured by a detector system (scintillator and photomultiplier). Density values are obtainable in both longitudinal core sections and planar cross-sections (the latter are a function of the axial rotation angle). Special studies on inhomogenity can be applied with core rotation. Detection of ice rafted debris (IRD) is made possible with this option. The processes that run the density measurement system are computer controlled. Besides the absorption measurement the core diameter at every measurement point is determined with a potentiometric system. The data values taken are stored on a personal computer. Before starting routine measurements on the sediment cores, a few experiments conceming the statistical aspects of the gamma-ray signal and its accuracy were carried out. These experiments led to such things as the optimum operational parameters. A high spatial resolution in the mm-range is possible with the 4mm-thin gamma-ray measurements. Within five seconds the wet bulk density can be deterrnined with an absolute accuracy of 1%. A comparison between data measured with the new system and conventional measurements on core samples after core splitting shows an agreement within +I- 5% for most of the values. For this thesis, density determinations were carried out on ten sediment cores. A few sediment characteristics are obtainable from using just the standard measurement results without core rotation. In addition to differentes and steps in the absolute density range, variations in the "frequency" of the density-depth structure can be detected due to the close spatial measurement interval and high resolution. Examples from measurements with small (9°) and great (90°) angle increments show that abrupt and smooth transitional changes of sedirnent layers as well as ice rafted debris of several dimensions can be detected and distiflguished clearly. After the presentation of the wet bulk density results, a comparison with data from other investigations was made. Measurements of the electrical resistivity correlated very well with the density data because both parameters are closely related to the porosity of the sedirnent. Additionally, results from measurements of the magnetic susceptibility and from ultra-sonic wave velocity investigations were considered for a integrative interpretation. The correlation of these both parameters and wet bulk density data is strongly dependent on the local (environmental) conditions. Finally, the densities were compared with recordings from sediment-echographic soundings and an X-ray computer tomography analysis. The individual results of all investigations were then finally combined into an accurate picture of the core. Problems of ambiguity, which exist when just one Parameter is determined alone, can be reduced more or less according to the number of parameters and sedimentary characteristics measured. The important role of the density data among other parameters of such an integrated interpretation is evident. Evidence of this role include the high resolution of the measurement, the excellent accuracy and the key position within methods and parameters concerning marine sediments.

Evaluación de la profundidad de la fisuración superficial descendente en pavimentos asfálticos mediante técnicas de ultrasonidos. Validación teórico-práctica y modelos

