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Estudio de compuestos Sr_2MgMo_0.9A_0.1O_6-[Delta] (A = Co, Mn y Ni) como material de ánodo SOFCs. / Study of Sr_2MgMo_0.9A_0.1O_6-[Delta] (A = Co, Mn y Ni) as SOFC anode mater.

Dager Caballero, Paola K. (2018) Estudio de compuestos Sr_2MgMo_0.9A_0.1O_6-[Delta] (A = Co, Mn y Ni) como material de ánodo SOFCs. / Study of Sr_2MgMo_0.9A_0.1O_6-[Delta] (A = Co, Mn y Ni) as SOFC anode mater. Tesis Doctoral en Física, Universidad Nacional de Cuyo, Instituto Balseiro.

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En esta tesis se desarrolló la síntesis y caracterización de compuestos dobles perovskitas Sr_2MgMoO_6 con sustituciones parciales en el sitio del Mo por metales de transición Co, Mn y Ni; es decir, Sr_2MgMo_0.9A_0.1O_6-δ (SMMA, A = Co, Mn y Ni). A la fecha de ejecución de este trabajo sólo se han reportado para el sitio-Mo, sustituciones parciales con Nb, W y V, mientras que, los metales de transición propuestos aquí han sido usados para dopar el sitio-Mg. Los compuestos Sr_2MgMoO_6 y Sr_2MgMo_0.9A_0.1O_6-δ fueron obtenidos a través de la síntesis por el método de combustión en solución y posterior tratamiento térmico en aire. Como parte de este trabajo se optimizaron parámetros relacionados con la síntesis (coeficiente estequiométrico, contenido de nitrato de amonio) y se ajustaron las condiciones de los tratamientos térmicos de manera de obtener materiales monofásicos. La mayoría de las síntesis reportadas en la literatura para los compuestos Sr_2MgMoO_6 y sus derivados se realizan por métodos de estado sólido y sol-gel bajo atmósfera reductora, y a temperaturas superiores a 1200 ºC, en esta tesis fue posible obtener los materiales monofásicos con tratamientos térmicos en aire a temperaturas de: 900 °C para Sr_2MgMoO_6 (SMMO), 1000 °C para Sr_2MgMo_0.9Mn_0.1O_6-δ (SMMMn), 1100 °C para Sr_2MgMo_0.9Ni_0.1O_6-δ (SMMNi) y 1200 °C para Sr_2MgMo_0.9Co_0.1O_6-δ (SMMCo). Los compuestos sintetizados en esta tesis presentan una estructura tipo sal de roca, formada por octaedros alternantes de Mo(A)O_6 y MgO_6 compartiendo las esquinas, con el Sr ubicado en las cavidades cubo-octaédricas. Estos materiales muestran una fase doble perovskita con grupo espacial 𝐼1̅ para polvos SMMO, SMMCo y SMMNi, e 𝐼4/𝑚 para SMMMn. A 800 °C en aire y bajo de 5%H_2 loscompuestos SMMO y SMMA, exhiben una estructura cúbica con grupo espacial 𝐹𝑚3̅𝑚. Estudios termogravimétricos, de titulación coulométrica y de difracción de neutrones desarrollados por otros autores, han reportado que el compuesto Sr_2MgMoO_6 es completamente estequiométrico (δ = 0) en aire. Sobre la base de estos resultados, se hicieron medidas termogravimétricas que permitieron determinar el contenido absoluto de oxígeno de los compuestos SMMO y SMMA bajo atmósfera de aire y de 10%H_2 a 800 ºC. Los ensayos TGA efectuados en esta tesis revelaron que bajo un flujo de 10%H_2 a 800 ºC, el compuestos Sr_2MgMoO_6-δ presenta una concentración de vacancias de oxígeno; δ ≈ 0,06. Mientras que, experimentos TGA en aire a 800 ºC mostraron que el ingreso de metales de transición; Co, Mn y Ni, con estados de oxidación menores al del Mo generan una deficiencia de oxígeno: 0,11 < δ < 0,27; en la doble perovskita Sr_2MgMoO_6-δ. Lo antes mencionado estaría asociado al cambio en el estado de oxidación del Mo (de 6+ a 5+), debido al ingreso de elementos aliovalentes a la estructura de SMMO. La concentración de vacancias de oxígeno aumentó durante las medidas termogravimétricas a 800 °C una vez que la atmósfera es cambiada de aire a 10%H2 (0,07 < ∆δ < 0,16). Experimentos de espectroscopia