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.

Zirconium dioxide (ZrO ₂ ) is widely recognized for its outstanding mechanical, thermal, and optical properties, making it a material of choice for advanced applications in catalysis, coatings, and other structural applications. In this study, monoclinic ZrO ₂ is ball milled for various milling durations up to 40 h, and changes in the microstructure and phase are identified. A dominant monoclinic phase is observed along with a minor tetragonal phase when milled beyond 10 h, with corresponding crystallite size reduction and enhanced surface area with increased milling duration. The examined photoluminescence spectra revealed a noticeable reduction in the peak intensity, which is attributed to a drop in the charge recombination. The deconvolution of photoluminescence spectra indicates the suitability of 20 h sample for enhanced catalysis. In line with this, the catalytic reduction-assisted degradation of rhodamine B (RhB) demonstrated a substantial increase in the catalytic activity for the 20 h sample, with about 97.11% degradation in 40 min, verifying the suitability of ball milled ZrO ₂ as an efficient catalyst for wastewater treatment.