Performance analysis of AlGaAs/GaAs tunnel junctions for ultra-high concentration photovoltaics

An n(++)-GaAs/p(++)-AlGaAs tunnel junction with a peak current density of 10 100Acm(-2) is developed. This device is a tunnel junction for multijunction solar cells, grown lattice-matched on standard GaAs or Ge substrates, with the highest peak current density ever reported. The voltage drop for a current density equivalent to the operation of the multijunction solar cell up to 10 000 suns is below 5 mV. Trap-assisted tunnelling is proposed to be behind this performance, which cannot be justified by simple band-to-band tunnelling. The metal-organic vapour-phase epitaxy growth conditions, which are in the limits of the transport-limited regime, and the heavy tellurium doping levels are the proposed origins of the defects enabling trap-assisted tunnelling. The hypothesis of trap-assisted tunnelling is supported by the observed annealing behaviour of the tunnel junctions, which cannot be explained in terms of dopant diffusion or passivation. For the integration of these tunnel junctions into a triple-junction solar cell, AlGaAs barrier layers are introduced to suppress the formation of parasitic junctions, but this is found to significantly degrade the performance of the tunnel junctions. However, the annealed tunnel junctions with barrier layers still exhibit a peak current density higher than 2500Acm(-2) and a voltage drop at 10 000 suns of around 20 mV, which are excellent properties for tunnel junctions and mean they can serve as low-loss interconnections in multijunction solar cells working at ultra-high concentrations.

Highly efficient potentiometric glucose biosensor based on functionalized InN quantum dots

We present a fast, highly sensitive, and efficient potentiometric glucose biosensor based on functionalized InN quantum-dots (QDs). The InN QDs are grown by molecular beam epitaxy. The InN QDs are bio-chemically functionalized through physical adsorption of glucose oxidase (GOD). GOD enzyme-coated InN QDs based biosensor exhibits excellent linear glucose concentration dependent electrochemical response against an Ag/AgCl reference electrode over a wide logarithmic glucose concentration range (1 × 10−5 M to 1 × 10−2 M) with a high sensitivity of 80 mV/decade. It exhibits a fast response time of less than 2 s with good stability and reusability and shows negligible response to common interferents such as ascorbic acid and uric acid. The fabricated biosensor has full potential to be an attractive candidate for blood sugar concentration detection in clinical diagnoses.

Epitaxial self-alignment: A new route to hybrid active plasmonic nanostructures

Concepts of lateral ordering of epitaxial semiconductor quantum dots (QDs) are for the first time transferred to hybrid nanostructures for active plasmonics. We review our recent research on the self-alignment of epitaxial nanocrystals of In and Ag on ordered one-dimensional In(Ga)As QD arrays and isolated QDs by molecular beam epitaxy. By changing the growth conditions the size and density of the metal nanocrystals are easily controlled and the surface plasmon resonance wavelength is tuned over a wide range in order to match the emission wavelength of the QDs. Photoluminescence measurements reveal large enhancement of the emitted light intensity due to plasmon enhanced emission and absorption down to the single QD level.

Low-density InAs QDs with subcritical coverage obtained by conversion of In nanocrystals

We report growth of InAs/GaAs quantum dots (QDs) by molecular beam epitaxy with low density of 2 μm−2 by conversion of In nanocrystals deposited at low temperatures. The total amount of InAs used is about one monolayer, which is less than the critical thickness for conventional Stranski–Krastanov QDs. We also demonstrate the importance of the starting surface reconstruction for obtaining uniform QDs. The QD emission wavelength is easily tunable upon post-growth annealing with no wetting layer signal visible for short anneals. Microphotoluminescence measurements reveal well separated and sharp emission lines of individual QDs.

In situ control of As dimer orientation on Ge(100) surfaces

We investigated the preparation of single domain Ge(100):As surfaces in a metal-organic vapor phase epitaxy reactor. In situ reflection anisotropy spectra (RAS) of vicinal substrates change when arsenic is supplied either by tertiarybutylarsine or by background As4 during annealing. Low energy electron diffraction shows mutually perpendicular orientations of dimers, scanning tunneling microscopy reveals distinct differences in the step structure, and x-ray photoelectron spectroscopy confirms differences in the As coverage of the Ge(100): As samples. Their RAS signals consist of contributions related to As dimer orientation and to step structure, enabling precise in situ control over preparation of single domain Ge(100): As surfaces.

