The high-resolution X-ray diffraction profiles observed at room temperature for NZFO ceramics are presented in Fig.1,which reveals that the stucture of the sample has a perfect spinel structure (space group:Fd3m[o]).The structure parameters of Ni Zn FeO wewe refined by Reitveld analysis with Rwp=23.23%and Rp=13.97%,as a=8.388อังสตรอม similar to the NiFeO and ZnFeO crystal data reported by Bid et al.via the same method. X-ray data analyses show clearly that Ni, Zn,Fe cations can occupy either tetrahedral or octahedral sites. Nonetheless, it is hard from refinements to obtain specific information on local cation environments owing to partial occupation of cations in both sites.