<p>U okviru doktorske disertacije predstavljene su elektronska i fononska struktura odabranih organometalnih materijala koji u svom sastavu imaju metale cink, kobalt ili bakar i organsko jedinjenje piridoksalaminogvanidin (PLAG). Predstavljene su realizacija i karakteristike organske svetleće diode zasnovane na najboljem od ispitivanih materijala. Urađena je detaljna analiza fotoluminescentnih spektara i njihovo razlaganje na proste komponente koristeći Lorencov model. Izvršeno je poređenje sa od ranije poznatim materijalom koji pokazuje visok stepen luminescencije. S obzirom da istraživanja vezana za organske svetleće diode uzimaju sve veći zamah i da ove diode postaju sve prisutnije u industrijskoj serijskoj proizvodnji, napravljena je detaljna analiza ove tehnologije i mehanizama koji se kriju iza nje. Urađeno je podrobno istraživanje kako na nivou elektrona u datim supstancama, tako i na nivou sloja organske svetleće diode. Na kraju je izvršena analiza rada diode sa integrisanim slojem sa materijalom koji u sebi sadrži cink i PLAG.</p> / <p>In this thesis electronic and phonon structure of specific organometallic<br />materials which have zinc, cobalt, copper metals and organic compound<br />pyridoxalaminoguanidin are presented. Implementation and characteristics of<br />organic light emitting diode based on the best material among examined<br />ones are also showed up. Detailed analysis of photoluminescence spectra<br />was done and its decomposition to its elementar components using<br />Lorentzian multipeak method. Comparison to well-known material that shows<br />high level of luminescence was implemented. In accordance to the fact that<br />research of organic light emitting diodes expands and that these diodes start<br />to be more present in industrial serial production, detailed analysis of this<br />technology and mechanisms behind it are made. Thorough research was<br />done both on electron level in these substances and organic light emitting<br />diode layer level. Finally, analysis of diode operation with integrated layer<br />made of material which includes zinc and pyridoxalaminoguanidin compound<br />is implemented.</p>

Tesis por compendio / [ES] La presente tesis doctoral plantea distintas estrategias para el desarrollo y aplicación de envases activos portadores de agentes de biocontrol, con el fin de inhibir la proliferación de microorganismos como bacterias y hongos patógenos y alterantes y así, conseguir aumentar la seguridad y prolongar la vida útil de los alimentos. El desarrollo de envases activos antibacterianos se llevó a cabo incorporando bacterias ácido lácticas productoras de bacteriocinas, Lactococcus lactis y Lactobacillus sakei en diferentes matrices formadoras de películas. Previa a la preparación de las películas activas, se estudió la actividad antimicrobiana de los agentes naturales seleccionados frente a Listeria monocytogenes. Los resultados sugirieron que, a partir de una determinada concentración inicial de bacterias viables, estos microorganismos son buenos candidatos para ser utilizados como aditivos naturales en materiales de envasado de alimentos, siendo una alternativa al uso de aditivos de origen sintético. En este trabajo se observó que la viabilidad inicial de las bacterias ácido lácticas (LAB) es esencial para obtener una buena capacidad antibacteriana por lo que la optimización de la composición de las películas o recubrimientos fue crucial para su aplicación con éxito. El polímero escogido como base para hacer las películas y recubrimientos mediante la técnica de casting, fue el alcohol polivinílico, (PVOH) mezclado con diferentes proteínas, gelatina y caseinato sódico y sus versiones hidrolizadas añadidas en diferentes proporciones. En este estudio L. lactis demostró tener una mayor resistencia a la deshidratación durante la preparación y almacenamiento de las películas que L. sakei. Las películas de PVOH mezcladas con gelatina hidrolizada y caseína hidrolizada dotaron de protección a las bacterias ácido lácticas durante el secado y demostraron tener una mayor efectividad antilisteria. Por último, se varió la proporción de caseína hidrolizada obteniendo una mayor viabilidad de las bacterias en las películas prolongada en el tiempo a mayor proporción de HCas. Para desarrollar un envase activo antilisteria, se adaptaron las matrices para ser aplicadas como recubrimiento sobre ácido poliláctico (PLA) con el objetivo de desarrollar bolsas activas antilisteria para crema de setas y como separadores de lonchas de jamón cocido. Los recubrimientos demostraron tener una efectividad similar a la obtenida con las películas in vitro. Sin embargo, su eficacia disminuyó ligeramente al ser aplicadas en la crema