Impact of MOVPE Environment on Silicon Substrates for III-V-on-Si Multijunction Solar Cells

With the final goal of integrating III-V materials to silicon for tandem solar cells, the influence of the metal-organic vapor phase epitaxy (MOVPE) environment on the minority carrier properties of silicon wafers has been evaluated. These properties will essentially determine the photovoltaic performance of the bottom cell in a III-V-on-Si tandem solar cell device. A comparison of the base minority carrier lifetimes obtained for different thermal processes carried out in a MOVPE reactor on Czochralski silicon wafers has been carried out. The effect of the formation of the emitter by phosphorus diffusion has also been evaluated.

E-beam nano-patterning for the ordered growth of GaN/InGaN nanorods

E-beam lithography was used to pattern a titanium mask on a GaN substrate with ordered arrays of nanoholes. This patterned mask served as a template for the subsequent ordered growth of GaN/InGaN nanorods by plasma-assisted molecular beam epitaxy. The mask patterning process was optimized for several holes configurations. The smallest holes were 30 nm in diameter with a pitch (center-to-center distance) of 100 nm only. High quality masks of several geometries were obtained that could be used to grow ordered GaN/InGaN nanorods with full selectivity (growth localized inside the nanoholes only) over areas of hundreds of microns. Although some parasitic InGaN growth occurred between the nanorods during the In incorporation, transmission electron microscopy and photoluminescence measurements demonstrated that these ordered nanorods exhibit high crystal quality and reproducible optical properties.

Understanding phosphorus diffusion into silicon in a MOVPE environment for III-V on silicon solar cells

Dual-junction solar cells formed by a GaAsP or GaInP top cell and a silicon bottom cell seem to be attractive candidates to materialize the long sought-for integration of III?V materials on silicon for photovoltaic applications. When manufacturing a multi-junction solar cell on silicon, one of the first processes to be addressed is the development of the bottom subcell and, in particular, the formation of its emitter. In this study, we analyze, both experimentally and by simulations, the formation of the emitter as a result of phosphorus diffusion that takes place during the first stages of the epitaxial growth of the solar cell. Different conditions for the Metal-Organic Vapor Phase Epitaxy (MOVPE) process have been evaluated to understand the impact of each parameter, namely, temperature, phosphine partial pressure, time exposure and memory effects in the final diffusion profiles obtained. A model based on SSupremIV process simulator has been developed and validated against experimental profiles measured by ECV and SIMS to calculate P diffusion profiles in silicon formed in a MOVPE environment taking in consideration all these factors.

Glassy State and Cryopreservation of Mint Shoot Tips

Vitrification refers to the physical process by which a liquid supercools to very low tem- peratures and finally solidifies into a metastable glass, without undergoing crystallization at a practical cooling rate. Thus, vitrification is an effective freeze-avoidance mechanism and living tissue cryopreservation is, in most cases, relying on it. As a glass is exceedingly vis- cous and stops all chemical reactions that require molecular diffusion, its formation leads to metabolic inactivity and stability over time. To investigate glassy state in cryopreserved plant material, mint shoot tips were submitted to the different stages of a frequently used cryopreservation protocol (droplet-vitrification) and evaluated for water content reduction and sucrose content, as determined by ion chromatography, frozen water fraction and glass transitions occurrence by differential scanning calorimetry, and investigated by low-tempera- ture scanning electron microscopy, as a way to ascertain if their cellular content was vitri- fied. Results show how tissues at intermediate treatment steps develop ice crystals during liquid nitrogen cooling, while specimens whose treatment was completed become vitrified, with no evidence of ice formation. The agreement between calorimetric and microscopic observations was perfect. Besides finding a higher sucrose concentration in tissues at the more advanced protocol steps, this level was also higher in plants precultured at 25/21?C than in plants cultivated at 25?C.

