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Estudio de óxidos cerámicos conductores protónicos / Study of proton conducting ceramic oxides

Basbus, Juan F. (2017) Estudio de óxidos cerámicos conductores protónicos / Study of proton conducting ceramic oxides. Tesis Doctoral en Física, Universidad Nacional de Cuyo, Instituto Balseiro.

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Resumen en español

En esta tesis se obtuvieron y caracterizaron posibles materiales para Celdas Combustibles de óxido solido conductoras protónicas (Proton Conducting Solid Oxide Fuel Cell PC-SOFC). Principalmente, se estudiaron materiales de electrolito y en menor medida materiales de cátodo. Se espera que las PC-SOFC operen a menores temperaturas y posean mayores eficiencias con respecto a las SOFC e IT-SOFC. Los ceratos de bario presentan interesantes características como electrolitos conductores protónicos para PC-SOFC. Se reportó que la inclusión de Pr disminuye las temperaturas de sinterizado en los ceratos y zirconatos de bario, pero introduciría conductividad electrónica. Se evaluó el efecto de la sustitución parcial de Ce por Pr en la perovskita BaCe_1-xPr_xO_3-δ (x = 0, 0.2, 0.4, 0.6, 0.8), en sus propiedades cristalográficas, morfológicas, mecánicas y eléctricas. Se observó que el incremento de Pr en la estructura disminuye la distorsión ortorrómbica, mejora el sinterizado e incrementa la conductividad total en atmósfera oxidante húmeda. Sin embargo, el contenido de Pr disminuye la estabilidad en atmósfera reductora y reduce el rango de tolerancia al CO_2. El compuesto BaCe_0.8Pr_0.2O_3−δ (BCP) mostró las mejores características de la serie estudiada, es decir, baja porosidad, tamaño de grano micrométrico, mayor resistencia mecánica, buena tolerancia en atmósferas oxidantes y reductoras, y mayor resistencia al CO_2. Sin embargo, BCP indicó conductividad mixta dominada por huecos y vacancias de oxígeno en aire sintético entre 100 y 600 °C. Por otro lado, BCP mostró conductividad protónica en atmósfera reductora acompañada por un brusco cambio en el volumen de la celda unidad. Recientemente se propuso a la perovskita BaCe_0.4Zr_0.4Y_0.2O_3-δ (BCZY) como electrolito para PC-SOFC por su alta conductividad protónica de bulk y su excelente tolerancia el CO_2. Sin embargo, este compuesto presenta una baja conductividad de borde de grano y una alta temperatura de sinterizado (1500-1700 °C). La aplicación de BCZY en una PC-SOFC requiere del estudio sistemático en diferentes condiciones. Por lo tanto, se caracterizaron las propiedades de alta temperatura de BCZY, como la estructura cristalina, no estequiometria de oxígeno, la expansión lineal y resistencia eléctrica en atmósferas oxidantes y reductoras. BCZY mostró cambios de comportamiento en las propiedades eléctricas y en la expansión térmica lineal dependiendo de la naturaleza de la atmósfera y del vapor de agua. BCZY presentó una alta conductividad protónica de bulk y buena tolerancia al CO_2, pero la baja conductividad de borde de grano podría ser una limitante. Por lo tanto, este compuesto podría ser utilizado como electrolito para PC-SOFC y como membranas para separación isotópica siempre que se pueda procesar en forma de películas delgadas con una contribución limitada de los bordes de grano Con el objetivo de bloquear la conductividad electrónica y mejorar la resistencia al CO_2 de BCP, se depositó una película de BCZY sobre BCP (material bicapa). A partir de la caracterización electroquímica de BCP, BCZY y del material bicapa se determinó que BCP dominaría los mecanismos de transporte en el material bicapa en aire sintético e hidrogeno diluido y la película de BCZY bloquearía la conducción electrónica de BCP en aire húmedo. BCP y BCZY poseen TECs compatibles por debajo de 400 °C, por lo que el material bicapa podría operar alrededor de 400-600 °C. Las perovskitas Ba_0.5Sr_0.5Fe_0.8M_0.2O_3-δ (M = Co, Ni, Cu, Zn) fueron propuestas como cátodos para SOFC entre 600 y 800 °C (IT-SOFC). Se reportó que la sustitución de Co por metales de transición disminuye la expansión térmica lineal y la degradación química. No se encontró un estudio sistemático de estos compuestos, por lo que se caracterizaron las propiedades de alta temperatura de estos materiales. Las perovskitas Ba_0.5Sr_0.5Fe_0.8M_0.2O_3-δ (M = Co, Ni, Cu y Zn), mostraron que la conductividad eléctrica aumenta con el número atómico, (excepto para Zn), los valores de expansión térmica lineal son superiores a la mayoría de los electrolitos comunes, incluso a los estudiados en esta tesis (BCP y BCZY). Se determinó que el compuesto Ba_0.5Sr_0.5Fe_0.8Cu_0.2O_3-δ (BSFCu) posee las mejores características de la serie estudiada y se reportó que este compuesto podría ser utilizado como cátodo para PC-SOFC. A partir de los resultados obtenidos, se propone la construcción de una PC-SOFC con la siguiente estructura multicapa: Ni-BCZY/BCZY/BCP/BCP-BSFCu/BSFCu dentro del rango 400-600 °C. Los electrolitos BCZY y BCP podrían utilizarse en la industria nuclear y/o petroquímica como membranas para la producción de H_2, membranas para la separación isotópica de H/D/T en desechos nucleares, y PC-SOFC para la cogeneración de energía.

