Stranski-Krastanov InN/InGaN quantum dots grown directly on Si(111)

The authors discuss and demonstrate the growth of InN surface quantum dots on a high-In-content In0.73Ga0.27N layer, directly on a Si(111) substrate by plasma-assisted molecular beam epitaxy. Atomic force microscopy and transmission electron microscopy reveal uniformly distributed quantum dots with diameters of 10–40 nm, heights of 2–4 nm, and a relatively low density of ∼7 × 109 cm−2. A thin InN wetting layer below the quantum dots proves the Stranski-Krastanov growth mode. Near-field scanning optical microscopy shows distinct and spatially well localized near-infrared emission from single surface quantum dots. This holds promise for future telecommunication and sensing devices.

Reduction of truncation errors in planar, cylindrical and partial spherical near-field antenna measurements

A method to reduce truncation errors in near-field antenna measurements is presented. The method is based on the Gerchberg-Papoulis iterative algorithm used to extrapolate band-limited functions and it is able to extend the valid region of the calculated far-field pattern up to the whole forward hemisphere. The extension of the valid region is achieved by the iterative application of a transformation between two different domains. After each transformation, a filtering process that is based on known information at each domain is applied. The first domain is the spectral domain in which the plane wave spectrum (PWS) is reliable only within a known region. The second domain is the field distribution over the antenna under test (AUT) plane in which the desired field is assumed to be concentrated on the antenna aperture. The method can be applied to any scanning geometry, but in this paper, only the planar, cylindrical, and partial spherical near-field measurements are considered. Several simulation and measurement examples are presented to verify the effectiveness of the method.

Near-field light focusing by wavelength-sized dielectric spheroids for photovoltaic applications

We explore the near-field concentration properties of dielectric spheroidal scatterers with sizes close to the wavelength, using an analytical separation-of-variables method. Such particles act as mesoscopic lenses whose physical parameters are optimized here for maximum scattered light enhancement in photovoltaic applications.

Novel method to improve the signal-to-noise ratio in the far-field results obtained from planar near-field measurements

A method to reduce the noise power in far-field pattern without modifying the desired signal is proposed. Therefore, an important signal-to-noise ratio improvement may be achieved. The method is used when the antenna measurement is performed in planar near-field, where the recorded data are assumed to be corrupted with white Gaussian and space-stationary noise, because of the receiver additive noise. Back-propagating the measured field from the scan plane to the antenna under test (AUT) plane, the noise remains white Gaussian and space-stationary, whereas the desired field is theoretically concentrated in the aperture antenna. Thanks to this fact, a spatial filtering may be applied, cancelling the field which is located out of the AUT dimensions and which is only composed by noise. Next, a planar field to far-field transformation is carried out, achieving a great improvement compared to the pattern obtained directly from the measurement. To verify the effectiveness of the method, two examples will be presented using both simulated and measured near-field data.

Desarrollo de estructuras nanofotonicas de campo cercano para intensificacion localizada de luz en celulas solares de banda intermedia - Near-field nanophotonic structures for localized light enhancement in intermediate band solar cells