Effect of concentration on the performance of quantum dot intermediate-band solar cells

Implementation of a high-efficiency quantum dot intermediate-band solar cell (QD-IBSC) must accompany a sufficient photocurrent generation via IB states. The demonstration of a QD-IBSC is presently undergoing two stages. The first is to develop a technology to fabricate high-density QD stacks or a superlattice of low defect density placed within the active region of a p-i-n SC, and the second is to realize half-filled IB states to maximize the photocurrent generation by two-step absorption of sub-bandgap photons. For this, we have investigated the effect of light concentration on the characteristics of QDSCs comprised of multi-layer stacks of self-organized InAs/GaNAs QDs grown with and without impurity doping in molecular beam epitaxy.

In situ control of Si(100) and Ge(100) surface preparation for the heteroepitaxy of III-V solar cell architectures

Si(100) and Ge(100) substrates essential for subsequent III-V integration were studied in the hydrogen ambient of a metalorganic vapor phase epitaxy reactor. Reflectance anisotropy spectroscopy (RAS) enabled us to distinguish characteristic configurations of vicinal Si(100) in situ: covered with oxide, cleaned by thermal removing in H2, and terminated with monohydrides when cooling in H2 ambient. RAS measurements during cooling in H2 ambient after the oxide removal process revealed a transition from the clean to the monohydride terminated Si(100) surface dependent on process temperature. For vicinal Ge(100) we observed a characteristic RA spectrum after annealing and cooling in H2 ambient. According to results from X-ray photo electron spectroscopy and Fourier-transform infrared spectroscopy the spectrum corresponds to the monohydride terminated Ge(100) surface.

Open-atmosphere structural depth profiling of multilayer samples of photovoltaic interest using laser-induced plasma spectrometry

The present work aims to assess Laser-Induced Plasma Spectrometry (LIPS) as a tool for the characterization of photovoltaic materials. Despite being a well-established technique with applications to many scientific and industrial fields, so far LIPS is little known to the photovoltaic scientific community. The technique allows the rapid characterization of layered samples without sample preparation, in open atmosphere and in real time. In this paper, we assess LIPS ability for the determination of elements that are difficult to analyze by other broadly used techniques, or for producing analytical information from very low-concentration elements. The results of the LIPS characterization of two different samples are presented: 1) a 90 nm, Al-doped ZnO layer deposited on a Si substrate by RF sputtering and 2) a Te-doped GaInP layer grown on GaAs by Metalorganic Vapor Phase Epitaxy. For both cases, the depth profile of the constituent and dopant elements is reported along with details of the experimental setup and the optimization of key parameters. It is remarkable that the longest time of analysis was ∼10 s, what, in conjunction with the other characteristics mentioned, makes of LIPS an appealing technique for rapid screening or quality control whether at the lab or at the production line.

Intermediate Band to Conduction Band optical absorption in ZnTe:O

ZnTe doped with high concentrations of oxygen has been proposed in previous works as intermediate band (IB) material for photovoltaic applications. The existence of extra optical transitions related to the presence of an IB has already been demonstrated in this material and it has been possible to measure the absorption coefficient of the transitions from the valence band (VB) to the IB. In this work we present the first measurement of the absorption coefficient associated to transitions from the IB to the conduction band (CB) in ZnTe:O. The samples used are 4 ?m thick ZnTe layers with or without O in a concentration ~ 1019 cm-3, which have been grown on semi-insulating GaAs substrates by molecular beam epitaxy (MBE). The IB-CB absorption coefficient peaks for photon energies ~ 0.4 eV. It is extracted from reflectance and transmittance spectra measured using Fourier Transform Infrared (FTIR) spectroscopy. Under typical FTIR measurement conditions (low light intensity, broadband spectrum) the absorption coefficient in IB-to-CB transitions reaches 700 cm-1. This is much weaker than the one observed for VB-IB absorption. This result is consistent with the fact that the IB is expected to be nearly empty of electrons under equilibrium conditions in ZnTe(:O). The absorption for VB to IB transitions is also observed in the same samples through reflectance measurements performed in the visible range using a monochromator. These measurements are compared with the quantum efficiency (QE) from solar cells fabricated under similar conditions.

