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In this work, nanocrystalline powders of iron-doped zinc oxide ZnO (iron content 3, 5, and 10 at.%) were prepared utilizing co-precipitation method. X-ray diffraction, scanning electron microscopy, and the Mössbauer spectroscopy were used as complementary methods to investigate the structure and hyperfine interactions of the material. It was found that Fe dopant is incorporated into the ZnO würtzite structure. As confirmed by energy-dispersive X-ray spectroscopy the distribution of Fe dopant in the obtained samples is homogeneous up to 5 at.%. For 10 at.% of iron, spinel ZnFe2O4 phase was registered both by X-ray diffraction and the Mössbauer techniques. Paramagnetic behavior in Fe-doped ZnO was observed in the Mössbauer spectra at room temperature. Hyperfine interactions parameters indicate the presence of Fe3+ ions substituting Zn2+ions at tetrahedral sites both in the crystallite interior and near the surface of grains