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Estudio De Mejora De Las Propiedades De Polímeros Conductores Electrogenerados

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Estudio De Mejora De Las Propiedades De Polímeros Conductores Electrogenerados Departamento de Ingeniería Química “Estudio de mejora de las propiedades de polímeros conductores electrogenerados. Verificación de parámetros de aplicación tecnológica.“ Margarita Sánchez Jiménez Directores de Tesis: Francesc Estrany Coda Carlos Alemán Llansó Memoria presentada para aspirar al grado de Doctor por la Universidad Politécnica de Cataluña Programa de Doctorado Polímeros y Biopolímeros Grupo Innovación en Materiales e Ingeniería Molecular (IMEM) Junio 2017 II A mi querida familia Nuestras horas son minutos cuando esperamos saber, y siglos cuando sabemos lo que se puede aprender. Antonio Machado III IV Agradecimientos En primer lugar quisiera agradecer a mis directores de tesis Dr. Francesc Estrany y Dr. Carlos Alemán la oportunidad que me brindaron de realizar este trabajo en el grupo de investigación IMEM. Han demostrado tener mucha paciencia en la guía y el estímulo de mi trabajo. También quisiera agradecer su colaboración directa en algún momento de la parte experimental a la Dra. Elaine Armelin (microscopia óptica, sonicación), Dra. Montserrat Domínguez (soporte técnico), Dr. Francesc Estrany (AFM), Dr. Joan Aymami (XRD), Dra. Lourdes Franco (DSC) y Dr. Trifón Trifonov (SEM y EDX). Una mención aparte merecen los compañeros: Dra. Mª del Mar Pérez (SEM) y Dra. Georgina Fabregat (SEM y EIS) y Sr. Rafael Peres (ensayos termoeléctricos) que también han contribuido directamente en la parte experimental de esta tesis. Con Damia Amoura también hubo una colaboración muy especial que resultó fructífera para ambas en un capítulo de esta tesis. No podía faltar una mención a Mari Cruz Saborío con la que sigo colaborando para mejorar nuestro conocimiento mutuo del software para el control de algunos de los potenciostatos empleados en la línea de investigación. Y por pequeñas ayudas puntuales pero vitales respecto a otros softwares quisiera mencionar a Aureli Calvet por su infinita paciencia. Gracias a todos por vuestra colaboración desinteresada. Para la elaboración de ciertos puntos del apartado 1.6 de esta memoria con conceptos puramente electrónicos y en labores de asesoramiento en uno de los estudios debo agradecer también la colaboración inestimable del Ingeniero Electrónico Sr. Francisco Casellas. Por último y no menos importante destacar el importante papel de soporte de la familia y amigos que en los momentos de desánimo se han mantenido firmes a mi lado. Por los que están ahí y los que ya no están con nosotros. V VI Resumen Desde su descubrimiento, las espectaculares propiedades de los polímeros llamados “conductores” han suscitado un importante campo de estudio en aras de conseguir su conocimiento y su aplicación comercial en multitud de campos como los que se repasan en el capítulo 1 (apartado 6) de la presente tesis. El gran potencial que presentan los polímeros conductores, pasa por facilitar y mejorar los procesos de polimerización. Pero también por encontrar formas de obtener materiales con propiedades electroactivas acordes con las aplicaciones correspondientes. La presente tesis presenta en el tercer capítulo el estudio de la optimización de las condiciones de electropolimerización de dos polímeros conductores como son Poli(3,4-etilendioxitiofeno) (PEDOT), Poli(N-metilpirrol) (PNMPy) y sistemas tricapa formados por films alternos de los dos PCs anteriores. Dicha mejora se enfoca en dos aspectos: Reducción de la concentración de monómero en la solución de generación y aplicación simultánea de condiciones dinámicas en dicha solución durante la electropolimerización. En la práctica ha consistido en disminuir a la quinta parte la concentración de monómero habitual y en mantener agitada la solución con una barra magnética sumergida. Reducción de la concentración de electrolito dopante, manteniendo la concentración de monómero en el valor reducido anterior y la agitación de la solución como en el caso anterior. Esta segunda disminución solo ha sido aplicada a PEDOT. Los dos aspectos se han empleado con el fin de disminuir la carga contaminante de las soluciones agotadas, reduciendo el impacto ambiental en la fabricación de films de PCs. Además se ha mantenido e incluso intentado incrementar las propiedades electroactivas de los PCs. También se ha tratado de demostrar la eficacia del método realizando una aplicación en un supercapacitor. En el cuarto capítulo, la tesis desarrolla estudios de electrogeneración y caracterización de las propiedades de los materiales compuestos obtenidos con base de PNMPy y dos tipos de incorporaciones: Nanopartículas de Cu obtenidas por reducción de una solución acuosa de CuCl2. VII Nanopartículas del óxido de molibdeno (VI) o MoO3 en suspensión en una mezcla