This doctoral thesis explores some of the possibilities that near-field optics can bring to photovoltaics, and in particular to quantum-dot intermediate band solar cells (QD-IBSCs). Our main focus is the analytical optimization of the electric field distribution produced in the vicinity of single scattering particles, in order to produce the highest possible absorption enhancement in the photovoltaic medium in their surroundings. Near-field scattering structures have also been fabricated in laboratory, allowing the application of the previously studied theoretical concepts to real devices. We start by looking into the electrostatic scattering regime, which is only applicable to sub-wavelength sized particles. In this regime it was found that metallic nano-spheroids can produce absorption enhancements of about two orders of magnitude on the material in their vicinity, due to their strong plasmonic resonance. The frequency of such resonance can be tuned with the shape of the particles, allowing us to match it with the optimal transition energies of the intermediate band material. Since these metallic nanoparticles (MNPs) are to be inserted inside the cell photovoltaic medium, they should be coated by a thin insulating layer to prevent electron-hole recombination at their surface. This analysis is then generalized, using an analytical separation-of-variables method implemented in Mathematica7.0, to compute scattering by spheroids of any size and material. This code allowed the study of the scattering properties of wavelengthsized particles (mesoscopic regime), and it was verified that in this regime dielectric spheroids perform better than metallic. The light intensity scattered from such dielectric spheroids can have more than two orders of magnitude than the incident intensity, and the focal region in front of the particle can be shaped in several ways by changing the particle geometry and/or material. Experimental work was also performed in this PhD to implement in practice the concepts studied in the analysis of sub-wavelength MNPs. A wet-coating method was developed to self-assemble regular arrays of colloidal MNPs on the surface of several materials, such as silicon wafers, amorphous silicon films, gallium arsenide and glass. A series of thermal and chemical tests have been performed showing what treatments the nanoparticles can withstand for their embedment in a photovoltaic medium. MNPs arrays are then inserted in an amorphous silicon medium to study the effect of their plasmonic near-field enhancement on the absorption spectrum of the material. The self-assembled arrays of MNPs constructed in these experiments inspired a new strategy for fabricating IBSCs using colloidal quantum dots (CQDs). Such CQDs can be deposited in self-assembled monolayers, using procedures similar to those developed for the patterning of colloidal MNPs. The use of CQDs to form the intermediate band presents several important practical and physical advantages relative to the conventional dots epitaxially grown by the Stranski-Krastanov method. Besides, this provides a fast and inexpensive method for patterning binary arrays of QDs and MNPs, envisioned in the theoretical part of this thesis, in which the MNPs act as antennas focusing the light in the QDs and therefore boosting their absorption

A New Method to Reduce Truncation Errors in Partial Spherical Near-Field Measurements

A new and effective method for reduction of truncation errors in partial spherical near-field (SNF) measurements is proposed. The method is useful when measuring electrically large antennas, where the measurement time with the classical SNF technique is prohibitively long and an acquisition over the whole spherical surface is not practical. Therefore, to reduce the data acquisition time, partial sphere measurement is usually made, taking samples over a portion of the spherical surface in the direction of the main beam. But in this case, the radiation pattern is not known outside the measured angular sector as well as a truncation error is present in the calculated far-field pattern within this sector. The method is based on the Gerchberg-Papoulis algorithm used to extrapolate functions and it is able to extend the valid region of the calculated far-field pattern up to the whole forward hemisphere. To verify the effectiveness of the method, several examples are presented using both simulated and measured truncated near-field data.

New methods to reduce leakage errors in planar near-field measurements

This paper describes two methods to cancel the effect of two kinds of leakage signals which may be presented when an antenna is measured in a planar near-field range. One method tries to reduce leakage bias errors from the receiver¿s quadrature detector and it is based on estimating the bias constant added to every near-field data sample. Then, that constant is subtracted from the data, removing its undesired effect on the far-field pattern. The estimation is performed by back-propagating the field from the scan plane to the antenna under test plane (AUT) and averaging all the data located outside the AUT aperture. The second method is able to cancel the effect of the leakage from faulty transmission lines, connectors or rotary joints. The basis of this method is also a reconstruction process to determine the field distribution on the AUT plane. Once this distribution is known, a spatial filtering is applied to cancel the contribution due to those faulty elements. After that, a near-field-to-far-field transformation is applied, obtaining a new radiation pattern where the leakage effects have disappeared. To verify the effectiveness of both methods, several examples are presented.

Prediction of near field overpressure from quarry blasting

This paper investigates the propagation of airblast or pressure waves in air produced by bench blasting (i.e. detonation of the explosive in a row of blastholes, breaking the burden of rock towards the free vertical face of the block). Peak overpressure is calculated as a function of blasting parameters (explosive mass per delay and velocity at which the detonation sequence proceeds along the bench) and the polar coordinates of the position of interest (distance to the source and azimuth with respect to the free face). The model has been fitted to empirical data using linear least squares. The data set is composed of 122 airblast records monitored at distances less than 400 m in 41 production blasts carried out in two quarries. The model is statistically significant and has a determination coefficient of 0.87. The formula is validated from 12 airblast measurements gathered in five additional blasts.

