This work reports the synthesis of sodium and vanadium co-doped zirconia, resulting in the stabilized cubic zirconia phase (Na/VSZ). The general formula for the solid solution formed is Zr1-2xVxNaxOδ, where δ denotes the oxygen deficiency. Solid solutions with nominal compositions of x = 0.01, 0.03, and 0.06 were prepared via the sol-gel method, using zirconium(IV) propoxide solution (Zr(OCH2CH2CH3)4) and sodium metavanadate (NaVO3) as precursors. The resulting gels were annealed at different temperatures. Annealing at 400 °C for 2 h produced highly crystalline cubic Na/VSZ nanoparticles, which transformed into the tetragonal phase at 610 °C and finally into the monoclinic phase after subsequent annealing at 900 °C. This method enabled the preparation of Na/VSZ nanopowders at a relatively low temperature compared to conventional ceramic methods. Sodium-vanadium stabilized zirconia (Na/VSZ) exhibits high structural stability compared to yttria-stabilized zirconia (YSZ), which is attributed to the high concentration of oxygen vacancies generated by the co-doping of Na+ and V4+. The band gap of Na/VSZ was estimated to be 3.02 eV, a value significantly lower than the 5.18 eV band gap reported for pure ZrO2. XRD results indicated that the samples annealed at 400 °C consist of Na/VSZ with a cubic fluorite structure, which is maintained up to 570 °C. Rietveld refinements confirmed the incorporation of Na+ and V4+ ions into the 4a Wyckoff sites of the cubic zirconia lattice. EDX analysis verified the chemical composition of Na/VSZ. UV–Vis and EPR spectra revealed the presence of V4+ ions within the zirconia. Na/VSZ has potential for applications such as sensors, photocatalysts, electrolytes in solid oxide fuel cells (SOFCs), and components in electronic devices.
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