La fisuración iniciada en la superficie de los pavimentos asfálticos constituye uno de los más frecuentes e importantes modos de deterioro que tienen lugar en los firmes bituminosos, como han demostrado los estudios teóricos y experimentales llevados a cabo en la última década. Sin embargo, este mecanismo de fallo no ha sido considerado por los métodos tradicionales de diseño de estos firmes. El concepto de firmes de larga duración se fundamenta en un adecuado seguimiento del proceso de avance en profundidad de estos deterioros y la intervención en el momento más apropiado para conseguir mantenerlos confinados como fisuras de profundidad parcial en la capa superficial más fácilmente accesible y reparable, de manera que pueda prolongarse la durabilidad y funcionalidad del firme y reducir los costes generalizados de su ciclo de vida. Por lo tanto, para la selección de la estrategia óptima de conservación de los firmes resulta esencial disponer de metodologías que posibiliten la identificación precisa in situ de la fisuración descendente, su seguimiento y control, y que además permitan una determinación fiable y con alto rendimiento de su profundidad y extensión. En esta Tesis Doctoral se presentan los resultados obtenidos mediante la investigación sistemática de laboratorio e in situ llevada a cabo para la obtención de datos sobre fisuración descendente en firmes asfálticos y para el estudio de procedimientos de evaluación de la profundidad de este tipo de fisuras empleando técnicas de ultrasonidos. Dichos resultados han permitido comprobar que la metodología no destructiva propuesta, de rápida ejecución, bajo coste y sencilla implementación (principalmente empleada hasta el momento en estructuras metálicas y de hormigón, debido a las dificultades que introduce la naturaleza viscoelástica de los materiales bituminosos) puede ser aplicada con suficiente fiabilidad y repetibilidad sobre firmes asfálticos. Las medidas resultan asimismo independientes del espesor total del firme. Además, permite resolver algunos de los inconvenientes frecuentes que presentan otros métodos de diagnóstico de las fisuras de pavimentos, tales como la extracción de testigos (sistema destructivo, de alto coste y prolongados tiempos de interrupción del tráfico) o algunas otras técnicas no destructivas como las basadas en medidas de deflexiones o el georradar, las cuales no resultan suficientemente precisas para la investigación de fisuras superficiales. Para ello se han realizado varias campañas de ensayos sobre probetas de laboratorio en las que se han estudiado diferentes condiciones empíricas como, por ejemplo, distintos tipos de mezclas bituminosas en caliente (AC, SMA y PA), espesores de firme y adherencias entre capas, temperaturas, texturas superficiales, materiales de relleno y agua en el interior de las grietas, posición de los sensores y un amplio rango de posibles profundidades de fisura. Los métodos empleados se basan en la realización de varias medidas de velocidad o de tiempo de transmisión del pulso ultrasónico sobre una única cara o superficie accesible del material, de manera que resulte posible obtener un coeficiente de transmisión de la señal (mediciones relativas o autocompensadas). Las mediciones se han realizado a bajas frecuencias de excitación mediante dos equipos de ultrasonidos diferentes dotados, en un caso, de transductores de contacto puntual seco (DPC) y siendo en el otro instrumento de contacto plano a través de un material especialmente seleccionado para el acoplamiento (CPC). Ello ha permitido superar algunos de los tradicionales inconvenientes que presenta el uso de los transductores convencionales y no precisar preparación previa de las superficies. La técnica de autocalibración empleada elimina los errores sistemáticos y la necesidad de una calibración local previa, demostrando el potencial de esta tecnología. Los resultados experimentales han sido comparados con modelos teóricos simplificados que simulan la propagación de las ondas ultrasónicas en estos materiales bituminosos fisurados, los cuales han sido deducidos previamente mediante un planteamiento analítico y han permitido la correcta interpretación de dichos datos empíricos. Posteriormente, estos modelos se han calibrado mediante los resultados de laboratorio, proporcionándose sus expresiones matemáticas generalizadas y gráficas para su uso rutinario en las aplicaciones prácticas. Mediante los ensayos con ultrasonidos efectuados en campañas llevadas a cabo in situ, acompañados de la extracción de testigos del firme, se han podido evaluar los modelos propuestos. El máximo error relativo promedio en la estimación de la profundidad de las fisuras al aplicar dichos modelos no ha superado el 13%, con un nivel de confianza del 95%, en el conjunto de todos los ensayos