Modelización de los Procesos de Cristalización en Poliolefinas

“Por lo tanto, la cristalización de polímeros se supone, y en las teorías se describe a menudo, como un proceso de múltiples pasos con muchos aspectos físico-químicos y estructurales influyendo en él. Debido a la propia estructura de la cadena, es fácil entender que un proceso que es termodinámicamente forzado a aumentar su ordenamiento local, se vea obstaculizado geométricamente y, por tanto, no puede conducirse a un estado de equilibrio final. Como resultado, se forman habitualmente estructuras de no equilibrio con diferentes características dependiendo de la temperatura, presión, cizallamiento y otros parámetros físico-químicos del sistema”. Estas palabras, pronunciadas recientemente por el profesor Bernhard Wunderlich, uno de los mas relevantes fisico-quimicos que han abordado en las ultimas décadas el estudio del estado físico de las macromoléculas, adelantan lo que de alguna manera se explicita en esta memoria y constituyen el “leitmotiv” de este trabajo de tesis. El mecanismo de la cristalización de polímeros esta aun bajo debate en la comunidad de la física de polímeros y la mayoría de los abordajes experimentales se explican a través de la teoría LH. Esta teoría clásica debida a Lauritzen y Hoffman (LH), y que es una generalización de la teoría de cristalización de una molécula pequeña desde la fase de vapor, describe satisfactoriamente muchas observaciones experimentales aunque esta lejos de explicar el complejo fenómeno de la cristalización de polímeros. De hecho, la formulación original de esta teoría en el National Bureau of Standards, a comienzos de la década de los 70, sufrió varias reformulaciones importantes a lo largo de la década de los 80, buscando su adaptación a los hallazgos experimentales. Así nació el régimen III de cristalización que posibilita la creacion de nichos moleculares en la superficie y que dio pie al paradigma ofrecido por Sadler y col., para justificar los experimentos que se obtenian por “scattering” de neutrones y otras técnicas como la técnica de “droplets” o enfriamiento rapido. Por encima de todo, el gran éxito de la teoría radica en que explica la dependencia inversa entre el tamaño del plegado molecular y el subenfriamiento, definido este ultimo como el intervalo de temperatura que media entre la temperatura de equilibrio y la temperatura de cristalización. El problema concreto que aborda esta tesis es el estudio de los procesos de ordenamiento de poliolefinas con distinto grado de ramificacion mediante simulaciones numéricas. Los copolimeros estudiados en esta tesis se consideran materiales modelo de gran homogeneidad molecular desde el punto de vista de la distribución de tamaños y de ramificaciones en la cadena polimérica. Se eligieron estas poliolefinas debido al gran interes experimental en conocer el cambio en las propiedades fisicas de los materiales dependiendo del tipo y cantidad de comonomero utilizado. Además, son modelos sobre los que existen una ingente cantidad de información experimental, que es algo que preocupa siempre al crear una realidad virtual como es la simulación. La experiencia en el grupo Biophym es que los resultados de simulación deben de tener siempre un correlato mas o menos próximo experimental y ese argumento se maneja a lo largo de esta memoria. Empíricamente, se conoce muy bien que las propiedades físicas de las poliolefinas, en suma dependen del tipo y de la cantidad de ramificaciones que presenta el material polimérico. Sin embargo, tal como se ha explicado no existen modelos teóricos adecuados que expliquen los mecanismos subyacentes de los efectos de las ramas. La memoria de este trabajo es amplia por la complejidad del tema. Se inicia con una extensa introducción sobre los conceptos básicos de una macromolecula que son relevantes para entender el contenido del resto de la memoria. Se definen los conceptos de macromolecula flexible, distribuciones y momentos, y su comportamiento en disolución y fundido con los correspondientes parametros caracteristicos. Se pone especial énfasis en el concepto de “entanglement” o enmaranamiento por considerarse clave a la hora de tratar macromoléculas con una longitud superior a la longitud critica de enmaranamiento. Finaliza esta introducción con una reseña sobre el estado del arte en la simulación de los procesos de cristalización. En un segundo capitulo del trabajo se expone detalladamente la metodología usada en cada grupo de casos. En el primer capitulo de resultados, se discuten los estudios de simulación en disolución diluida para sistemas