On the Sintering Behavior of Nb₂O₅ and Ta₂O₅ Mixed Oxide Powders

A mixed oxide system consisting of Nb₂O₅ and Ta₂O_5, was subjected to annealing in air/hydrogen up to 950 °C for 1–4 h to study its sintering behavior. The thermogravimetric–differential scanning calorimetry (TGA–DSC) thermograms indicated the formation of multiple endothermic peaks at temperatures higher than 925 °C. Subsequently, a 30% Ta₂O₅ and 70% Nb₂O₅ (mol%) pellet resulted in good sintering behavior at both 900 and 950 °C. The scanning electron microscope (SEM) images corroborated these observations with necking and particle coarsening. The sintered pellets contained a 20.4 and 20.8% mixed oxide (Nb₄Ta₂O₁₅) phase, along with Ta₂O₅ and Nb₂O₅, at both 900 and 950 °C, indicating the possibility of the formation of a solid solution phase. In situ high-temperature X-ray diffraction (XRD) scans also confirmed the formation of the ternary oxide phase at 6 and 19.8% at 890 and 950 °C, respectively. The Hume–Rothery rules could explain the good sintering behavior of the Ta₂O₅ and Nb₂O₅ mixed oxides. An oxide composition of 30% Ta₂O₅ and 70% Nb₂O₅ (mol%) and a sintering temperature of 950 °C appeared adequate for fabricating well-sintered oxide precursors for subsequent electrochemical polarization studies in fused salts.