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Highly reactive monoclinic ZrO 2 powders were mixed with Na 3 PO 4 •12H 2 O and amorphous SiO 2 in the stoichiometric quantities to obtain Na 3 Zr 2 Si 2 PO 12 . The mixtures were calcined at different temperatures (T calc ) and for variable periods of time (t calc ). Their morphology was analysed by SEM and the composition by powder XRD. NASICON reflections are not detected for T calc =900°C and for relatively short t calc values of 2 h. At 1100°C, the onset of low intensity NASICON peaks indicate the early stages of the formation reaction which is significantly enhanced when T calc increases up to 1200 and 1300°C. For higher temperatures, an apparent decrease of the reaction rate is suggested. On the other hand, the intensities of the ZrO 2 peaks suffer a drastic decrease when T calc varies from 900 to 1300°C, followed by a slight increase for T calc =1400°C. The studies were extended for mixtures kept in isothermal conditions at 1100, 1200 and 1300°C during 0.5, 1, 2, 4, 8 and 16 h. In the three temperatures, the increase of the t calc up to ca. 4 h leads to a significant increase in the intensity of the NASICON reflections while that of mZrO 2 decreases. A plateau is apparent for higher t calc values suggesting that equilibrium may be attained. The use of a highly reactive tetragonal zirconia powder (also thermodynamically unstable at low temperature) clearly improved the overall reaction extension and kinetics at moderate temperatures, yielding a single phase product. Keywords: NASICON, microstructure, solid state reaction, XRD. Restricciones para obtener nasicon por una ruta cerámicaPolvos de ZrO 2 monoclínica altamente reactivos fueron mezclados con Na 3 PO 4 •12H 2 O y SiO 2 amorfo en cantidades apropiadas para obtener Na 3 Zr 2 Si 2 PO 12 . Las mezclas fueron calcinadas a diferentes temperaturas (T calc ) y diferentes tiempos (t calc ) y caracterizadas por SEM y DRX. Líneas características del NASICON no son detectadas a T calc =900°C y a tiempos de calcinado relativamente cortos (< 2h). A 1100°C, la presencia de picos de NASICON de baja intensidad indica los primeros momentos de la reacción de formación, la cual es significativamente mejorada cuando T calc es aumentada a 1200 y 1300°C. Para altas temperaturas (<1300ºC), se sugiere una aparente disminución de la velocidad de reacción. Por otra parte, la intensidad de los picos de ZrO 2 sufren una drástica disminución cuando T calc varía desde 900 a 1300°C, seguido de un leve incremento a T calc =1400°C. Los estudios fueron realizados manteniendo condiciones isotérmicas a 1100, 1200 y 1300°C durante 0,5, 1, 2, 4, 8 y 16 h. En las tres temperaturas, el aumento de t calc hasta 4 h conduce a un marcado aumento de la intensidad de las líneas características del NASICON, mientras que las correspondientes a mZrO 2 disminuyen. Un "plateau" es observado a valores altos de t calc , lo que sugiere que un equilibrio está siendo alcanzado. La utilización de polvos altamente reactivos de ZrO 2 tetragonal (termodinámicamente inestable a baja temperatura) mejoró claram...
Highly reactive monoclinic ZrO 2 powders were mixed with Na 3 PO 4 •12H 2 O and amorphous SiO 2 in the stoichiometric quantities to obtain Na 3 Zr 2 Si 2 PO 12 . The mixtures were calcined at different temperatures (T calc ) and for variable periods of time (t calc ). Their morphology was analysed by SEM and the composition by powder XRD. NASICON reflections are not detected for T calc =900°C and for relatively short t calc values of 2 h. At 1100°C, the onset of low intensity NASICON peaks indicate the early stages of the formation reaction which is significantly enhanced when T calc increases up to 1200 and 1300°C. For higher temperatures, an apparent decrease of the reaction rate is suggested. On the other hand, the intensities of the ZrO 2 peaks suffer a drastic decrease when T calc varies from 900 to 1300°C, followed by a slight increase for T calc =1400°C. The studies were extended for mixtures kept in isothermal conditions at 1100, 1200 and 1300°C during 0.5, 1, 2, 4, 8 and 16 h. In the three temperatures, the increase of the t calc up to ca. 4 h leads to a significant increase in the intensity of the NASICON reflections while that of mZrO 2 decreases. A plateau is apparent for higher t calc values suggesting that equilibrium may be attained. The use of a highly reactive tetragonal zirconia powder (also thermodynamically unstable at low temperature) clearly improved the overall reaction extension and kinetics at moderate temperatures, yielding a single phase product. Keywords: NASICON, microstructure, solid state reaction, XRD. Restricciones para obtener nasicon por una ruta cerámicaPolvos de ZrO 2 monoclínica altamente reactivos fueron mezclados con Na 3 PO 4 •12H 2 O y SiO 2 amorfo en cantidades apropiadas para obtener Na 3 Zr 2 Si 2 PO 12 . Las mezclas fueron calcinadas a diferentes temperaturas (T calc ) y diferentes tiempos (t calc ) y caracterizadas por SEM y DRX. Líneas características del NASICON no son detectadas a T calc =900°C y a tiempos de calcinado relativamente cortos (< 2h). A 1100°C, la presencia de picos de NASICON de baja intensidad indica los primeros momentos de la reacción de formación, la cual es significativamente mejorada cuando T calc es aumentada a 1200 y 1300°C. Para altas temperaturas (<1300ºC), se sugiere una aparente disminución de la velocidad de reacción. Por otra parte, la intensidad de los picos de ZrO 2 sufren una drástica disminución cuando T calc varía desde 900 a 1300°C, seguido de un leve incremento a T calc =1400°C. Los estudios fueron realizados manteniendo condiciones isotérmicas a 1100, 1200 y 1300°C durante 0,5, 1, 2, 4, 8 y 16 h. En las tres temperaturas, el aumento de t calc hasta 4 h conduce a un marcado aumento de la intensidad de las líneas características del NASICON, mientras que las correspondientes a mZrO 2 disminuyen. Un "plateau" es observado a valores altos de t calc , lo que sugiere que un equilibrio está siendo alcanzado. La utilización de polvos altamente reactivos de ZrO 2 tetragonal (termodinámicamente inestable a baja temperatura) mejoró claram...
All‐solid‐state sodium batteries are particularly attractive for large‐scale energy storage and electric vehicles due to their exceptional safety, abundant resource availability, and cost‐effectiveness. The growing demand for all‐solid‐state sodium batteries underscores the significance of sodium solid electrolytes. However, the existed challenges of sodium solid electrolytes hinder their practical application despite continuous research efforts. Herein, we review recent advancements and the challenges for sodium solid electrolytes from material to battery level. The in‐depth understanding of their fundamental properties, synthesis techniques, crystal structures and recent breakthroughs are presented. Moreover, critical challenges on inorganic sodium solid electrolytes are emphasized, including the imperative need to enhance ionic conductivity, fortifying interfacial compatibility with anode/cathode materials, and addressing dendrite formation issues. Finally, potential applications of these inorganic sodium solid electrolytes are explored in all‐solid‐state sodium batteries and emerging battery systems, offering insights into future research directions.This article is protected by copyright. All rights reserved
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