Abstract

Nanocrystalline ZnFe 2O 4 spinel powders are synthesized by high-energy ball milling, starting from a powder mixture of hematite ( α-Fe 2O 3) and zincite (ZnO). The millings are performed under air using hardened steel vials and balls. X-ray diffraction and Mössbauer spectrometry are used to characterize the powders. A spinel phase begins to appear after 3 h of milling and the synthesis is achieved after 9 h. Phase transformation is accompanied by a contamination due to iron coming from the milling tools. A redox reaction is also observed between Fe(III) and metallic iron during milling, leading to a spinel phase containing some Fe(II). The mechanism for the appearance of this phase is studied: ZnO seems to have a non-negligeable influence on the synthesis, by creating an intermediate wüstite-type phase solid solution with FeO.

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