Phase and Microstructure Modifications in Monoclinic Zirconia: Synergistic Effects of Extended Ball Milling and Annealing

The structural response of ceramics to extreme deformation is of significant scientific and technological relevance since such conditions are commonly encountered during both processing and service. In this study, monoclinic zirconia was subjected to high-energy ball milling for extended durations of 80 h and 120 h, followed by annealing at 1000 °C. X-ray diffraction revealed a progressive increase in the tetragonal phase content with milling duration, while subsequent annealing promoted its consolidation alongside the principal monoclinic phase, resulting in a stable biphasic structure. The phase evolution is also evaluated through a Raman spectroscopy analysis and correlated with the morphology, mechanical properties, and surface area analyses. Scanning electron microscopy confirmed the preservation of nanoscale features in the milled and annealed specimens, in contrast to the unmilled sample, which exhibited pronounced grain coarsening. The combined presence of nanostructural stability and biphasic phase constitution underscores the efficacy of high-energy ball milling, in conjunction with thermal treatment, as an effective strategy to tailor the microstructure and phase stability of zirconia ceramics for advanced engineering applications.