NASICON Membrane with High Ionic Conductivity Synthesized by High-Temperature Solid-State Reaction

In the present work, we studied the impact of excess Na addition on the structure of the standard NASICON ion conductor along with Na ion transport mechanisms. In this sense, NASICON ceramic membranes (NZSP) were prepared by a simple chemical synthesis method, the solid state reaction (SSR), using an excess of 5% Na (Na_3.15Zr₂Si₂PO₁₂) and an excess of 10% Na (Na_3.3Zr₂Si₂PO₁₂), in order to improve the conduction properties of the ceramic membrane. The characterization of the NZSP nanoparticles was performed by measuring the particle size by dynamic light scattering (DLS), the morphology of the NASICON samples pre-sintered at 1100 °C was analyzed by the SEM method (scanning electron microscope), and X-ray diffraction (XRD) analysis was used to investigate the crystal structure of samples, while the surface area was measured using the BET technique. The electrical properties (i.e., ionic conductivity) were evaluated by impedance spectroscopic methods at room temperature (RT). Following the experiments for NASICON membranes without Na excess, with 5% Na excess, and with 10% Na excess synthesized at different pressing forces and sintering temperatures, it was found that membranes with a 10% Na excess, sintered at 1175 °C for 10 h, presented a good ionic conductivity (4.72 × 10^-4 S/cm).