lineales y ramificados de cadena única. Este caso mas simple depende claramente del potencial de torsión elegido tal como se discute a lo largo del texto. La formación de los núcleos “babys” propuestos por Muthukumar parece que son consecuencia del potencial de torsión, ya que este facilita los estados de torsión mas estables. Así que se propone el análisis de otros potenciales que son igualmente utilizados y los resultados obtenidos sobre la cristalización, discutidos en consecuencia. Seguidamente, en un segundo capitulo de resultados se estudian moleculas de alcanos de cadena larga lineales y ramificados en un fundido por simulaciones atomisticas como un modelo de polietileno. Los resultados atomisticos pese a ser de gran detalle no logran captar en su totalidad los efectos experimentales que se observan en los fundidos subenfriados en su etapa previa al estado ordenado. Por esta razon se discuten en los capítulos 3 y 4 de resultados sistemas de cadenas cortas y largas utilizando dos modelos de grano grueso (CG-PVA y CG-PE). El modelo CG-PE se desarrollo durante la tesis. El uso de modelos de grano grueso garantiza una mayor eficiencia computacional con respecto a los modelos atomísticos y son suficientes para mostrar los fenómenos a la escala relevante para la cristalización. En todos estos estudios mencionados se sigue la evolución de los procesos de ordenamiento y de fusión en simulaciones de relajación isoterma y no isoterma. Como resultado de los modelos de simulación, se han evaluado distintas propiedades fisicas como la longitud de segmento ordenado, la cristalinidad, temperaturas de fusion/cristalizacion, etc., lo que permite una comparación con los resultados experimentales. Se demuestra claramente que los sistemas ramificados retrasan y dificultan el orden de la cadena polimérica y por tanto, las regiones cristalinas ordenadas decrecen al crecer las ramas. Como una conclusión general parece mostrarse una tendencia a la formación de estructuras localmente ordenadas que crecen como bloques para completar el espacio de cristalización que puede alcanzarse a una temperatura y a una escala de tiempo determinada. Finalmente hay que señalar que los efectos observados, estan en concordancia con otros resultados tanto teoricos/simulacion como experimentales discutidos a lo largo de esta memoria. Su resumen se muestra en un capitulo de conclusiones y líneas futuras de investigación que se abren como consecuencia de esta memoria. Hay que mencionar que el ritmo de investigación se ha acentuado notablemente en el ultimo ano de trabajo, en parte debido a las ventajas notables obtenidas por el uso de la metodología de grano grueso que pese a ser muy importante para esta memoria no repercute fácilmente en trabajos publicables. Todo ello justifica que gran parte de los resultados esten en fase de publicación. Abstract “Polymer crystallization is therefore assumed, and in theories often described, to be a multi step process with many influencing aspects. Because of the chain structure, it is easy to understand that a process which is thermodynamically forced to increase local ordering but is geometrically hindered cannot proceed into a final equilibrium state. As a result, nonequilibrium structures with different characteristics are usually formed, which depend on temperature, pressure, shearing and other parameters”. These words, recently written by Professor Bernhard Wunderlich, one of the most prominent researchers in polymer physics, put somehow in value the "leitmotiv "of this thesis. The crystallization mechanism of polymers is still under debate in the physics community and most of the experimental findings are still explained by invoking the LH theory. This classical theory, which was initially formulated by Lauritzen and Hoffman (LH), is indeed a generalization of the crystallization theory for small molecules from the vapor phase. Even though it describes satisfactorily many experimental observations, it is far from explaining the complex phenomenon of polymer crystallization. This theory was firstly devised in the early 70s at the National Bureau of Standards. It was successively reformulated along the 80s to fit the experimental findings. Thus, the crystallization regime III was introduced into the theory in order to explain the results found in neutron scattering, droplet or quenching experiments. This concept defines the roughness of the crystallization surface leading to the paradigm proposed by Sadler et al. The great success of this theory is the ability to explain the inverse dependence of the molecular folding size