de champiñones y el jamón cocido debido a la complejidad de las matrices alimentarias utilizadas, pero siendo una buena herramienta para, junto a otras estrategias de conservación, asegurar la salubridad de los alimentos. Se llevaron a cabo ensayos sensoriales con consumidores y se obtuvo una buena aceptación de ambos productos. Sin embargo, los consumidores percibieron una alteración del sabor debido a la generación de ácido láctico en la crema de champiñones, acidez que puede ser controlada mediante correctores de acidez sin modificar la efectividad antimicrobiana. Para desarrollar envases que aumentaran la vida útil, se trabajó para ampliar el espectro de acción de L. lactis frente a las bacterias Gram-negativas, normalmente responsables de la descomposición de los alimentos. Combinar el agente de biocontrol productor de nisina, L. lactis, con una baja concentración de ácido fítico, sustancia quelante y desestabilizadora de la membrana bacteriana, amplió el espectro antimicrobiano de L. lactis frente a las bacterias Gram-negativas obteniendo una nueva herramienta para garantizar la seguridad alimentaria y prolongar la vida útil de los alimentos. / [CA] La present tesi doctoral planteja diferents estratègies per al desenvolupament i aplicació d'envasos actius portadors d'agents de biocontrol, amb la finalitat d'inhibir la proliferació de microorganismes com a bacteris i fongs patògens i alteradors i així, aconseguir augmentar la seguretat i prolongar la vida útil dels aliments. El desenvolupament d'envasos actius antibacterians, es va dur a terme incorporant bacteris àcid làctics productores de bacteriocines, Lactococcus lactis i Lactobacillus sakei en diferents matrius formadores de pel·lícules. Prèvia a la preparació de les pel·lícules actives, es va estudiar l'activitat antimicrobiana dels agents naturals seleccionats enfront de Listeria monocytogenes. Els resultats van suggerir que, a partir d'una determinada concentració inicial de bacteris viables, aquests microorganismes són bons candidats per a ser utilitzats com a additius naturals en materials d'envasament d'aliments, sent una alternativa a l'ús d'additius d'origen sintètic. En aquest treball es va observar que la viabilitat inicial dels bacteris àcid làctics (LAB) és essencial per a obtindre una bona capacitat antibacteriana pel que l'optimització de la composició de les pel·lícules o recobriments va ser crucial per a la seua aplicació amb èxit. El polímer triat com a base per a fer les pel·lícules i recobriments mitjançant la tècnica de càsting, va ser l'alcohol polivinílic, (PVOH) mesclat amb diferents proteïnes, gelatina i caseinat sòdic i les seues versions hidrolitzades afegides en diferents proporcions. En aquest estudi L. lactis va demostrar tindre una major resistència a la deshidratació durant la preparació i emmagatzematge de les pel·lícules que L. sakei. Les pel·lícules de PVOH mesclades amb gelatina hidrolitzada i caseina hidrolitzada van dotar de protecció als bacteris àcid làctics durant l'assecat i van demostrar tindre una major efectivitat antilistèria. Finalment, es va variar la proporció de caseïna hidrolitzada obtenint una millor resposta de les pel·lícules no sols des d'un punt de vista antimicrobià, sinó també de les propietats fisicoquímiques de les pel·lícules, a major proporció de caseïna hidrolitzada.Per a desenvolupar un envàs actiu antilistèria, es van adaptar les matrius per a ser aplicades com a recobriment sobre àcid polilàctic (PLA) amb l'objectiu de desenvolupar bosses actives antilistèria per a crema de bolets i com a separadors de rodanxes de pernil cuit. Els recobriments van demostrar tindre una efectivitat similar a l'obtinguda amb les pel·lícules in vitro. No obstant això, la seua eficàcia va disminuir lleugerament en ser aplicades en la crema de xampinyons i el pernil cuit a causa de la complexitat de les matrius alimentàries utilitzades, però sent una bona eina per a, al costat d'altres estratègies de conservació, assegurar la salubritat dels aliments. Es van dur a terme assajos sensorials amb consumidors i es va obtindre una bona acceptació de tots dos productes, però una alteració del sabor degut a la generació d'àcid làctic en la crema de xampinyons corregible mitjançant correctors d'acidesa sense modificació de l'efectivitat antimicrobiana. Per a desenvolupar envasos que augmentaren la vida útil, es va treballar per a ampliar l'espectre d'acció de L. lactis enfront dels bacteris Gram-negatives, normalment responsables de la descomposició dels aliments. Combinar l'agent de biocontrol productor de nisina, L. lactis, amb una baixa concentració d'àcid fític, substància quelant i desestabilitzadora de la membrana bacteriana, va ampliar l'espectre antimicrobià