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Polyimides for Piezoelectric Materials, Magnetoelectric Nanocomposites and Battery Separators: Synthesis and Characterization

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Polyimides for Piezoelectric Materials, Magnetoelectric Nanocomposites and Battery Separators: Synthesis and Characterization POLYIMIDES FOR PIEZOELECTRIC MATERIALS, MAGNETOELECTRIC NANOCOMPOSITES AND BATTERY SEPARATORS: SYNTHESIS AND CHARACTERIZATION Memoria para optar al Grado de Doctor por la Universidad del País Vasco (UPV/EHU) presentada por Alberto Maceiras Martínez Leioa, Junio 2016 (cc)2016 ALBERTO MACEIRAS MARTINEZ (cc by-nc-sa 4.0) Agradecimientos – Acknowledgements AGRADECIMIENTOS Durante los últimos años he estado rodeado por personas que me han apoyado en este viaje. Nunca hubiese sido capaz de acabar esta tesis sin su guía, ayuda o, aún más importante, sin su paciencia conmigo. Ahora es tiempo de acabar este periodo de mi vida, pero no sin antes de daros las gracias a todos. Primeramente me gustaría agradecer a la Universidad del País Vasco / Euskal Herriko Unibertsitatea (UPV/EHU) por el apoyo económico recibido para la realización de mi doctorado (Convocatoria de Ayuda para la Formación de Personal Investigador). Asímismo quiero agradecer el apoyo técnico y humano de los servicios SGIker (UPV/EHU, MICINN, GV/EJ, FEDER y FSE) Me gustaría expresar mi gratitud a mi director, Luis Manuel León, y a mi co-directora, María San Sebastián, por proporcionarme las condiciones necesarias para desarrollar mi investigación. Desearía especialmente dar las gracias a Luis por darme la oportunidad de trabajar en su grupo de investigación. Nunca olvidaré todas las cosas que has hecho por mí. Estoy agradecido por tu paciencia, cariño, confianza y amistad. También me gustaría reconocer el trabajo incansable de Matilde, ha sido verdadero placer trabajar contigo, todos sabemos lo mucho que el grupo tiene que agradecerte. Tampoco puedo olvidar a los profesores del grupo recientemente retirados, Fernando Mijangos y Maite Garay, por el cariño y las palabras amables que siempre me han brindado; ahora os toca disfrutar de la bien merecida jubilación. A Jose Luis Vilas darle las gracias por haberme permitido trabajar con él desde que me dirigió el proyecto de Máster, y desearle toda la suerte del mundo como jefe de grupo. A las nuevas profesoras del laboratorio, Leyre Pérez, Amaia Saracibar y Leire Ruiz, os deseo el mayor de los éxitos en vuestra carrera. Al Dr. José Manuel Laza, uno de los pilares indispensables del grupo, simplemente gracias por tus consejos y por todas las cosas que he aprendido contigo. Ahora quisiera agradecer a mis compañeros de laboratorio (Postdoc, doctorandos, técnicos de laboratorio, alumnos de máster y de grado) que han pasado por el Agradecimientos – Acknowledgements laboratorio en estos años y que sin duda me han hecho la vida más feliz y divertida. Por mi parte, espero haberos ayudado en todo lo posible y haber contribuido al buen ambiente. Sois muchos, así que si me olvido de alguno de vosotros os pido disculpas. A los “minions” del labo: Alain, Veronica, Nerea G., Janire, Maitane, Mari Paz, Sara, Aitor, María, Paula, Garazi, Mireia, Estela, Christian, Eva, Maru, Nerea A., Ane. ¡Gracias, colegas! En especial a Ander, gracias por esas simulaciones; espero que hayas disfrutado trabajando conmigo. Alazne, gracias por ser siempre tan dulce y simpática con todos. A Nuria, en estos años te he visto crecer mucho y en el futuro espero seguir viéndolo. A Míriam, espero que en este tiempo te lo hayas pasado tan bien conmigo como yo me lo he pasado contigo. A Erlantz, gran investigador y persona, espero poder trabajar algún día contigo y discutir juntos como se merece. A Mikel, tranquilo que no me olvido de nombrarte, algún día montaremos un spin-off utópico juntos, no te preocupes. Y por último a David, empezamos esta aventura juntos y también la terminaremos juntos, pero aunque esta etapa se termine otras nuevas vendrán, no te libras tan fácil de mí. Quiero expresar mi gratitud al Profesor Senentxu Lanceros-Mendez por darme la oportunidad de trabajar durante varios meses en su grupo de investigación (Electroactive Smart Materials Group) en la Universidade do Minho, Braga, Portugal. Asimismo, quiero dar las gracias a todos los miembros de su grupo por su inestimable ayuda, por su valía profesional y, sobre todo, por la amistad que siempre me han demostrado. Muito obrigado. Quiero agradecer al Basque Center for Materials, Applications and Nanostructures (BCmaterials) por permitirme usar sus instalaciones y equipamientos. Al Grupo de Magnetismo y Materiales Magnéticos del Departamento de Electricidad y Electrónica de la UPV/EHU, en especial al profesor Jon Gutierrez y a Andoni Lasheras, por toda su ayuda y colaboración siempre que lo he necesitado. A la profesora Aintzane Goñi del Departamento de Química Inorgánica de la UPV/EHU deseo agradecerle toda la ayuda prestada con el estudio y