on the supercooling, the latter defined as the temperature interval between the equilibrium temperature and the crystallization temperature. The main scope of this thesis is the study of ordering processes in polyolefins with different degree of branching by using computer simulations. The copolymers studied along this work are considered materials of high molecular homogeneity, from the point of view of both size and branching distributions of the polymer chain. These polyolefins were selected due to the great interest to understand their structure– property relationships. It is important to note that there is a vast amount of experimental data concerning these materials, which is essential to create a virtual reality as is the simulation. The Biophym research group has a wide experience in the correlation between simulation data and experimental results, being this idea highly alive along this work. Empirically, it is well-known that the physical properties of the polyolefins depend on the type and amount of branches presented in the polymeric material. However, there are not suitable models to explain the underlying mechanisms associated to branching. This report is extensive due to the complexity of the topic under study. It begins with a general introduction to the basics concepts of macromolecular physics. This chapter is relevant to understand the content of the present document. Some concepts are defined along this section, among others the flexibility of macromolecules, size distributions and moments, and the behavior in solution and melt along with their corresponding characteristic parameters. Special emphasis is placed on the concept of "entanglement" which is a key item when dealing with macromolecules having a molecular size greater than the critical entanglement length. The introduction finishes with a review of the state of art on the simulation of crystallization processes. The second chapter of the thesis describes, in detail, the computational methodology used in each study. In the first results section, we discuss the simulation studies in dilute solution for linear and short chain branched single chain models. The simplest case is clearly dependent on the selected torsion potential as it is discussed throughout the text. For example, the formation of baby nuclei proposed by Mutukhumar seems to result from the effects of the torsion potential. Thus, we propose the analysis of other torsion potentials that are also used by other research groups. The results obtained on crystallization processes are accordingly discussed. Then, in a second results section, we study linear and branched long-chain alkane molecules in a melt by atomistic simulations as a polyethylene-like model. In spite of the great detail given by atomistic simulations, they are not able to fully capture the experimental facts observed in supercooled melts, in particular the pre-ordered states. For this reason, we discuss short and long chains systems using two coarse-grained models (CG-PVA and CG-PE) in section 3 and 4 of chapter 2. The CG-PE model was developed during the thesis. The use of coarse-grained models ensures greater computational efficiency with respect to atomistic models and is enough to show the relevant scale phenomena for crystallization. In all the analysis we follow the evolution of the ordering and melting processes by both isothermal and non isothermal simulations. During this thesis we have obtained different physical properties such as stem length, crystallinity, melting/crystallization temperatures, and so on. We show that branches in the chains cause a delay in the crystallization and hinder the ordering of the polymer chain. Therefore, crystalline regions decrease in size as branching increases. As a general conclusion, it seems that there is a tendency in the macromolecular systems to form ordered structures, which can grown locally as blocks, occupying the crystallization space at a given temperature and time scale. Finally it should be noted that the observed effects are consistent with both, other theoretical/simulation and experimental results. The summary is provided in the conclusions chapter along with future research lines that open as result of this report. It should be mentioned that the research work has speeded up markedly in the last year, in part because of the remarkable benefits obtained by the use of coarse-grained methodology that despite being very important for this thesis work, is not easily publishable by itself. All this justify that most of the results are still in the publication phase.