acetonitrilo-agua. Con la obtención de estos materiales compuestos se ha pretendido modular las propiedades electroactivas del PNMPy. En el quinto capítulo se presenta el estudio de obtención de films tricapa constituidos por películas alternas de PEDOT y PNMPy, cuya capa intermedia incorpora un material dieléctrico como la arcilla denominada montmorillonita (MMT). Se ha relacionado la influencia de la arcilla en las propiedades respecto al espesor de las capas interna y externa de PEDOT. Estos materiales se han caracterizado para su aplicación como supercapacitores eléctricos. En el sexto capítulo se desarrolla un tratamiento térmico sencillo sobre films de PEDOT generado en solución de acetonitrilo y de agua desionizada que modifica su estructura física con incremento de la conductividad. Se ha buscado la naturaleza de los cambios estructurales producidos según el disolvente utilizado en la electrogeneración. VIII Abstract Since its discovery, the spectacular properties of polymers called "conducting" have given rise to an important scope of study in order to obtain their knowledge and commercial application in many fields such as those reviewed in the first chapter of this thesis. To achieve the greatest potential of the conducting polymers (CP) it is needed to improve and make easier the polymerization processes. It’s required to find some ways to obtain conducting polymer based materials with electric properties in accordance with the corresponding applications. In the second chapter, the experimental methodology applied for the development of the studies that constitute the later chapters has been exposed. This chapter also has included all the analytical techniques used. The study of the optimization of the electrochemical polymerization conditions of two conducting polymers such as poly (3,4-ethylenedioxythiophene) (PEDOT), poly (N- methylpyrrole) (PNMPy) and three-layered systems formed of alternating films from the two previous CPs has been presented in the third chapter. This improvement has been divided into two phases: The reduction of the monomer concentration in the solution and simultaneous application of dynamic flow conditions therein during the electrochemical generation. The reduction of the concentration of supporting electrolyte, keeping the monomer concentration at the previous reduced value and stirring the solution as in the previous case. This second decrease has only been applied to PEDOT. The purpose of these studies has been to decrease the pollutant load of depleted solutions, reducing the environmental impact in the CP films manufacturing, which has also maintained and even increased some of the properties of their electrical response. It has also been demonstrated the effectiveness of the method by making an application in a supercapacitor. In the fourth chapter, studies about electrolytic polymerization and characterization of the properties of composites materials obtained with a PNMPy base and two types of incorporations have been developed as: Cu nanoparticles obtained by reduction reaction of an aqueous solution of CuCl2. IX Nanoparticles of molybdenum oxide (VI) suspended in an acetonitrile-water mixture. Making these composite materials it has been pursued to modulate the electroactive properties of the PNMPy. Fifth chapter has been focused on the study of obtaining PEDOT and PNMPy alternating layers to form three-layered films whose intermediate layer incorporates a dielectric material such as montmorillonite (MMT) clay. The influence of this type of clay has been related to the properties regarding the thickness of the PEDOT inner and outer layers. These materials have also been characterized for their application as supercapacitors. Finally, PEDOT films generated in acetonitrile and deionized water solutions have been subjected to a simple thermal treatment whose results have been studied in chapter sixth. This treatment has caused an increase in the material conductivity that has been associated to a modification of its physical structure, which depended on the solvent used in the anodic polymerization. The nature of the structural changes promoted by the thermal treatment has also been analysed. X Índice Agradecimientos…….…………………………………………………………… V Resumen…………....……………………………………………………………... VI Abstract……………………………………………………………………………. IX Índice……………………………………………………………………………….. XI Objetivos…………………………………………………………………………… XVII Glosario de abreviaturas y símbolos..……………………………………….. XXI Publicaciones y contribuciones a conferencias........................................ XXIX 1. INTRODUCCIÓN………………………………………………………………. 1 1.1. Antecedentes……………………………………………………………… 3 1.2. Propiedades de los monómeros implicados………..………………….. 6 1.2.1. 3,4-Etilendioxitiofeno (EDOT)...…………………………...... 8 1.2.2. N-metilpirrol (NMPy).……………………………..………...... 9 1.3. Propiedades de los polímeros objeto de estudio……..……………….
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