An yttria‐stabilized zirconia powder, free of monoclinic phase, may be prepared by an oxalate method in an ethanol solution at strong acidity. This study demonstrates that the control of pH in the preparation of precursors has a significant effect on the ability of precursors to crystallize and hence plays an important role in determining the formation and fraction of various crystalline phases in the resulting yttria‐stabilized zirconia powder. With the increase of pH, a precursor with a certain crystalline form may be transformed into an amorphous precursor, and a monoclinic phase appers in the phase composition of the resulting powder. The results of XRD analysis and Raman spectroscopy are discus