Please use this identifier to cite or link to this item: http://repositorio.uptc.edu.co/handle/001/2584
Title: Síntesis y caracterización de óxidos nanoestructurados de cerio modificados con praseodimio para ser aplicados en pilas de combustible de óxido sólido
Authors: Cruz Pacheco, Andrés Felipe
metadata.dc.contributor.role: Gómez Cuaspud, Jairo Alberto (Director de tesis)
Parra Vargas, Carlos Arturo (Codirector de tesis)
Keywords: Perovskita
Pilas de combustible
Maestría en Química - Tesis y disertaciones académicas
Nanopartículas
Materiales de nanoestructuras
Método de combustión
Nanomateriales
Oxido de cerio
Praseodimio
SOFC
Issue Date: 2017
Publisher: Universidad Pedagógica y Tecnológica de Colombia
Citation: Cruz Pacheco, A. F. (2017) . Síntesis y caracterización de óxidos nanoestructurados de cerio modificados con praseodimio para ser aplicados en pilas de combustible de óxido sólido. (Tesis de Maestría). Universidad Pedagógica y Tecnológica de Colombia, Tunja. http://repositorio.uptc.edu.co/handle/001/2584
Abstract: Las propiedades del dióxido de cerio se deben en gran medida a la estructura cristalina tipo fluorita, la cual garantiza la movilidad de iones oxígeno y electrones tanto en la superficie como al interior del material. Además, la modificación de cationes cerio por praseodimio logra aumentar las vacancias de oxígeno debido a la interconversión de sus estados de oxidación, provocando en los sólidos, alta estabilidad estructural a altas temperaturas, acompañada de las mejoras en las propiedades de conductividad iónica y electrónica que lo hacen de gran interés para ser usado como componente en pilas de combustible de óxido sólido (SOFC). En este sentido se obtuvieron cinco óxidos de cerio modificados con praseodimio y praseodimio puro (Ce1-xPrxO2 (X = 0.0, 0.2, 0.4, 0.6, 0.8) y Pr6O11) por el método de combustión, utilizando ácido cítrico como agente quelante. Para determinar las mejores condiciones de síntesis en términos de la temperatura óptima para la consolidación de las fases cristalinas deseadas se realizaron análisis termogravimétricos y térmicos diferenciales (ATG-ATD) en un intervalo de temperatura entre 25 °C y 1000 °C. Luego de los procesos de combustión y calcinación, los sólidos obtenidos se caracterizaron por espectroscopia infrarroja con transformada de Fourier (FTIR), para determinar las bandas de absorción asociadas con las especies citrato formadas y la posterior eliminación de las mismas luego del tratamiento térmico. Las características estructurales y morfológicas que resultaron en las diferentes modificaciones del óxido de cerio después del proceso de calcinación a 800 °C se analizaron, mediante difracción de rayos X (DRX), microscopia electrónica de transmisión (MET) y microscopia electrónica de barrido (MEB), evidenciándose la obtención de cristalitos nanométricos con morfología homogénea. El comportamiento magnético de los diferentes sistemas sintetizados se evaluó mediante las medidas de magnetización en función de la temperatura y el campo magnético aplicado, dejando entrever que todas las modificaciones del óxido de cerio con iones praseodimio y el óxido de praseodimio puro presentan un comportamiento paramagnético, en contraste con el CeO2, el cual exhibe un comportamiento diamagnético. De la misma manera, los análisis de susceptibilidad magnética permitieron dar una aproximación de los estados de oxidación en los que se encuentran los iones Ce y Pr en cada uno de los óxidos sintetizados, mediante el cálculo de los momentos magnéticos efectivos. Los análisis de espectroscopia fotoelectrónica de rayos X (XPS), corroboraron los análisis magnéticos, en cuanto a la identificación de los estados de oxidación y las energías de enlace de los cationes cerio y praseodimio. Los análisis de área superficial usando isotermas de adsorción de nitrógeno, por el método BET, revelo que todos los sistemas sintetizados exhiben valores entre 70 y 135 m2 g-1, con volúmenes de poro acordes a la clasificación de materiales mesoporosos. Las medidas de capacidad de almacenamiento de oxígeno (OSC), demuestran que la sustitución proporcional de iones Ce por Pr, incrementa el almacenamiento de oxígeno debido a la generación de vacancias de oxígeno, provocadas por la presencia de iones Pr3+. Para determinar la estabilidad estructural de cada óxido sintetizado en ambientes reductores, se llevaron a cabo experimentos de reducción a temperatura programada de hidrógeno (RTP-H2), los cuales permitieron determinar que los materiales son parcialmente estables hasta 830 °C. Por último, la caracterización eléctrica mediante espectroscopia de impedancias (EI), permitió determinar los procesos de conducción eléctrica y iónica mediante el análisis de los circuitos equivalentes y los diagramas de Nyquist de todos los sólidos sintetizados y calcinados, logrando identificar el material más relevante en términos de conducción, estabilidad estructural, morfología y textura para ser un posible componente anódico en pilas de combustible de óxido sólido.
Description: 1 recurso en línea (114 páginas) : ilustraciones color, figuras, tablas.
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