Estudios termodinámicos de los procesos de vitrificación en la crioconservación de germoplasma vegetal=Thermodynamic studies of vitrification processes in plant germplasm cryopreservation

En la actualidad, las técnicas de crioconservación poseen una importancia creciente para el almacenamiento a largo plazo de germoplasma vegetal. En las dos últimas décadas, estos métodos experimentaron un gran desarrollo y se han elaborado protocolos adecuados a diferentes sistemas vegetales, utilizando diversas estrategias como la vitrificación, la encapsulación-desecación con cuentas de alginato y el método de “droplet”-vitrificación. La presente tesis doctoral tiene como objetivo aumentar el conocimiento sobre los procesos implicados en los distintos pasos de un protocolo de crioconservación, en relación con el estado del agua presente en los tejidos y sus cambios, abordado mediante diversas técnicas biofísicas, principalmente calorimetría diferencial de barrido (DSC) y microscopía electrónica de barrido a baja temperatura (crio-SEM). En un primer estudio sobre estos métodos de crioconservación, se describen las fases de enfriamiento hasta la temperatura del nitrógeno líquido y de calentamiento hasta temperatura ambiente, al final del periodo de almacenamiento, que son críticas para la supervivencia del material crioconservado. Tanto enfriamiento como calentamiento deben ser realizados lo más rápidamente posible pues, aunque los bajos contenidos en agua logrados en etapas previas de los protocolos reducen significativamente las probabilidades de formación de hielo, éstas no son del todo nulas. En ese contexto, se analiza también la influencia de las velocidades de enfriamiento y calentamiento de las soluciones de crioconservación de plantas en sus parámetros termofísicos referente a la vitrificación, en relación su composición y concentración de compuestos. Estas soluciones son empleadas en la mayor parte de los protocolos actualmente utilizados para la crioconservación de material vegetal. Además, se estudia la influencia de otros factores que pueden determinar la estabilidad del material vitrificado, tales como en envejecimiento del vidrio. Se ha llevado a cabo una investigación experimental en el empleo del crio-SEM como una herramienta para visualizar el estado vítreo de las células y tejidos sometidos a los procesos de crioconservación. Se ha comparado con la más conocida técnica de calorimetría diferencial de barrido, obteniéndose resultados muy concordantes y complementarios. Se exploró también por estas técnicas el efecto sobre tejidos vegetales de la adaptación a bajas temperaturas y de la deshidratación inducida por los diferentes tratamientos utilizados en los protocolos. Este estudio permite observar la evolución biofísica de los sistemas en el proceso de crioconservación. Por último, se estudió la aplicación de películas de quitosano en las cuentas de alginato utilizadas en el protocolo de encapsulación. No se observaron cambios significativos en su comportamiento frente a la deshidratación, en sus parámetros calorimétricos y en la superficie de las cuentas. Su aplicación puede conferir propiedades adicionales prometedoras. ABSTRACT Currently, cryopreservation techniques have a growing importance for long term plant germplasm storage. These methods have undergone great progress during the last two decades, and adequate protocols for different plant systems have been developed, making use of diverse strategies, such as vitrification, encapsulation-dehydration with alginate beads and the dropletvitrification method. This PhD thesis has the goal of increasing the knowledge on the processes underlying the different steps of cryopreservation protocols, in relation with the state of water on tissues and its changes, approached through diverse biophysical techniques, especially differential scanning calorimetry (DSC) and low-temperature scanning electron microscopy (cryo-SEM). The processes of cooling to liquid nitrogen temperature and warming to room temperature, at the end of the storage period, critical for the survival of the cryopreserved material, are described in a first study on these cryopreservation methods. Both cooling and warming must be carried out as quickly as possible because, although the low water content achieved during previous protocol steps significantly reduces ice formation probability, it does not completely disappear. Within this context, the influence of plant vitrification solutions cooling and warming rate on their vitrification related thermophysical parameters is also analyzed, in relation to its composition and component concentration. These solutions are used in most of the currently employed plant material cryopreservation protocols. Additionally, the influence of other factors determining the stability of vitrified material is studied, such as glass aging. An experimental research work has been carried out on the use of cryo-SEM as a tool for visualizing the glassy state in cells and tissues, submitted to cryopreservation processes. It has been compared with the better known differential scanning calorimetry technique, and results in good agreement and complementary have been obtained. The effect on plant tissues of adaptation to low temperature and of the dehydration induced by the different treatments used in the protocols was explored also by these techniques. This study allows observation of the system biophysical evolution in the cryopreservation process. Lastly, the potential use of an additional chitosan film over the alginate beads used in encapsulation protocols was examined. No significant changes could be observed in its dehydration and calorimetric behavior, as well as in its surface aspect; its application for conferring additional properties to gel beads is promising.