fotelectrónica de rayos X (XPS) “ex -situ” (antes y después de tratamiento térmico en 10%H_2 a 800 ºC durante 12h) sobre los materiales SMMO y SMMA, permitieron verificar los resultados obtenidos a través de medidas TGA. La concentración de vacancias de oxígeno (δ) en aire por el ingreso de metales de transición en la estructura del SMMO se puede explicar por la presencia de Mo"5+ en los compuestos SMMCo y SMMNi. Por otro lado, el cambio en la no-estequiometria de oxígeno (∆δ) en 10%H_2 a 800 ºC está vinculado al incremento del contenido de Mo"5+ en todos los compuestos (SMMO y SMMA). En los materiales dopados con Co y Mn también se presenta la reducción del estado de oxidación del metal de transición respectivo, lo que incrementa el número de vacancias de oxígeno. En el caso del compuesto SMMNi, los ensayos XPSposteriores a la calcinación en 10%H_2 señalan que la variación en el contenido de oxígeno (∆δ) se debe sólo al cambio de valencia del Mo. Medidas de conductividad eléctrica en aire y 10%H_2 en función de la temperatura indicaron que las dobles perovskitas SMMO y SMMA presentan una conductividad tipo-n. La incorporación de los metales de transición; Co, Mn y Ni resultó perjudicial para la conductividad de la doble perovskita Sr_2MgMoO_6 en aire, ya que los valores de conductividad disminuyeron de 3 × 10"−2 S/cm para SMMO a 1 × 10"−5 S/cm para SMMMn y SMMNi. Por otra parte, en atmósfera de 10%H_2 se observó que, la conductividad de la muestra no dopada, SMMO, fue de aproximadamente 0,7 S/cm; mientras que los compuestos dopados con los metales de transición; Co, Mn y Ni mostraron valores de conductividad de 0,8; 0,25 y 0,6 S/cm respectivamente. Los valores de energía de activación, Ea ~ 0,9 eV; calculados para los materiales dopados con Mn y Ni fueron asociados a conductividad predominantemente de tipo iónico. Por otro lado, los valores Ea ~ 0,3 eV para los compuestos SMMO y SMMCo se relacionaron con conductividad mayoritariamente electrónica. Los tamaños de granos de los compuestos SMMO y SMMA sintetizados en esta tesis, el cual estuvo en un rango entre 200 nm y 1 μm, tuvieron un impacto positivo sobre la respuesta electroquímica de los materiales, como fue visto por medidas de impedancia a 800 °C en 10%H_2. Los valores de resistencia de área específica para los compuestos SMMO y SMMA en condición de ánodo fueron hasta 2 órdenes de magnitud menores a las reportadas en la literatura. En condición de cátodo (800 °C y aire), usando el compuesto La_0.85Sr_0.15MnO_3 (LSM) como colector de corriente se observó que el ingreso de metal de transición a la estructura del compuesto Sr_2MgMoO_6 disminuye la resistencia de área específica de un valor aproximado de 10 Ωcm"2 para SMMO a 2 Ωcm"2 para SMMCo. Lo anterior, abre la posibilidad de una configuración de celda de combustible de óxido sólido simétrica (S-SOFC, del inglés: Symmetrical-SOFC), lo que disminuiría los costos de fabricación.Finalmente, estudios de difracción de rayos X a temperatura ambiente de polvos SMMO y SMMA antes y después de un tratamiento térmico en 10%CH_4 a 800 °C durante 18 h, mostraron que la estructura doble perovskita para estos compuestos se conserva. Los patrones de XRD posteriores a la calcinación en metano no mostraron picos de fases adicionales relacionados al carbón. La resistencia a la deposición de carbón de las dobles perovskitas SMMO y SMMA en comparación con polvos comerciales de Ni-CGO, hace que los compuestos Sr_2MgMoO_6 y Sr_2MgMo_0.9A_0.1O_6-δ sean particularmente atractivos para ser usados como ánodos en SOFCs que utilicen hidrocarburos ligeros como combustibles.

