Pure ultrafine ZnFe 2 O 4 particles have been obtained from mechanosynthesis of the ZnO and Fe 2 O 3 oxides. The average grain diameter was estimated from x-ray diffraction to be = 36(6) nm. Refinement of neutron diffraction (ND) data showed that the resulting cubic spinel structure is oxygen-deficient, with ~7% of Fe 3+ ions occupying the tetrahedral A sites.Magnetization curves taken at 4.2 K showed absence of saturation up to fields H = 9 Tesla, associated to a spin-canted produced by the milling process. Field-cooled (FC) and zero-fieldcooled (ZFC) curves showed irreversible behavior extending well above room temperature, which is associated to spin disorder. Annealing samples at 300 °C yields an average grain size = 50(6) nm, and ~16% of Fe 3+ ions at A sites.