de L. lactis enfront dels bacteris Gram-negatives obtenint una nova eina per a garantir la seguretat alimentària i prolongar la vida útil dels aliments. / [EN] This doctoral thesis proposes different strategies for the development and application of active packaging containing biocontrol agents, to inhibit the proliferation of microorganisms such as pathogenic and spoilage bacteria and fungi, thus increasing the safety and increasing the shelf life of foodstuffs. The development of antibacterial active packaging was carried out by incorporating bacteriocin-producing lactic acid bacteria, Lactococcus lactis and Lactobacillus sakei in different film-forming matrices. Prior to the preparation of the active films, the antimicrobial activity of the selected natural agents against Listeria monocytogenes was studied. The results suggested that, from a certain initial concentration of viable bacteria, these microorganisms are good candidates to be used as natural additives in food packaging materials, being an alternative to the use of additives of synthetic origin. In this work it was observed that the initial viability of lactic acid bacteria (LAB) is essential to obtain a good antibacterial capacity, so the optimization of the composition of the films or coatings was crucial for their successful application. The polymer chosen as a base to make the films and coatings by casting technique was polyvinyl alcohol (PVOH) mixed with different proteins, gelatin and sodium caseinate and their hydrolysed versions added in different proportions. In this study L. lactis showed higher resistance to dehydration during film preparation and storage than L. sakei. PVOH films mixed with hydrolysed gelatin and hydrolysed casein provided protection to lactic acid bacteria during drying and were shown to have a greater antilisteria effectiveness. Finally, the proportion of hydrolysed casein was varied, obtaining a better response of the films not only from an antimicrobial point of view, but also from the physicochemical properties of the films, the higher the proportion of HCas. To develop an antilisteria active packaging, the matrices were adapted to be applied as a coating on polylactic acid (PLA) with the objective of developing antilisteria active bags for cream of mushroom soup and as separator liner for cooked ham slices. The coatings showed similar effectiveness to that obtained with in vitro films. However, their effectiveness decreased slightly when applied to mushroom soup and cooked ham due to the complexity of the food matrices used, but being a good tool to, together with other preservation strategies, ensure food wholesomeness. Sensory tests were carried out with consumers and a good acceptance of both products was obtained. However, an alteration of taste due to the generation of lactic acid was detected in the mushroom soup that could be corrected by means of acidity correctors without modifying the antimicrobial effectiveness. Finally, life cycle analysis of conventional and active packaging for pastry cream was studied. In any case, despite the limitations regarding the waste product estimation, shelf-life extension through packaging innovation could significantly reduce the environmental impacts of the entire food packaging system. In the present thesis, the potential use of indigenous yeasts with antifungal capacity for the control of Penicillium expansum and the control of the mycotoxin they generate, called patulin, was also explored. In the present investigation, three new yeast strains isolated from the surface of apples were selected for their efficacy against P. expansum. The yeasts were identified as Metschnikowia pulcherrima being 3 different strains. The ability of these yeasts for patulin biodegradation was also demonstrated. Then, different studies on the viability of the yeast and its antifungal effectiveness on different films made with biopolymers naturally present in apples (pectin, cellulose ethers, and apple pomace) were carried out. / The authors acknowledge the financial support of the Spanish Ministry of Economy and Competitiveness (AGL2015-64595-R and RTI2018-093452-B-I00). / Settier Ramírez, L. (2021). Envases activos portadores de microorganismos para la bioconservación de alimentos [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/175807 / TESIS / Compendio