realizados. La comprobación in situ de los modelos ha permitido establecer los criterios y las necesarias recomendaciones para su utilización sobre firmes en servicio. La experiencia obtenida posibilita la integración de esta metodología entre las técnicas de auscultación para la gestión de su conservación. Abstract Surface-initiated cracking of asphalt pavements constitutes one of the most frequent and important types of distress that occur in flexible bituminous pavements, as clearly has been demonstrated in the technical and experimental studies done over the past decade. However, this failure mechanism has not been taken into consideration for traditional methods of flexible pavement design. The concept of long-lasting pavements is based on adequate monitoring of the depth and extent of these deteriorations and on intervention at the most appropriate moment so as to contain them in the surface layer in the form of easily-accessible and repairable partial-depth topdown cracks, thereby prolonging the durability and serviceability of the pavement and reducing the overall cost of its life cycle. Therefore, to select the optimal maintenance strategy for perpetual pavements, it becomes essential to have access to methodologies that enable precise on-site identification, monitoring and control of top-down propagated cracks and that also permit a reliable, high-performance determination of the extent and depth of cracking. This PhD Thesis presents the results of systematic laboratory and in situ research carried out to obtain information about top-down cracking in asphalt pavements and to study methods of depth evaluation of this type of cracking using ultrasonic techniques. These results have demonstrated that the proposed non-destructive methodology –cost-effective, fast and easy-to-implement– (mainly used to date for concrete and metal structures, due to the difficulties caused by the viscoelastic nature of bituminous materials) can be applied with sufficient reliability and repeatability to asphalt pavements. Measurements are also independent of the asphalt thickness. Furthermore, it resolves some of the common inconveniences presented by other methods used to evaluate pavement cracking, such as core extraction (a destructive and expensive procedure that requires prolonged traffic interruptions) and other non-destructive techniques, such as those based on deflection measurements or ground-penetrating radar, which are not sufficiently precise to measure surface cracks. To obtain these results, extensive tests were performed on laboratory specimens. Different empirical conditions were studied, such as various types of hot bituminous mixtures (AC, SMA and PA), differing thicknesses of asphalt and adhesions between layers, varied temperatures, surface textures, filling materials and water within the crack, different sensor positions, as well as an ample range of possible crack depths. The methods employed in the study are based on a series of measurements of ultrasonic pulse velocities or transmission times over a single accessible side or surface of the material that make it possible to obtain a signal transmission coefficient (relative or auto-calibrated readings). Measurements were taken at low frequencies by two short-pulse ultrasonic devices: one equipped with dry point contact transducers (DPC) and the other with flat contact transducers that require a specially-selected coupling material (CPC). In this way, some of the traditional inconveniences presented by the use of conventional transducers were overcome and a prior preparation of the surfaces was not required. The auto-compensating technique eliminated systematic errors and the need for previous local calibration, demonstrating the potential for this technology. The experimental results have been compared with simplified theoretical models that simulate ultrasonic wave propagation in cracked bituminous materials, which had been previously deduced using an analytical approach and have permitted the correct interpretation of the aforementioned empirical results. These models were subsequently calibrated using the laboratory results, providing generalized mathematical expressions and graphics for routine use in practical applications. Through a series of on-site ultrasound test campaigns, accompanied by asphalt core extraction, it was possible to evaluate the proposed models, with differences between predicted crack depths and those measured in situ lower than 13% (with a confidence level of 95%). Thereby, the criteria and the necessary recommendations for their implementation on in-service asphalt pavements have been established. The experience obtained through this study makes it possible to integrate this methodology into the evaluation techniques for pavement management systems.

