Mechanochemical synthesis of zinc ferrite, ZnFe2O4, was attempted from a powder mixture of iron (III) oxide, alpha-Fe2O3 and zinc (II) oxide, ZnO. Nanocrystalline zinc ferrite, ZnFe2O4 powders were successfully synthesized only bymilling for 30 hours. Evidence of the ZnFe2O4 formation was absent for the powders milled for 10 and 20 hours; the milling lowered the crystallinity of the starting materials. Heating after milling enhanced the formation of ZnFe2O4, crystal growth of ZnFe2O4 and the unreacted starting materials. The unreacted starting materials decreased their amounts by heating at higher temperatures.