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The selective laser melting (SLM) process allows for the control of unique part form and function characteristics not achievable with conventional manufacturing methods and has thus gained interest in several industries such as the aerospace and biomedical fields. The fabrication processing parameters selected to manufacture a given part influence the created material microstructure and the final mechanical performance of the part. Understanding the process-structure and structure-performance relationships is very important for the design and quality assurance of SLM parts. Image based analysis methods are commonly used to characterize material microstructures, but are very time consuming, traditionally requiring manual segmentation of imaged features. Two Python-based image analysis tools are developed here to automate the instance segmentation of manufacturing defects and subgranular cell features commonly found in SLM 316L stainless steel (SS) for quantitative analysis. A custom trained mask region-based convolution neural network (Mask R-CNN) model is used to segment cell features from scanning electron microscopy (SEM) images with an instance segmentation accuracy nearly identical to that of a human researcher, but about four orders of magnitude faster. The defect segmentation tool uses techniques from the OpenCV Python library to identify and segment defect instances from optical images. A melt pool structure generation tool is also developed to create custom melt-pool geometries based on a few user inputs with the ability to create functionally graded structures for use in a virtual testing framework. This tool allows for the study of complex melt-pool geometries and graded structures commonly seen in SLM parts and is applied to three finite element analyses to investigate the effects of different melt-pool geometries on part stress concentrations. / Master of Science / Recent advancements in additive manufacturing (AM) processes like the selective laser melting (SLM) process are revolutionizing the way many products are manufactured. The geometric form and material microstructure of SLM parts can be controlled by manufacturing settings, referred to as fabrication processing parameters, in ways not previously possible via conventional manufacturing techniques such as machining and casting. The improved geometric control of SLM parts has enabled more complex part geometries as well as significant manufacturing cost savings for some parts. With improved control over the material microstructure, the mechanical performance of SLM parts can be finely tailored and optimized for a particular application. Complex functionally graded materials (FGM) can also easily be created with the SLM process by varying the fabrication processing parameters spatially within the manufactured part to improve mechanical performance for a desired application. The added control offered by the SLM process has created a need for understanding how changes in the fabrication processing parameters affect the material structure, and in turn, how the produced structure affects the mechanical properties of the part. This study presents three different tools developed for the automated characterization of SLM 316L stainless steel (SS) material structures and the generation of realistic material structures for numerical simulation of mechanical performance. A defect content tool is presented to automatically identify and create binary segmentations of defects in SLM parts, consisting of small air pockets within the volume of the parts, from digital optical images. A machine learning based instance segmentation tool is also trained on a custom data set and used to measure the size of nanoscale cell features unique to 316L (SS) and some other metal alloys processed with SLM from scanning electron microscopy (SEM) images. Both these tools automate the laborious process of segmenting individual objects of interest from hundreds or thousands of images and are shown to have an accuracy very close to that of manually produced results from a human. The results are also used to analyze three different samples produced with different fabrication processing parameters which showed similar process-structure relationships with other studies. The SLM structure generation tool is developed to create melt pool structures similar to those seen in SLM parts from the successive melting and solidification of material from the laser scanning path. This structural feature is unique to AM processes such as SLM, and the example test cases investigated in this study shows that changes in the melt pool structure geometry have a measurable effect, slightly above 10% difference, on the stress and strain response of the material when a tensile load is applied. The melt pool structure generation tool can create complex geometries capable of varying spatially to create FGMs from a few user inputs, and when applied to existing simulation methods for SLM parts, offers improved estimates for the mechanical response of SLM parts.