Evaluation of the influence of visual parameters on wave transmission velocity in sawn chestnut timber

Non-destructive, visual evaluation and mechanical testing techniques were used to assess the structural properties of 374 samples of chestnut (Castanea sativa). The principal components method was applied to establish and interpret correlations between variables obtained of modulus of elasticity, bending strength and density. The static modulus of elasticity presented higher correlation values than those obtained using non-destructive methods. Bending strength presented low correlations with the non-destructive parameters, but there was some relation to the different knot ratios defined. The relationship was stronger with the most widely used ratio, CKDR. No significant correlations were observed between any of the variables and density.

Thermal diffusion profile by NRA of Deuterium implanted in solid breeder blanket materials

This paper studies the relationship between aging, physical changes and the results of non-destructive testing of plywood. 176 pieces of plywood were tested to analyze their actual and estimated density using non-destructive methods (screw withdrawal force and ultrasound wave velocity) during a laboratory aging test. From the results of statistical analysis it can be concluded that there is a strong relationship between the non-destructive measurements carried out, and the decline in the physical properties of the panels due to aging. The authors propose several models to estimate board density. The best results are obtained with ultrasound. A reliable prediction of the degree of deterioration (aging) of board is presented. Breeder blanket materials have to produce tritium from lithium while fulfilling several strict conditions. In particular, when dealing with materials to be applied in fusion reactors, one of the key questions is the study of light ions retention, which can be produced by transmutation reactions and/or introduced by interaction with the plasma. In ceramic breeders the understanding of the hydrogen isotopes behaviour and specially the diffusion of tritium to the surface is crucial. Moreover the evolution of the microstructure during irradiation with energetic ions, neutrons and electrons is complex because of the interaction of a high number of processes.

Mealiness assessment in apples and peaches using MRI techniques.

Since Januarv 1946 a wade EC Project entitled "Mealiness in fruits Consumers perception and means for detection is being carried out. Mealiness is a sensory attribute that cannot be defined by a single parameter but through a combination of variables (multidimensional structure) Previous studies propose the definition of mealiness as the lack of crispiness of hardness and of juiciness. A destructive instrumental procedure combined with a integration technique has been already developed enabling to identify mealy fruits by destructive instrumental means use other contributions of Barreiro and Ortiz to this Ag Eng 98. Current aims .are focused on establishing non destructive tests for mealiness assessment. Magnetic resonance Imaging (MRI) makes use of the magnetic properties that some atomic nuclei have. especially hidrogen nuclei from water molecules to obtain high quality images in the field of internal quality evaluation the MRI has been used to assess internal injury due to conservation as o treatments as chilling injury un Persimmons Clark&Forbes (1994) and water-core in apples (Wang et al. 1998. In the case of persimmons the chilling injury is described as an initial tissue breakdown and lack of cohesion between cells followed by formation of a firm gel and by a lack of juiciness without changes in the total amount ol water content. Also a browning of the flesh is indicated (Clark&Forhes 1994). This definition fits into the previous description of mealiness.

