Nanocrystalline Ni Zn Fe 2 O 4 was synthesized by milling a powder mixture of Zn, NiO, and Fe 2 O 3 in a highenergy ball mill for 30 h under three different atmospheres of air, argon, and oxygen. After sintering the 30 h milled samples at 500°C, the XRD patterns suggested the formation of a single phase of NiZn ferrite.