Resumen en inglés

In this thesis, possible materials for proton conducting solid oxide fuels cells (PC-SOFC) were obtained and characterized. In this thesis, was studied mainly electrolyte materials and to a lesser extent cathode materials. It is expected that PC-SOFCs operate at lower temperatures and has higher efficiencies than IT-SOFC and SOFC. The barium cerates have interesting features such as protonic conductor electrolytes for PC-SOFC. It was reported that Pr inclusion decreases sintering temperatures on barium cerates and barium zirconates, but introduces electronic conductivity. The effect of partial substitution of Ce by Pr on BaCe_1-xPr_xO_3-δ (x = 0, 0.2, 0.4, 0.6, 0.8) perovskite were evaluated into crystallographic, morphological, mechanical and electrical properties. It was observed that an increase of Pr content in the structure decreases the orthorhombic distortion, improves sintering and increases the total conductivity under wet oxidizing atmosphere. However, Pr content decreases stability under reducing atmosphere and reduces CO_2 tolerance temperature range. BaCe_0.8Pr_0.2O_3-δ (BCP) compound showed best features of the series, i.e., low porosity, micrometric grain size, higher mechanical resistance, good stability under oxidizing and reducing atmospheres, and greater resistance to CO2 atmosphere. However, BCP showed mixed conductivity dominated by oxygen vacancies and holes under wet synthetic air between 100 and 600 °C. Otherwise, BCP indicates proton conductivity under reducing atmosphere accompanied by an abrupt change in unit cell volume. Recently, BaCe_0.4Zr_0.4Y_0.2O_3-δ (BCZY) perovskite was proposed as PC-SOFC electrolyte by its high bulk proton conductivity and excellent CO_2 tolerance. However, this compound has low grain boundary conductivity and high sintering temperature (1500-1700 °C). The application of BCZY on PC-SOFC requires a systematic study under different conditions. Therefore, high temperature properties of BCZY, such as crystal structure, oxygen non-stoichiometry, linear expansion and electrical resistance under oxidizing and reducing atmospheres were characterized. BCZY showed behavior changes on electrical properties and linear thermal expansion depending on nature of atmosphere and water vapor. BCZY presented high bulk conductivity and good CO_2 tolerance, however low grain boundary conductivity could be a limiting factor. Therefore, this compound could be used as PC-SOFC electrolyte and isotopic separation membranes as long it can be processed as thin films with a limited contribution of grain boundaries. In order to block electronic conductivity and improve CO_2 resistance of BCP, a BCZY film was deposited on BCP (bilayer material). From the electrochemical characterization of BCP, BCZY and bilayer material it was determined that BCP dominates the transport mechanisms on bilayer material under synthetic air and diluted hydrogen, and BCZY film blocks electronic conduction of BCP under wet air. BCP and BCZY have similar TECs below 400 ° C, furthermore bilayer material could operate between 400-600 °C. Ba_0.5Sr_0.5Fe_0.8M_0.2O_3-δ (M = Co, Ni, Cu, Zn) perovskites were proposed such as SOFC cathodes between 600 and 800 °C (IT-SOFC). It was reported that the substitution of Co by transition metals decreases the linear thermal expansion and chemical degradation. No systematic study of these compounds was found, furthermore high temperature properties of these materials were characterized. Ba_0.5Sr_0.5Fe_0.8M_0.2O_3-δ (M = Co, Ni, Cu, Zn) perovskites showed that the electrical conductivity increases with atomic number, (except for Zn), linear thermal expansion values are higher than most common electrolytes, including those studied in this thesis (BCP and BCZY). Was determined that Ba_0.5Sr_0.5Fe_0.8Cu_0.2O_3-δ (BSFCu) compound has the best qualities of the series and it was reported that this compound could be used as PC-SOFC cathode. From the results obtained, it was proposed construction of a PC-SOFC with the following multilayer structure: Ni-BCZY/BCZY/BCP/BCP-BSFCu/BSFCu as PC-SOFC to operate between 400-600 °C. The BCP and BCZY electrolytes could be used in nuclear and petrochemical industries as membranes for H_2 purification, isotopic separation membranes of H/D/T in nuclear waste, and PC-SOFC for energy cogeneration.

Tipo de objeto:Tesis (Tesis Doctoral en Física)
Palabras Clave:Electrolytes; Electrolitos; Proton conductivity; Conductividad de protones; Barium; Bario; [Barium cerates; Cerato de bario; Proton Conducting Solid Oxide Fuel Cell; PC-SOFC]
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Materias:Química > Materiales
Divisiones:Aplicaciones de la energía nuclear > Tecnología de materiales y dispositivos > Caracterización de materiales
Código ID:1087
Depositado Por:Tamara Cárcamo
Depositado En:19 Jul 2022 13:39
Última Modificación:19 Jul 2022 13:39

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