Methods for noise reduction in far-field patterns obtained from cylindrical near-field antenna measurements

Two different methods to reduce the noise power in the far-field pattern of an antenna as measured in cylindrical near-field (CNF) are proposed. Both methods are based on the same principle: the data recorded in the CNF measurement, assumed to be corrupted by white Gaussian and space-stationary noise, are transformed into a new domain where it is possible to filter out a portion of noise. Those filtered data are then used to calculate a far-field pattern with less noise power than that one obtained from the measured data without applying any filtering. Statistical analyses are carried out to deduce the expressions of the signal-to-noise ratio improvement achieved with each method. Although the idea of the two alternatives is the same, there are important differences between them. The first one applies a modal filtering, requires an oversampling and improves the far-field pattern in all directions. The second method employs a spatial filtering on the antenna plane, does not require oversampling and the far-field pattern is only improved in the forward hemisphere. Several examples are presented using both simulated and measured near-field data to verify the effectiveness of the methods.

Application of postprocessing techniques methods for noise reduction in cylindrical near field antenna measurements

Three different methods to reduce the noise power in the far-field pattern of an antenna when it is measured in a cylindrical near field system are presented and compared. The first one is based on a modal filtering while the other two are based on spatial filtering, either on an antenna plane or either on a cylinder of smaller radius. Simulated and measured results will be presented.

Analysis of the modified optical properties and band structure of GaAs12xSbx-capped InAs/GaAs quantum dots

The origin of the modified optical properties of InAs/GaAs quantum dots (QD) capped with a thin GaAs1−xSbx layer is analyzed in terms of the band structure. To do so, the size, shape, and composition of the QDs and capping layer are determined through cross-sectional scanning tunnelling microscopy and used as input parameters in an 8 × 8 k·p model. As the Sb content is increased, there are two competing effects determining carrier confinement and the oscillator strength: the increased QD height and reduced strain on one side and the reduced QD-capping layer valence band offset on the other. Nevertheless, the observed evolution of the photoluminescence (PL) intensity with Sb cannot be explained in terms of the oscillator strength between ground states, which decreases dramatically for Sb > 16%, where the band alignment becomes type II with the hole wavefunction localized outside the QD in the capping layer. Contrary to this behaviour, the PL intensity in the type II QDs is similar (at 15 K) or even larger (at room temperature) than in the type I Sb-free reference QDs. This indicates that the PL efficiency is dominated by carrier dynamics, which is altered by the presence of the GaAsSb capping layer. In particular, the presence of Sb leads to an enhanced PL thermal stability. From the comparison between the activation energies for thermal quenching of the PL and the modelled band structure, the main carrier escape mechanisms are suggested. In standard GaAs-capped QDs, escape of both electrons and holes to the GaAs barrier is the main PL quenching mechanism. For small-moderate Sb (<16%) for which the type I band alignment is kept, electrons escape to the GaAs barrier and holes escape to the GaAsSb capping layer, where redistribution and retraping processes can take place. For Sb contents above 16% (type-II region), holes remain in the GaAsSb layer and the escape of electrons from the QD to the GaAs barrier is most likely the dominant PL quenching mechanism. This means that electrons and holes behave dynamically as uncorrelated pairs in both the type-I and type-II structures.

Laser shock peening without absorbent coating (LSPwC) effect on 3D surface topography and mechanical properties of 6082-T651 Al alloy

