RESUMEN
Metal-organic frameworks (MOFs) are hybrid materials that are being explored as active electrode materials in energy storage devices, such as rechargeable batteries and supercapacitors (SCs), due to their high surface area, controllable chemical composition, and periodic ordering. However, the facile and controlled synthesis of a pure MOF phase without impurities or without going through a complicated purification process (that also reduces the yield) are challenges that must be resolved for their potential industrial applications. Moreover, various oxide formations of the Ni during Ni-MOF synthesis also represent an issue that affects the purity and performance. To resolve these issues, we report the controlled synthesis of nickel-based metal-organic frameworks (NiMOFs) by optimizing different growth parameters during hydrothermal synthesis and by utilizing nickel chloride as metal salt and H2bdt as the organic ligand, in a ratio of 1:1 at 150 °C. Furthermore, the synthesis was optimized by introducing a magnetic stirring stage, and the reaction temperature varied across 100, 150, and 200 °C to achieve the optimized growth of the NiMOFs crystal. The rarely used H2bdt ligand for Ni-MOF synthesis and the introduction of the ultrasonication stage before putting it in the furnace led to the formation of a pure phase without impurities and oxide formation. The synthesized materials were further characterized by powder X-ray diffraction (XRD) technique, scanning electron microscopy (SEM), and UV-vis spectroscopy. The SEM images exhibited the formation of nano NiMOFs having a rectangular prism shape. The average size was 126.25 nm, 176.0 nm, and 268.4 nm for the samples (1:1)s synthesized at 100 °C, 150 °C, and 200 °C, respectively. The electrochemical performances were examined in a three-electrode configuration, in a wide potential window from -0.4 V to 0.55 V, and an electrolyte concentration of 2M KOH was maintained for each measurement. The charge-discharge galvanostatic measurement results in specific capacitances of 606.62 F/g, 307.33 F/g, and 287.42 F/g at a current density of 1 A/g for the synthesized materials at 100 °C, 150 °C, and 200 °C, respectively.
RESUMEN
This work presents the structural and electrical characterization of K2NiF4-type layered perovskites of LaSrAl1-xMgxO4-δ composition to be used as oxide-ion electrolytes for a solid-oxide fuel cell (SOFC). These perovskites were prepared by mechano-chemical synthesis (ball milling), an alternative to traditional synthesis methods such as citrate-nitrates and solid-state reaction. With these methods, two things are avoided: first, the use of nitrate salts, which are more environmentally harmful than oxide precursors, and second, it saves the series of long thermal treatments associated with solid-state reactions. After grinding the precursors, nanometric particles were obtained with a combination of crystalline regions and amorphous regions; this effect was determined by XRD and TEM, showing that Mg has a positive effect on the phase formation by only mechanical synthesis. R2C4: After sintering, it was found by XRD that the sample x = 0.1 only presents the diffraction peaks corresponding to the desired phase, which shows a phase purity greater than 97%, even higher than that of the standard undoped sample. For x = 0.2 and 0.3, there was a segregation of impurities, possibly by the local migration of La and Sr heavy cations; this was determined by SEM and EDS. The electrical characterization of the sintered pellets was carried out by electrochemical impedance spectroscopy, which determined that the incorporation of Mg in the structure improves the ionic conductivity by three orders of magnitude, obtaining conductivities of 1.6 mS/cm at 900 °C for x = 0.2. Although the improvement in conductivity is considerable, many challenges such as densification, the segregation of impurities, and the study of mechanical and thermal properties must be carried out on these materials to endorse them as solid electrolytes in SOFC.