We present the preparation of massive Zn 1−x Fe x O ternary oxides using the mechanical mill. The Fe atom is a particular dopant since it presents two different oxidation states which allow us to vary the starting materials: Fe 2 O 3 , α-Fe or FeO. Parameters such as initial concentrations, atmosphere and milling times were varied. X-ray diffraction and 57 Fe Mössbauer spectrometry (MS) were applied in order to analyze the structure evolution and iron incorporation in the wurtzite crystalline structure with milling time. At final stages, Fe atoms seem to be incorporated in the ZnO structure for those samples milled under Ar atmosphere. In all cases, two paramagnetic components, attributed to Fe atoms in both valence states, were observed by MS.