A novel, nontraditional route for controlling the morphology of yttria-stabilized zirconia nanopowders is explained. For understanding the real nature of yttrium. zirconium oxalate nonisothermal decomposition and for the development of nanosize 3 mol% Y2O3-97mol% ZrO2, mass spectrometry, X-ray, and TEM investigation were used. Characteristics of zirconia crystallization under nonisothermal beating conditions were studied. Morphology evolution during Y-Zr oxalate nonisothermal decomposition was investigated to optimize the heating schedule of calcination. The nonlinear heating regime has been used to produce nanosized Y2O3-stabilized tetragonal ZrO2 powder with the finest primary crystallites and narrowest secondary aggregate size distribution.