The ZnO and ZrO2 powders were prepared by mechanochemical processing and subsequent heat treatment of the starting powder of precursors mixture of ZnCl2 and Ca(OH)2, and ZrOCl2·8H2O and NaOH, respectively. Inert salt matrix, ether CaCl2 or NaCl, which prevents particle agglomeration was formed during mechanochemical solid state reaction. After mechanochemical treatment, samples were calcined at various temperatures. Selective removal of the matrix phase by washing the resulting powder with appropriate solvent yields almost pure ZnO and ZrO2 powders. Characterization of the powders was performed by X-ray diffraction (XRD), differential thermal and thermo gravimetric analysis (DTA−TG) and scanning electron microscopy (SEM).