The influence of nanosecond laser pulses applied by laser shock peening without absorbent coating (LSPwC) with a Q-switched Nd:YAG laser operating at a wavelength of λ = 1064 nm on 6082-T651 Al alloy has been investigated. The first portion of the present study assesses laser shock peening effect at two pulse densities on three-dimensional (3D) surface topography characteristics. In the second part of the study, the peening effect on surface texture orientation and micro-structure modification, i.e. the effect of surface craters due to plasma and shock waves, were investigated in both longitudinal (L) and transverse (T) directions of the laser-beam movement. In the final portion of the study, the changes of mechanical properties were evaluated with a residual stress profile and Vickers micro-hardness through depth variation in the near surface layer, whereas factorial design with a response surface methodology (RSM) was applied. The surface topographic and micro-structural effect of laser shock peening were characterised with optical microscopy, InfiniteFocus® microscopy and scanning electron microscopy (SEM). Residual stress evaluation based on a hole-drilling integral method confirmed higher compression at the near surface layer (33 μm) in the transverse direction (σmin) of laser-beam movement, i.e. − 407 ± 81 MPa and − 346 ± 124 MPa, after 900 and 2500 pulses/cm2, respectively. Moreover, RSM analysis of micro-hardness through depth distribution confirmed an increase at both pulse densities, whereas LSPwC-generated shock waves showed the impact effect of up to 800 μm below the surface. Furthermore, ANOVA results confirmed the insignificant influence of LSPwC treatment direction on micro-hardness distribution indicating essentially homogeneous conditions, in both L and T directions.

Estudio de los materiales que componen el sistema constructivo de las viviendas del casco histórico de Maracaibo (Venezuela)

