The paper deals with preparation of nanocrystalline zinc oxide doped with iron oxide obtained via calcination process. Mixture of iron and zinc hydroxides of various composition was used as precursor of nanopowders. The zinc ferrite samples were prepared by wet chemistry method - precipitation from the corresponding metals nitrates solutions using ammonia. The obtained hydroxides were filtered, dried and calcined at 300^oC for 1 hour. Series of the samples containing 5 to 95 wt.% of Fe₂O₃ was obtained. The phase compositions of the samples were determined using XRD. Depending on the chemical composition the phases of hexagonal ZnO, and/or romboedric Fe₂O₃ and/or cubic ZnFe₂O₄ were identified. The mean crystallite size of ZnFe₂O₄ phase present in all the samples, determined using Scherrer’s formula, varied from 8 to 13 nm. The morphology of the samples was investigated using SEM and HRTEM. XPS measurements were conducted using Prevac UHV system. X-ray photoelectron spectra of all samples were analysed. Charging was reduced using neutralization cannon. Detailed spectroscopic and morphological analysis of the samples suggests core-shell model of the produced grains.

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