Numerische Prozessanalysen werden heute standardmäßig zur virtuellen Prozessabsicherung der Herstellung umgeformter Blechformteile eingesetzt. Die dabei notwendige hohe Prognosegüte kann nur mit einer hinreichend präzisen Materialmodellierung realisiert werden. Ein wesentlicher Aspekt ist dabei die Modellierung des Fließverhaltens und der Werkstoffanisotropie. Zur Charakterisierung des Werkstoffverhaltens existieren zahlreiche Versuchs- und Auswertestrategien; diese werden aufgrund des hohen Versuchs- und Rechenaufwands in der industriellen Anwendung jedoch nur vereinzelt eingesetzt. Im Rahmen dieser Arbeit wird eine neuentwickelte halbanalytische Methode zur Charakterisierung von Fließortkurven sowie der Folgefließortkurven vorgestellt. Dazu wurde eine Spannungsanalyse auf Messdaten einer digitalen Bildkorrelation sowie ein Schnittlinienansatz zur Berechnung innerer Kräfte entwickelt. Durch Bilanzierung dieser inneren Schnittkräfte mit gemessenen äußeren Prüfkräften werden Parameter eines gewählten Materialmodells in einer inversen Analyse identifiziert. Die Methode zur Parameteridentifikation wurde zunächst an synthetischen und anschließend an realen Experimenten untersucht. Es wurde eine sequentielle Identifikationsstrategie aufgestellt, die an den Blechwerkstoffen DX54, DP600 sowie AA5182 untersucht wurde. Abschließend wurde die Methode mithilfe von Validierungsversuchen hinsichtlich der identifizierten Materialantworten überprüft.:Inhaltsverzeichnis I Symbolverzeichnis IV Abkürzungen und Begriffe VIII 1 Einleitung 1 2 Stand der Technik 3 2.1 Grundlagen zur Umformung von Blechwerkstoffen 3 2.1.1 Umformprozesse zur Herstellung von Blechformteilen 3 2.1.2 Anforderungen bei der Herstellung von Blechbauteilen 4 2.2 Numerische Prozessauslegung von Blechumformoperationen 5 2.2.1 Anwendung der FEM als Hilfsmittel in der Prozessauslegung 5 2.2.2 Kritische Punkte der numerischen Prozessauslegung 7 2.3 Werkstoffverhalten und Materialmodellierung 8 2.3.1 Kenngrößen zur Beschreibung großer Deformation 8 2.3.2 Grundlagen zur Beschreibung elastoplastischen Materialverhaltens 9 2.3.3 Beschreibung der Verfestigungsregel in Materialmodellen 11 2.3.4 Modellierung anisotroper Fließortkurven 12 2.3.5 Modellierung der Fließortkurvenentwicklung 18 2.3.6 Zusammenfassende Hinweise zu den Fließkriterien 25 2.4 Kennwertermittlung und Werkstoffcharakterisierung 26 2.4.1 Experimentelle Methoden und analytische Verfahren zur Fließortkurvenermittlung 26 2.4.2 Erweiterte Messtechnik zur Identifikation von Fließortkurven 33 2.4.3 Inverse Strategien zur Identifikation von Fließortkurven 36 2.5 Zusammenfassung zum Stand der Technik 43 3 Zielsetzung und Vorgehensweise 45 3.1 Zielsetzung 45 3.2 Vorgehensweise 45 4 Experimentelle Versuchsdurchführung 47 4.1 Versuchsaufbau und Messtechnik 47 4.2 Prüfverfahren zur Werkstoffprüfung 48 4.2.1 Zugversuch 49 4.2.2 Kerbzugversuch 49 4.2.3 Scherzugversuch 49 4.2.4 Biaxialer Zugversuch 50 4.3 Wahl der Versuchswerkstoffe 51 4.3.1 Kaltgewalzter Tiefziehstahl DX54 51 4.3.2 Kaltgewalzter Dualphasenstahl DP600 52 4.3.3 Aluminiumknetlegierung AA5182 52 4.4 Messergebnisse aus den Werkstoffprüfungen 53 4.5 Zusammenfassung zur Versuchsdurchführung 55 5 Entwicklung einer halbanalytischen Methode zur Parameteridentifikation 56 5.1 Spannungsanalyse 56 5.1.1 Spannungsrichtung 57 5.1.2 Spannungszuwachs 58 5.1.3 Elastische Kompensation 59 5.2 Schnittkraftermittlung 60 5.3 Inverse Analyse 62 5.4 Zusammenfassende Darstellung der Entwicklung 64 6 Validierung der Methode an virtuellen Experimenten 67 6.1 Virtuelle Versuche 67 6.2 Validierung der Spannungsanalyse 68 6.2.1 Vorgehensweise zur Prüfung der Spannungsanalyse 69 6.2.2 Ergebnisse der Überprüfung der Spannungsanalyse 70 6.3 Validierung der Schnittkraftermittlung 76 6.4 Sensitivität der Materialantwort