En este trabajo de investigación que se presenta para optar al grado de Doctor, se analizan y estudian los materiales que conforman las viviendas de mampostería de arenisca “Piedra de Ojo” del casco histórico de Maracaibo, Venezuela, construidas en el siglo XIX. No existe una bibliografía descriptiva técnico-constructiva del sistema constructivo, por lo que esta tesis complementa la escasa descripción estilística existente donde apenas se mencionan algunos materiales de construcción. Definido el marco histórico y las manzanas del área en donde se encontraban las viviendas preseleccionadas a estudiar, en la visita de campo se seleccionaron 12 que se encontraban en estado de deterioro, y que permitieron recolectar las muestras más fácilmente. Para realizar la caracterización y comportamientos de los diferentes materiales utilizados: piedra y morteros en los cerramientos, maderas en armaduras de tejados, techos y carpintería de puertas y ventanas, cerámicos en muros y acabados, etc. Para complementar lo antes dicho se ha dividido esta tesis en seis capítulos: En el capítulo I se desarrolla el estado del arte a nivel nacional e internacional de trabajos de investigación, similares. Se aborda la memoria histórica, que es una reseña de la evolución de la vivienda en la ciudad de Maracaibo. En el capítulo II se describe la metodología empleada en la tesis, de acuerdo a los objetivos, tanto generales como específicos de la investigación. Que ha cubierto diferentes frentes: consulta bibliográfica, levantamiento planimétrico, toma de muestras, análisis de visu, caracterización físico-química y correlación de resultados. Se ha desarrollado el trabajo tanto in situ como en laboratorio y despacho. El capítulo III presenta la caracterización de la arenisca “Piedra de Ojo”, se desarrolla: la descripción geológica y caracterización petrológica. Se reseñan los ensayos realizados en laboratorio como: caracterización de visu, caracterización petrográfica, estudio petrográfico por microcopia óptica de trasmisión, estudio petrográfico por microcopia electrónica de barrido, microscopia electrónica de barrido en modo electrones secundarios (SSE) y microscopia electrónica de barrido en modo electrones retrodispersados. También las propiedades escalares de los mampuestos y los siguientes valores: densidades, porosidades y resistencia mecánicas, entre otros. En el capítulo IV se analizan las características de los morteros aplicados en las viviendas, y la patología o lesiones que presentan. Se clasifican en tres tipos: mortero de junta o asiento, de enfoscado y revoco. Se documenta la realización de los ensayos físicos y químicos, resistencia mecánica y de granulometría; se explican sus componentes principales: conglomerante de cal, áridos y aditivos y la tecnología de fabricación, así como las características físicas, hídricas, químicas y granulométricas. El capítulo V, contiene las aplicaciones constructivas de los materiales de albañilería, Se describen otros elementos de la vivienda como; cimentaciones, muros mixtos, molduras, apliques y pinturas y finalmente pavimentos. Y en el capítulo VI se analizan las especies de madera más representativas usadas en las armaduras de las cubiertas, así como los elementos de cubrición. De igual forma se describe la carpintería de puertas y ventanas, así como sus dinteles o cargaderos de madera y se realiza la identificación anatómica, las propiedades físicas y mecánicas de las utilizadas. Entre los resultados y conclusiones se determinó que el 90% de los materiales utilizados en su construcción proceden de zonas cercanas a la construcción de la vivienda, como la formación El Milagro convertida en cantera de piedra y que el resto de los materiales provenían de la Isla de Toas y de la exportación de las islas del Caribe y de Europa como el cemento. El principal aporte de esta investigación es el análisis técnico constructivo y la caracterización física, mecánica y química de los materiales de la vivienda, con el fin de que dicha información sea usada para definir los materiales nuevos a utilizar en las restauraciones de las viviendas y en futuras líneas de investigación. ABSTRACT In this research paper submitted to opt to the degree of Doctor, the materials that make the “Piedra de Ojo” sandstone masonry houses of the historical center of Maracaibo, Venezuela, built in the XIX century, are analyzed and studied. There exists no technical-constructive descriptive literature of the constructive system, so this thesis complements the very limited existing stylistic description, where barely some construction materials are mentioned. With the historical context and the blocks of the area where the preselected houses to be studied being defined, 12 of these houses that were in a state of decay (deterioration) were selected and this condition allowed to collect samples more easily, in order to carry out the characterization and behavior of the different materials used: stone and mortars in the walls, wood trusses in roofs, ceilings and woodwork of doors and windows, walls and ceramic finishes, etc. To complement the foregoing, this thesis has been divided in six chapters: In Chapter I, the state of art at national and international levels of similar research is developed, which is a review of the evolution of housing in the city of Maracaibo. In Chapter II, the methodology used in the thesis is described, according to the research’s objectives, general and specific ones, which have covered several fronts: literature survey, planimetric survey, sampling, visu analysis, physical-chemical characterization and correlation of results. Chapter III presents the characterization of the “Piedra de Ojo” sandstone; geological description and petrologic characterization are developed. Essays performed in the laboratory are reviewed, such as: visu characterization, petrographic characaterization, petrographic study by optical microscopy of transmission, petrographic study by electronic scanning microscopy in secondary electron mode (SSE) and electron microscopy scaning by backscattered electron mode. Also scalar properties of the masonry and the following: density, porosity and mechanical resistance, among others. In Chapter IV, characteristics of the mortars used in the houses are analyzed and pathology or damages are presented. They are classified into three types: grout, cement render and plaster. Physical and chemical testing, mechanical strength and grain size (granulometric) is documented; its main components are explained: lime binder, aggregates and additives and manufacturing technology as well as the physical, water, chemical and granulometric characteristics. Chapter V contains the constructive applications of masonry materials. Other housing elements are described, such as; foundations, mixed walls, moldings, wall paintings and finally floorings (pavements). And in chapter VI the most representative species of wood used in the overhead fixtures and cover elements are analyzed. Likewise, woodwork of doors and windows and their wooden lintels or landings are described; anatomical identification and physical and mechanical properties of the ones used is made. The results and conclusions determined that 90% of the materials used in its construction came from areas near the construction of housing, such as El Milagro formation, converted into stone quarry and other materials came from the Toas Island and from the export of the Caribbean islands and Europe, such as cement. The main contribution of this research is the constructive technical analysis and physical, mechanical and chemical characterization of the materials of the houses, in order that such information is used to define the new materials to be used in the housing restoration and future research lines.