Integrated Studies for the Evaluation of Conservation Treatments on Stone Material from Archaeological Sites. Application to the Case of Merida (Spain)

The application of conservation treatments, such as consolidation and protection ones, has been demonstrated ineffective in many cases, and even harmful. Evaluation studies should be a mandatory task, ideally before and after the intervention, but both tasks are complex and unusual in the case of archaeological heritage. This study is mainly focused on analyzing changes in petrophysical properties of stone material from archaeological sites of Merida (Spain), evaluating, both on site and in laboratory, effects derived from different conservation treatments applied in past interventions, throughout the integration of different non-destructive techniques (NDT) and portable devices of analysis available at the Institute of Geosciences (CSIC,UCM). These techniques allow, not only assessment of effectiveness and alteration processes, but also monitoring durability of treatments, focused mainly on 1996 intervention in the case of Roman Theater, as well as different punctual interventions from the 90’s until date in the House of Mitreo. Studies carried out on archaeological sites of Merida permit us to compare outcomes and also check limitations in the use of those equipments. In this paper we discuss about the use of some techniques, their integration and limits, for the assessment of conservation treatments, showing some examples of Merida’s case study.

Fatiga en CFRP: Caracterización y Método Óptico para la Estimación del Daño

El desarrollo de nuevas estructuras aeroespaciales optimizadas, utilizan materiales compuestos, para los componentes críticos y subsistemas, principalmente polímeros reforzados con fibra de carbono (CFRP). Un conocimiento profundo del estado de daño por fatiga de estructuras de CFRP avanzado, es esencial para predecir la vida residual y optimizar los intervalos de inspección estructural, reparaciones y/o sustitución de componentes. Las técnicas actuales se basan principalmente en la medición de cargas estructurales a lo largo de la vida útil de la estructura mediante galgas extensométricas eléctricas. Con esos datos, se estima la vida a fatiga utilizando modelos de acumulación de daño. En la presente tesis, se evalúa la metodología convencional para la estimación de la vida a fatiga de un CFRP aeronáutico. Esta metodología está basada en la regla de acumulación de daño lineal de Palmgren-Miner, y es aplicada para determinar la vida a fatiga de estructuras sometidas a cargas de amplitud variable. Se ha realizado una campaña de ensayos con cargas de amplitud constante para caracterizar un CFRP aeronáutico a fatiga, obteniendo las curvas clásicas S-N, en diferentes relaciones de esfuerzo. Se determinaron los diagramas de vida constante, (CLD), también conocidos como diagramas de Goodman, utilizando redes neuronales artificiales debido a la ausencia de modelos coherentes para materiales compuestos. Se ha caracterizado la degradación de la rigidez debido al daño por fatiga. Se ha ensayado un segundo grupo de probetas con secuencias estandarizadas de cargas de amplitud variable, para obtener la vida a fatiga y la degradación de rigidez en condiciones realistas. Las cargas aplicadas son representativas de misiones de aviones de combate (Falstaff), y de aviones de transporte (Twist). La vida a fatiga de las probetas cicladas con cargas de amplitud variable, se comparó con el índice de daño teórico calculado en base a la regla de acumulación de daño lineal convencional. Los resultados obtenidos muestran predicciones no conservativas. Esta tesis también presenta el estudio y desarrollo, de una nueva técnica de no contacto para evaluar el estado de daño por fatiga de estructuras de CFRP por medio de cambios de los parámetros de rugosidad. La rugosidad superficial se puede medir fácilmente en campo con métodos sin contacto, mediante técnicas ópticas tales como speckle y perfilómetros ópticos. En el presente estudio, se han medido parámetros de rugosidad superficial, y el factor de irregularidad de la superficie, a lo largo de la vida de las probetas cicladas con cargas de amplitud constante y variable, Se ha obtenido una buena tendencia de ajuste al correlacionar la magnitud de la rugosidad y el factor de irregularidad de la superficie con la degradación de la rigidez de las probetas fatigadas. Estos resultados sugieren que los cambios en la rugosidad superficial medida en zonas estratégicas de componentes y estructuras hechas de CFRP, podrían ser indicativas del nivel de daño interno debido a cargas de fatiga. Los resultados también sugieren que el método es independiente del tipo de carga de fatiga que ha causado el daño. Esto último hace que esta técnica de medición sea aplicable como inspección para una amplia gama de estructuras de materiales compuestos, desde tanques presurizados con cargas de amplitud constante, estructuras aeronáuticas como alas y colas de aeronaves cicladas con cargas de amplitud variable, hasta aplicaciones industriales como automoción, entre otros. ABSTRACT New optimized aerospace structures use composite materials, mainly carbon fiber reinforced polymer composite (CFRP), for critical components and subsystems. A strong knowledge of the fatigue state of highly advanced (CFRP) structures is essential to predict the residual life and optimize intervals of structural inspection, repairs, and/or replacements. Current techniques are based mostly on measurement of structural loads throughout the service life by electric strain gauge sensors. These sensors are affected by extreme environmental conditions and by fatigue loads in such a way that the sensors and their systems require exhaustive maintenance throughout system life. In the present thesis, the conventional methodology based on linear damage accumulation rules, applied to determine the fatigue life of structures subjected to variable amplitude loads was evaluated for an aeronautical CFRP. A test program with constant amplitude loads has been performed to obtain the classical S-N curves at different stress ratios. Constant life diagrams, CLDs, where determined by means of Artificial Neural Networks due to the absence of consistent models for composites. The stiffness degradation due to fatigue damage has been characterized for coupons under cyclic tensile loads. A second group of coupons have been tested until failure with a standardized sequence of variable amplitude loads, representative of missions for combat aircraft (Falstaff), and representative of commercial flights (Twist), to obtain the fatigue life and the stiffness degradation under realistic conditions. The fatigue life of the coupons cycled with variable amplitude loads were compared to the theoretical damage index calculated based on the conventional linear damage accumulation rule. The obtained results show non-conservative predictions. This thesis also presents the evaluation of a new non-contact technique to evaluate the fatigue damage state of CFRP structures by means of measuring roughness parameters to evaluate changes in the surface topography. Surface roughness can be measured easily on field with non-contact methods by optical techniques such as speckle and optical perfilometers. In the present study, surface roughness parameters, and the surface irregularity factor, have been measured along the life of the coupons cycled with constant and variable amplitude loads of different magnitude. A good agreement has been obtained when correlating the magnitude of the roughness and the surface irregularity factor with the stiffness degradation. These results suggest that the changes on the surface roughness measured in strategic zones of components and structures made of CFRP, could be indicative of the level of internal damage due to fatigue loads. The results also suggest that the method is independent of the type of fatigue load that have caused the damage. It makes this measurement technique applicable for a wide range of inspections of composite materials structures, from pressurized tanks with constant amplitude loads, to variable amplitude loaded aeronautical structures like wings and empennages, up to automotive and other industrial applications.