gegenüber den Materialparametern 80 6.4.1 Einfluss variierender Fließkurvenapproximationen 80 6.4.2 Einfluss variierender Fließortkurven 82 6.5 Diskussion zur Wahl geeigneter Schnittlinien 88 6.6 Fehlerbetrachtung 89 / Numerical process analysis is widely used today for the virtual process validation of the production of formed sheet metal parts. In this context, sufficiently precise material modeling is essential, especially for the flow behavior and the material anisotropy. Numerous test and evaluation strategies are known for the material characterization. However, these strategies are only used occasionally in industrial applications due to high experimental and computational costs. In the context of this work, a newly developed semi-analytical method for the characterization of yield locus curves and subsequent yield locus curves is presented. For this purpose, a stress analysis based on digital image correlation data and a cutting-line approach for internal forces computation was developed. By balancing these internal cutting forces with measured external test forces, parameters of a material model are identified in an inverse analysis. The method for parameter identification was first examined on synthetic and subsequently on real experiments. A sequential identification strategy was set up and examined on the sheet metal materials DX54, DP600 and AA5182. Finally, the method was checked using validation tests with regard to the identified material responses.:Inhaltsverzeichnis I Symbolverzeichnis IV Abkürzungen und Begriffe VIII 1 Einleitung 1 2 Stand der Technik 3 2.1 Grundlagen zur Umformung von Blechwerkstoffen 3 2.1.1 Umformprozesse zur Herstellung von Blechformteilen 3 2.1.2 Anforderungen bei der Herstellung von Blechbauteilen 4 2.2 Numerische Prozessauslegung von Blechumformoperationen 5 2.2.1 Anwendung der FEM als Hilfsmittel in der Prozessauslegung 5 2.2.2 Kritische Punkte der numerischen Prozessauslegung 7 2.3 Werkstoffverhalten und Materialmodellierung 8 2.3.1 Kenngrößen zur Beschreibung großer Deformation 8 2.3.2 Grundlagen zur Beschreibung elastoplastischen Materialverhaltens 9 2.3.3 Beschreibung der Verfestigungsregel in Materialmodellen 11 2.3.4 Modellierung anisotroper Fließortkurven 12 2.3.5 Modellierung der Fließortkurvenentwicklung 18 2.3.6 Zusammenfassende Hinweise zu den Fließkriterien 25 2.4 Kennwertermittlung und Werkstoffcharakterisierung 26 2.4.1 Experimentelle Methoden und analytische Verfahren zur Fließortkurvenermittlung 26 2.4.2 Erweiterte Messtechnik zur Identifikation von Fließortkurven 33 2.4.3 Inverse Strategien zur Identifikation von Fließortkurven 36 2.5 Zusammenfassung zum Stand der Technik 43 3 Zielsetzung und Vorgehensweise 45 3.1 Zielsetzung 45 3.2 Vorgehensweise 45 4 Experimentelle Versuchsdurchführung 47 4.1 Versuchsaufbau und Messtechnik 47 4.2 Prüfverfahren zur Werkstoffprüfung 48 4.2.1 Zugversuch 49 4.2.2 Kerbzugversuch 49 4.2.3 Scherzugversuch 49 4.2.4 Biaxialer Zugversuch 50 4.3 Wahl der Versuchswerkstoffe 51 4.3.1 Kaltgewalzter Tiefziehstahl DX54 51 4.3.2 Kaltgewalzter Dualphasenstahl DP600 52 4.3.3 Aluminiumknetlegierung AA5182 52 4.4 Messergebnisse aus den Werkstoffprüfungen 53 4.5 Zusammenfassung zur Versuchsdurchführung 55 5 Entwicklung einer halbanalytischen Methode zur Parameteridentifikation 56 5.1 Spannungsanalyse 56 5.1.1 Spannungsrichtung 57 5.1.2 Spannungszuwachs 58 5.1.3 Elastische Kompensation 59 5.2 Schnittkraftermittlung 60 5.3 Inverse Analyse 62 5.4 Zusammenfassende Darstellung der Entwicklung 64 6 Validierung der Methode an virtuellen Experimenten 67 6.1 Virtuelle Versuche 67 6.2 Validierung der Spannungsanalyse 68 6.2.1 Vorgehensweise zur Prüfung der Spannungsanalyse 69 6.2.2 Ergebnisse der Überprüfung der Spannungsanalyse 70 6.3 Validierung der Schnittkraftermittlung 76 6.4 Sensitivität der Materialantwort gegenüber den Materialparametern 80 6.4.1 Einfluss variierender Fließkurvenapproximationen 80 6.4.2 Einfluss variierender Fließortkurven 82 6.5 Diskussion zur Wahl geeigneter Schnittlinien 88 6.6 Fehlerbetrachtung 89