Aplicación de la celulosa bacteriana a la restauración del patrimonio bibliográfico y documental en papel

La preservación del patrimonio bibliográfico y documental en papel es uno de los mayores retos a los que se enfrentan bibliotecas y archivos de todo el mundo. La búsqueda de soluciones al problema del papel degradado ha sido abordada históricamente desde dos líneas de trabajo predominantes: la conservación de estos documentos mediante la neutralización de los ácidos presentes en ellos con agentes alcalinos, y su restauración mediante el método de laminación fundamentalmente con papel de origen vegetal. Sin embargo, no se ha explorado con éxito la posibilidad de reforzar la celulosa dañada, y el problema sigue sin encontrar una solución satisfactoria. Hasta el día de hoy, el desarrollo de tratamientos basados en biotecnología en la conservación del patrimonio documental ha sido muy escaso, aunque la capacidad de ciertas bacterias de producir celulosa lleva a plantear su uso en el campo de la conservación y restauración del papel. La celulosa bacteriana (CB) es químicamente idéntica a la celulosa vegetal, pero su organización macroscópica es diferente. Sus propiedades únicas (alto grado de cristalinidad, durabilidad, resistencia y biocompatibilidad) han hecho de este material un excelente recurso en diferentes campos. En el desarrollo de esta tesis se ha estudiado el uso de la celulosa bacteriana, de alta calidad, generada por Gluconacetobacter sucrofermentans CECT 7291, para restaurar documentos deteriorados y consolidar los que puedan estar en peligro de degradación, evitando así su destrucción y proporcionando al papel que se restaura unas buenas propiedades mecánicas, ópticas y estructurales. Se desarrollan asimismo protocolos de trabajo que permitan la aplicación de dicha celulosa. En primer lugar se seleccionó el medio de cultivo que proporcionó una celulosa adecuada para su uso en restauración. Para ello se evaluó el efecto que tienen sobre la celulosa generada las fuentes de carbono y nitrógeno del medio de cultivo, manteniendo como parámetros fijos la temperatura y el pH inicial del medio, y efectuando los ensayos en condiciones estáticas. Se evaluó, también, el efecto que tiene en la CB la adición de un 1% de etanol al medio de cultivo. Las capas de celulosa se recolectaron a cuatro tiempos distintos, caracterizando en cada uno de ellos el medio de cultivo (pH y consumo de fuente de carbono), y las capas de CB (pH, peso seco y propiedades ópticas y mecánicas). La mejor combinación de fuentes de carbono y nitrógeno resultó ser fructosa más extracto de levadura y extracto de maíz, con o sin etanol, que proporcionaban una buena relación entre la producción de celulosa y el consumo de fuente de carbono, y que generaban una capa de celulosa resistente y homogénea. La adición de etanol al medio de cultivo, si bien aumentaba la productividad, causaba un descenso apreciable de pH. Las capas de CB obtenidas con los medios de cultivo optimizados se caracterizaron en términos de sus índices de desgarro y estallido, propiedades ópticas, microscopía electrónica de barrido (SEM), difracción de rayos-X, espectroscopía infrarroja con transformada de Fourier (FTIR), grado de polimerización, ángulos de contacto estáticos y dinámicos, y porosimetría de intrusión de mercurio. Por otro lado hay que tener en cuenta que el material restaurado debe ser estable con el tiempo. Por ello esta misma caracterización se efectuó tras someter a las capas de CB a un proceso de envejecimiento acelerado. Los resultados mostraron que la CB resultante tiene un elevado índice de cristalinidad, baja porosidad interna, buenas propiedades mecánicas, y alta estabilidad en el tiempo. Para desarrollar los protocolos de trabajo que permitan la restauración con esta celulosa optimizada, se comienzó con un proceso de selección de los papeles que van a ser restaurados. Se eligieron tres tipos de papeles modelo, hechos con pasta mecánica, química y filtro (antes y después de ser sometidos a un proceso de envejecimiento acelerado), y tres libros viejos adquiridos en el mercado de segunda mano. Estos ejemplares a restaurar se caracterizaron también en términos de sus propiedades mecánicas y fisicoquímicas. El primer protocolo de restauración con CB que se evaluó fue el denominado laminación. Consiste en aplicar un material de refuerzo al documento mediante el uso de un adhesivo. Se seleccionó para ello la CB producida en el medio de cultivo optimizado con un 1% de etanol. Se aplicó un método de purificación alcalino (1 hora a 90 °C en NaOH al 1%) y como adhesivo se seleccionó almidón de trigo. El proceso de laminación se efectuó también con papel japonés (PJ), un material habitualmente utilizado en conservación, para comparar ambos materiales. Se concluyó que no hay diferencias significativas en las características estudiadas entre los dos tipos de materiales de refuerzo. Se caracterizó