caracterización de los separadores de baterías. Agradecimientos – Acknowledgements Bueno, también agradecer al resto de amigos de dentro y fuera de la universidad por todos los momentos que hemos compartido. Para finalizar quiero dar las gracias a mi familia. Os debo todo. A mi familia “La ciencia no sabe de países, porque el conocimiento le pertenece a la humanidad y es la antorcha que ilumina el mundo. La ciencia es el alma de la prosperidad de las naciones y la fuente de todo progreso.” Louis Pasteur (1822 – 1895) “Cree a aquellos que buscan la verdad. Duda de los que la encuentran.” André Gide (1869 – 1951) Abstract - Resumen ABSTRACT A series of nitrile containing polyimide polymers and copolymers were synthesized, and subsequently poled by corona poling in order to provide them piezoelectric behavior. The corona poling conditions were optimized for our samples, and coefficients showed thermal stability and over time. Moreover, the influence in the piezoelectric properties of the repeating unit with two nitrile groups was studied, observing that a progressive increase in the content of the component with two nitrile groups (2CN) in the film improves the piezoelectric response. High thermal stability of polymer films was demonstrated by means of DSC and TGA, allowing their use at temperatures higher than 100ºC. Dielectric properties of the samples were determined by dielectric spectroscopy to understand the dielectric behaviour of the polyimide films. The contribution of nitrile groups in the dielectric relaxations and the types of polarization involved were analyzed. The use of polyimides in magnetoelectric (ME) nanocomposites was demonstrated for the first time. Magnetoelectric voltage coefficient was measured in a 0–3 nanocomposite film, prepared via in-situ polymerization method, using spherical cobalt ferrite nanoparticles as fillers and an amorphous copolyimide, as matrix. Different polyimide fibers were prepared by electrospinning, characterized and tested as separators for Li-ion batteries. It was the first approach in the development of gel polymer separators based in nitrile containing polyimides. Abstract - Resumen RESUMEN Se ha sintetizado una serie de poliimidas y copoliimidas que contienen grupos nitrilo en su estructura, y posteriormente han sido polarizadas por corona con objeto de dotarlas de comportamiento piezoeléctrico. Las condiciones de la polarización por corona han sido optimizadas para las muestras estudiadas, mostrando los coeficientes una buena estabilidad térmica y a lo largo del tiempo. Además, se ha estudiado la influencia en la piezoelectricidad de la unidad repetitiva con dos grupos nitrilo, observando que un incremento progresivo del contenido en el componente con dos grupos nitrilo (2CN) aumenta la respuesta piezoeléctrica. Los films poliméricos han demostrado alta estabilidad térmica mediante DSC y TGA, demostrando su uso a temperaturas superiores a 100ºC. Las propiedades dieléctricas de las muestras han sido determinadas mediante espectroscopia dieléctrica para comprender el comportamiento dieléctrico de los films de poliimida. Se ha analizado la contribución de los grupos nitrilo en las relajaciones dieléctricas y en los tipos de polarización que se ven implicados. El uso de poliimidas en nanocomposites magnetoeléctricos (ME) ha sido demostrado por primera vez en esta Memoria. Se ha medido el coeficiente magnetoeléctrico en un film de nanocomposite, preparado mediante un método de polimerización in-situ, usando nanopartículas esféricas de ferrita de cobalto como inclusión y una copoliimida amorfa, como matriz. Se han preparado diferentes fibras de poliimida mediante electrospinning (electrohilado), han sido caracterizadas y testadas como separadores para baterías de ion Litio. Ha sido la primera aproximación en el desarrollo de separadores de polímero gel basados en poliimidas que contienen grupos nitrilo. Table of contents TABLE OF CONTENTS Chapter 1. Introduction ............................................................................................................................ 1 1.1. Smart materials ................................................................................................................................. 2 1.2. Piezoelectric materials ..................................................................................................................... 6 1.2.1. Discovery and main events ....................................................................................................... 6 1.2.2. Definitions and general concepts ............................................................................................ 12 1.2.3. Types of piezoelectric materials.............................................................................................. 33 A. Ceramics .................................................................................................................................
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