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[pt] Neste trabalho é apresentado o estudo dos dispositivos orgânicos emissores de luz fosforescentes (PHOLED) baseados em compostos de baixo peso molecular. O estudo foi fundamentado nas análises dos complexos baseados no íon de Ir3+: [Ir(t-pzp)2pic] [fac-Ir(t-bupzp)3] e outros complexos já estudados anteriormente a base de Eu3+: [Eu(DBM)3PHEN] e [Eu(DBM)3DMSO2]. No desenvolvimento dos PHOLEDs, a dopagem de uma matriz orgânica com estes complexos reveste uma importância fundamental. Por tanto, como o intuito de estudar e analisar estes sistemas os complexos foram dopados com diversas concentrações em diferentes matrizes orgânicas. Os resultados obtidos revelaram que no caso dos complexos de Ir3+ os melhores valores da concentração do complexo encontram-se na faixa 13-15 porcento em peso. Já no caso dos complexos de íons de terra rara (Eu3+) as melhores concentrações devem ser superiores a 15 porcento em massa, para que ocorra uma transferência de energia eficiente e mantendo o espectro de emissão dos complexos resultando em um aumento da eficiência externa dos dispositivos. Neste trabalho foi desenvolvida também, uma metodologia que, combinando as técnicas de XRF e RBS, permite elaborar um gráfico de calibração para a determinação da concentração efetiva do dopante nos diferentes filmes co-depositados. Finalmente, para aumentar a eficiência dos PHOLEDs foi investigado o efeito da vibração do substrato durante a deposição térmica dos filmes. Os resultados indicam uma redução na densidade de aglomerados e na rugosidade, além de uma melhoria na homogeneidade dos filmes depositados. O aumento de 40 porcento na eficiência do dispositivo fabricados indica que a técnica de vibração é promissora para o desenvolvimento de dispositivos eficientes. / [en] This thesis reports the investigation of the phosphorescent organic light emitting devices (PHOLED) based on low molecular compounds. The study was carried out by analyzes the optical and electrical characteristics of thin films of Ir3+: [Ir(t-pzp)2pic] and [fac-Ir(t-bupzp)3] and other complexes based on Eu3+: [Eu(DBM)3PHEN] and [Eu(DBM)3(DMSO)2]. In developing of PHOLEDs, technology, the doping of an organic matrix with these complexes has a fundamental importance. Therefore, in order to investigate these systems Ir3+ and Eu3+ organic complexes were used as doping with a variety of concentrations in different organic matrix. The results revealed that in the case of Iridium complexes the best values are in the range 13-15 percent. On the other hand, for the rare earth complexes the best concentrations should be greater than 15 percent in order to obtain a efficient energy transfer preserving the emission spectrum of the complexes. Furthermore, the use of the doping results in an increased of the external efficiency of the device. In this work, a methodology combining the XRF and RBS techniques was also developed which allows the direct determination of the effective dopant concentration in co-deposited films through a calibration curve. Finally, to increase the efficiency of the PHOLEDs, the effect of mechanical vibration of the substrate on the thin films characteristics during the thermal deposition was investigated. The results indicate a reduction in the clusters density and film roughness, and an improved homogeneity of the deposited films. The 40 percent increase in efficiency of the devices fabricated under these conditions is a clear indication that the technology holds promise for the development of efficient devices.