el material reforzado y, también, después de sufrir un proceso de envejecimiento acelerado. Los papeles laminados con CB mostraban diferencias más marcadas en las propiedades ópticas que los restaurados con PJ, con respecto a los originales. Sin embargo, el texto era más legible cuando el material de restauración era la CB. La mojabilidad disminuía con ambos tipos de refuerzo, aunque en los papeles laminados con CB de manera más marcada e independiente del material a restaurar. Esto se debe a la estructura cerrada de la CB, que también conduce a una disminución en la permeabilidad al aire. Este estudio sugiere que la CB mejora la calidad del papel deteriorado, sin alterar la información que contiene, y que esta mejora se mantiene a lo largo del tiempo. Por tanto, la CB puede ser utilizada como material de refuerzo para laminar, pudiendo ser más adecuada que el PJ para ciertos tipos de papeles. El otro método de restauración que se estudió fue la generación in situ de la CB sobre el papel a restaurar. Para ello se seleccionó el medio de cultivo sin etanol, ya que el descenso de pH que causaba su presencia podría dañar el documento a restaurar. El método de purificación elegido fue un tratamiento térmico (24 horas a 65 °C), menos agresivo para el material a restaurar que el tratamiento alcalino. Se seleccionó la aplicación del medio de cultivo con la bacteria mediante pincel sobre el material a restaurar. Una vez caracterizado el material restaurado, y éste mismo tras sufrir un proceso de envejecimiento acelerado, se concluyó que no hay modificación apreciable en ninguna característica, salvo en la permeabilidad al aire, que disminuye de manera muy evidente con la generación de CB, dando lugar a un material prácticamente impermeable al aire. En general se puede concluir que ha quedado demostrada la capacidad que tiene la celulosa generada por la bacteria Gluconacetobacter sucrofermentans CECT 7291 para ser utilizada como material de refuerzo en la restauración del patrimonio documental en papel. Asimismo se han desarrollado dos métodos de aplicación, uno ex situ y otro in situ, para efectuar esta tarea de restauración. ABSTRACT The preservation of bibliographic and documentary heritage is one of the biggest challenges that libraries and archives around the world have to face. The search for solutions to the problem of degraded paper has historically been focused from two predominants lines of work: the conservation of these documents by the neutralization of acids in them with alkaline agents, and their restoration by lining them with, basically, cellulose from vegetal sources. However, the possibility of strengthening the damaged cellulose has not been successfully explored, and the problem still persists. Until today, the development of biotechnology-based treatments in documentary heritage conservation has been scarce, although the ability of certain bacteria to produce cellulose takes to propose its use in the field of conservation and restoration of paper. The bacterial cellulose (BC) is chemically identical to the plant cellulose, but its macroscopic organization is different. Its unique properties (high degree of crystallinity, durability, strength and biocompatibility), makes it an excellent resource in different fields. The use of high-quality BC generated by Gluconacetobacter sucrofermentans CECT 7291 to restore damaged documents and to consolidate those that may be at risk of degradation, has been studied in this thesis, trying to prevent the document destruction, and to get reinforced papers with good mechanical, optical and structural properties. Protocols that allow the implementation of the BC as a reinforcing material were also developed. First of all, in order to select the culture medium that provides a cellulose suitable for its use in restoration, it has been evaluated the effect that the carbon and nitrogen sources from the culture medium have on the generated BC, keeping the temperature and the initial pH of the medium as fixed parameters, and performing the culture without shaking. The effect of the addition of 1% ethanol to the culture medium on BC properties was also evaluated. The cellulose layers were collected at four different times, characterizing in all of them the culture medium (pH and carbon source consumption), and the BC sheets (pH, dry weight and optical and mechanical properties). The best combination of carbon and nitrogen sources proved to be fructose plus yeast extract and corn steep liquor, with or without ethanol, which provided a good balance between the cellulose production and the consumption of carbon source, and generating BC sheets homogeneous and resistant. The addition of ethanol to the culture medium increased productivity but caused a noticeable decrement in pH. The BC layers generated with these optimized culture media, have been characterized in terms of tear and burst index, optical