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Nanocrystalline zirconium oxide powder has been prepared by the glowing combustion method using sucrose as the fuel and zirconyl nitrate as an oxidant in aqueous solution. The oxidant-to-fuel ratio was optimized (0.2) to prepare nanocrystalline zirconia. The influence of calcination temperature on the phase evolution of zirconia was also studied. The prepared powder was characterized by X-ray diffraction (XRD), fourier-transform infrared spectroscopy, thermal analysis, Raman spectroscopy, particle size analysis, scanning electron microscopy, transmission electron microscopy (TEM), and surface area analysis. Powder XRD pattern itself clearly revealed the presence of metastable tetragonal phase at room temperature. Raman spectrum revealed the presence of both tetragonal and monoclinic phases. TEM and surface area studies confirmed that the particles were in the nanoregime (5–30 nm).