Resumen en inglés

In this thesis the synthesis and characterisation of Sr_2MgMoO_6 (SMMO) double perovskite compound with partial substitutions of Mo by transition metals Co, Mn and Ni; i.e, Sr_2MgMo_0.9A_0.1O_6-δ (SMMA; A = Co, Mn and Ni) was carried out. At the beginning of this work, only partial substitutions with Nb, W, and V on Mo-site hadbeen reported, whilst transition metals as those proposed here (Co, Mn and Ni) only had been used to replace Mg in SMMO compound. Sr_2MgMoO_6 and Sr_2MgMo_0.9A_0.1O_6-δ compounds were synthesised through the combustion-solution method followed by a thermal treatment in air. In order to obtain single-phase materials, several parameters related to synthesis such as stoichiometry coefficient and amount of ammonium nitrate, as well as the thermal treatment conditions were optimised. According to literature most of Sr_2MgMoO_6 compounds and its derivatives have been synthesised by solid state reaction, and sol-gel method under reductive atmosphere at temperatures above 1200 ºC. In the present thesis it was possible to obtain single phase materials at lower temperatures: 900 °C for Sr_2MgMoO_6 (SMMO), 1000 °C for Sr_2MgMo_0.9Mn_0.1O_6-δ (SMMMn), 1100 °C for Sr_2MgMo_0.9Ni_0.1O_6-δ (SMMNi) and 1200 °C for Sr_2MgMo_0.9Co_0.1O_6-δ (SMMCo). The SMMO and SMMA compounds synthesised in this thesis present a rocksalt structure formed by alternating Mo(A)O_6 and MgO_6 octahedra sharing the corners with Sr located in the cube-octahedral cavities. These materials showed a double perovskite phase with space group (s.g) 𝐼1̅ for SMMO, SMMCo and SMMNi, also 𝐼4/𝑚 for SMMMn. At 800 ºC under air and 5%H_2 atmospheres SMMO and SMMA displayed a cubic structure with s.g 𝐹𝑚3̅𝑚. Thermogravimetric, coulometric titration and neutron diffraction studies reported by other authors indicate that Sr_2MgMoO_6-δ has full stoichiometry in air (δ = 0). Based on the above mentioned, thermogravimetric analysis (TGA) measurements were performed to determine the absolute oxygen content for SMMO and SMMA compounds under air and 10%H_2 atmospheres at 800 ºC. TGA measurements indicated that Sr_2MgMoO_6-δ under 10%H_2 flux at 800 ºC displayed a concentration of oxygen vacancies, δ ≈ 0.06. The incorporation Mn, Co, Ni to the SMMO double perovskite structure increases the oxygen non-stoichiometry to values 0.11 < δ < 0.27, in air at 800 ºC. This behaviour should be mainly related toa change of the oxidation state of Mo (from 6+ to 5+) due to the incorporation of aliovalent elements to SMMO-structure. The concentration of oxygen vacancies increased once the atmosphere was switched from air to 10%H_2 (0.07 < Δδ< 0.16). “Ex-situ” X-ray photoelectron spectroscopy experiments (XPS) (before and after a thermal treatment in 10%H_2-Ar at 800 ºC for 12 h) on SMMO and SMMA materials allowed verifying the TGA results. Concentration of oxygen vacancies (δ) in air due to the partial substitution of Mo by transition metals can be explained by the presence of Mo"5+ in SMMCo and SMMNi compounds. The change of oxygen non-stoichiometry (Δδ) in 10%H_2 at 800 ºC is related to an increase of Mo"5+ content in SMMO and SMMA compounds. In addition to this, a change on the oxidation state of transition metals was also observed for the Co- and Mn-containing compounds. In regard to SMMNi compound, XPS experiments after thermal treatment in 10%H_2 indicate that the variation in oxygen content is only associated to an increase of Mo"5+ content. Electrical conductivity measurements at 800 ºC in air and 10%H_2 with temperature displayed that SMMO and SMMA exhibit n-type conductivity. The transition metal (Co, Mn or Ni) incorporation was detrimental for conductivity of Sr_2MgMoO_6 double perovskite in air. Conductivity values decreased from 3 × 10−2 S/cm for SMMO to 1 × 10−5 S/cm for SMMMn and SMMNi compounds. On the other hand, under 10%H_2 flux it was detected that, conductivity for non-doped sample was 0.7 S/cm; whilst conductivity values for SMMCo, SMMMn and SMMNi were 0.8, 0.25 and 0.6 S/cm respectively. The activation energy values, Ea < 0.9 eV for SMMMn and SMMNi double perovskitas, were associated to conductivity with a predominant ionic transport, and Ea < 0.3 eV for SMMO and SMMCo samples were mainly related to electronic conductivity. The EIS measurements at 800 ºC and 10%H_2 showed that the small grain size (200 nm - 1μm) of SMMO and SMMA compounds had a positive impact on the electrochemical response of these materials. Under condition of anode, the area specific resistance (ASR) values were up to 2 orders of magnitude smaller than those registered in literature. Meanwhile, under condition of cathode (air-800 ºC) andusing La_0.85Sr_0.15MnO_3 (LSM) compound as current collector, it was observed that Mo-substitution by transition metals (Co, Mn or Ni) on Mo-site of Sr_2MgMoO_6 structure decreases from 10 Ωcm"2 for SMMO to 2 Ωcm"2 for SMMCo. The aforementioned, opens up the possibility of a symmetrical solid oxide fuel cell (SSOFC) configuration, which would reduce fabrication costs. Finally, XRD studies at room temperature of SMMO and SMMA powders, before and after a thermal treatment under 10%CH_4 atmosphere at 800 ºC during 18 h, showed that SMMO and SMMA maintenance their double perovskita structure. The carbon-deposition resistance showed by Sr2MgMoO6 and Sr_2MgMo_0.9A_0.1O_6-δ double perovskites in comparison with Ni-CGO commercial powders indicates that SMMO and SMMA compounds shaping up as candidates for SOFC’s anodes using light hydrocarbons as fuels.

Tipo de objeto:Tesis (Tesis Doctoral en Física)
Palabras Clave:Anodes; Anodos; Perovskite; Perovoskita; Conductivity; Conductividad; [Double perovskite; Doble perovskita; Electrochemical properties; Propiedades electroquímicas]
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Materias:Física > Física de materiales
Divisiones:Gcia. de área de Aplicaciones de la tecnología nuclear > Gcia. de Investigación aplicada > Caracterización de materiales
Código ID:786
Depositado Por:Tamara Cárcamo
Depositado En:27 Feb 2019 12:17
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