properties, scanning electron microscopy (SEM), X-ray diffraction, infrared Fourier transform spectroscopy (FTIR), polymerization degree, static and dynamic contact angles, and mercury intrusion porosimetry. Moreover it must be kept in mind that the restored materials should be stable over time. Therefore, the same characterization was performed after subjecting the layers of BC to an accelerated aging process. The results showed that the BC sheets obtained have a high crystallinity index, low internal porosity, good mechanical properties, and high stability over time. To develop working protocols to use this optimized BC in paper restoration, the first step was to select the samples to restore. Three types of model papers, made from mechanical pulp, chemical pulp and filter paper (before and after an accelerated aging process), and three old books purchased in the second hand market, were chosen. These specimens to be restored were also characterized in terms of its mechanical and physicochemical properties. The first protocol of restoration with BC to be evaluated is called linning. It consists on applying a reinforcing material to the document using an adhesive. The BC produced in the optimized culture medium with 1% ethanol was selected. An alkali purification method (1 hour at 90 °C in 1% NaOH) was applied, and wheat starch was selected as adhesive. The linning process was also carried out with Japanese paper (JP), a material commonly used in conservation, in order to compare both materials. It was concluded that there are no significant differences in the characteristics studied of the two types of reinforcing materials. The reinforced materials were characterized before and after undergoing to an accelerated aging. Papers lined with BC showed more marked differences in the optical properties that papers restored with JP. However, the text was more readable when BC was the reinforcing material. Wettability decreased with both types of reinforcement, although in the papers linned with BC it happened more marked and independently of the sample to restore. This is due to the closed structure of BC, which also leads to a decrement in air permeance. This study suggests that BC improves the deteriorated paper quality, without altering the information on it, and that this improvement is maintained over time. Therefore, the BC may be used as reinforcing material for linning, being more suitable than the JP to restore certain types of papers. The other restoration method to be evaluated was the in situ generation of BC over the paper to restore. For this purpose the culture medium without ethanol was selected, as the pH decrement caused by his presence would damage the document to restore. As purification method a heat treatment (24 hours at 65 °C) was chosen, less aggressive to the material to restore than the alkaline treatment. It was decided to apply the culture medium with the bacteria onto the material to restore with a brush. The reinforced material was characterized before and after an accelerated aging process. It was concluded that there was no substantial change in any characteristic, except for air permeance, which decreases very sharply after the generation of BC, getting a substantially air impermeable material. In general, it can be concluded that the ability of BC produced by Gluconacetobacter sucrofermentans CECT 7291 for its use as a reinforcing material in the restoration of paper documentary heritage, has been demonstrated. Also, two restoration methods, one ex situ and another in situ have been developed.

The effects of tantalum addition on the microtexture and mechanical behaviour of tungsten for ITER applications

Tungsten (W) and its alloys are very promising materials for producing plasma-facing components (PFCs) in the fusion power reactors of the near future, even as a structural part in them. However, whereas the properties of pure tungsten are suitable for a PFC, its structural applications are still limited due to its low toughness, ductile to brittle transition temperature and recrystallization behaviour. Therefore, many efforts have been made to improve its performance by alloying tungsten with other elements. Hence, in this investigation, the thermo-mechanical performance of two new tungsten-tantalum materials has been evaluated. Materials with We5wt.%Ta and We15wt.%Ta were processed by mechanical alloying (MA) and later consolidation by hot isostatic pressing (HIP), with distinct settings for each composition. Thus, it was possible to determine the relationship between the microstructure and the addition of Ta with the macroscopic mechanical properties. These were measured by means of hardness, flexural strength and fracture toughness, in the temperature range of 300e1473 K. The microstructure and the fracture surfaces features of the tested materials were analysed by Field Emission Scanning Electron Microscopy (FESEM).