Determining the elastic-plastic properties of metallic materials through instrumented indentation

En los últimos años, y asociado al desarrollo de la tecnología MEMS, la técnica de indentación instrumentada se ha convertido en un método de ensayo no destructivo ampliamente utilizado para hallar las características elástico-plásticas de recubrimientos y capas delgadas, desde la escala macroscópica a la microscópica. Sin embargo, debido al complejo mecanismo de contacto debajo de la indentación, es urgente proponer un método más simple y conveniente para obtener unos resultados comparables con otras mediciones tradicionales. En este estudio, el objetivo es mejorar el procedimiento analítico para extraer las propiedades elástico-plásticas del material mediante la técnica de indentación instrumentada. La primera parte se centra en la metodología llevada a cabo para medir las propiedades elásticas de los materiales elásticos, presentándose una nueva metodología de indentación, basada en la evolución de la rigidez de contacto y en la curva fuerza-desplazamiento del ensayo de indentación. El método propuesto permite discriminar los valores de indentación experimental que pudieran estar afectados por el redondeo de la punta del indentador. Además, esta técnica parece ser robusta y permite obtener valores fiables del modulo elástico. La segunda parte se centra en el proceso analítico para determinar la curva tensión-deformación a partir del ensayo de indentación, empleando un indentador esférico. Para poder asemejar la curva tension-deformación de indentación con la que se obtendría de un ensayo de tracción, Tabor determinó empíricamente un factor de constricción de la tensión () y un factor de constricción de la deformación (). Sin embargo, la elección del valor de y  necesitan una derivación analítica. Se describió analíticamente una nueva visión de la relación entre los factores de constricción de tensión y la deformación basado en la deducción de la ecuación de Tabor. Un modelo de elementos finitos y un diseño experimental se realizan para evaluar estos factores de constricción. A partir de los resultados obtenidos, las curvas tension-deformación extraidas de los ensayos de indentación esférica, afectadas por los correspondientes factores de constricción de tension y deformación, se ajustaron a la curva nominal tensión-deformación obtenida de ensayos de tracción convencionales. En la última parte, se estudian las propiedades del revestimiento de cermet Inconel 625-Cr3C2 que es depositado en el medio de una aleación de acero mediante un láser. Las propiedades mecánicas de la matriz de cermet son estudiadas mediante la técnica de indentación instrumentada, haciendo uso de las metodologías propuestas en el presente trabajo. In recent years, along with the development of MEMS technology, instrumented indentation, as one type of a non-destructive measurement technique, is widely used to characterize the elastic and plastic properties of metallic materials from the macro to the micro scale. However, due to the complex contact mechanisms under the indentation tip, it is necessary to propose a more convenient and simple method of instrumented indention to obtain comparable results from other conventional measurements. In this study, the aim is to improve the analytical procedure for extracting the elastic plastic properties of metallic materials by instrumented indentation. The first part focuses on the methodology for measuring the elastic properties of metallic materials. An alternative instrumented indentation methodology is presented. Based on the evolution of the contact stiffness and indentation load versus the depth of penetration, the possibility of obtaining the actual elastic modulus of an elastic-plastic bulk material through instrumented sharp indentation tests has been explored. The proposed methodology allows correcting the effect of the rounding of the indenter tip on the experimental indentation data. Additionally, this technique does not seem too sensitive to the pile-up phenomenon and allows obtaining convincing values of the elastic modulus. In the second part, an analytical procedure is proposed to determine the representative stress-strain curve from the spherical indentation. Tabor has determined the stress constraint factor (stress CF), and strain constraint factor (strain CF), empirically but the choice of a value for and is debatable and lacks analytical derivation. A new insight into the relationship between stress and strain constraint factors is analytically described based on the formulation of Tabor’s equation. Finite element model and experimental tests have been carried out to evaluate these constraint factors. From the results, representative stress-strain curves using the proposed strain constraint factor fit better with the nominal stress-strain curve than those using Tabor’s constraint factors. In the last part, the mechanical properties of an Inconel 625-Cr3C2 cermet coating which is deposited onto a medium alloy steel by laser cladding has been studied. The elastic and plastic mechanical properties of the cermet matrix are studied using depth-sensing indentation (DSI) on the micro scale.

In silico identification and characterisation of 17 polymorphic anonymous non-coding sequence markers (ANMs) for red grouse (Lagopus lagopus scotica)

Peer reviewed

Synthesis and Characterisation of Functional Magnetic and Plasmonic Nanomaterials

The main aim of this thesis is the controlled and reproducible synthesis of functional materials at the nanoscale. In the first chapter, a tuning of morphology and magnetic properties of magnetite nanoparticles is presented. It was achieved by an innovative approach, which involves the use of an organic macrocycle (calixarene) to induce the oriented aggregation of NPs during the synthesis. This method is potentially applicable to the preparation of other metal oxide NPs by thermal decomposition of the respective precursors. Products obtained, in particular the multi-core nanoparticles, show remarkable magnetic and colloidal properties, making them very interesting for biomedical applications. The synthesis and functionalisation of plasmonic Au and Ag nanoparticles is presented in the second chapter. Here, a supramolecular approach was exploited to achieve a controlled and potentially reversible aggregation between Au and Ag NPs. This aggregation phenomena was followed by UV - visible spectroscopy and dynamic light scattering. In the final chapters, the conjugation of plasmonic and magnetic functionalities was tackled through the preparation of dimeric nanostructures. Au - Fe oxide heterodimeric nanoparticles were prepared and their magnetic properties thoroughly characterised. The results demonstrate the formation of FeO (wustite), together with magnetite, during the thermal decomposition of the iron precursor. By an oxidation process that preserves Au in the dimeric structures, wustite completely disappeared, with the formation of either magnetite and / or maghemite, much better from the magnetic point of view. The plasmon resonance of Au results damped by the presence of the iron oxide, a material with high refractive index, but it is still present if the Au domain of the nanoparticles is exposed towards the bulk. Finally, remarkable hyperthermia, also in vitro, was found for these structures.