With the purpose of studying the cation distribution in Ni(1-x)ZnxFe2O4spinel, a series of joined ZnFe2O4-NiFe2O4spinels were synthesized by dry reaction of oxides at 1×105Pa and 1400℃in a vertical atmospheric furnace. Some of the spinels were re-equilibrated at the temperatures of 1100℃and 1600℃to show the temperature dependence of the cation distribution.Samples were quenched in H2O or liquid nitrogen. No other minerals or redidual oxides were found after run by examination with optical microscopy and powder X-ray diffraction. The lattice parameters of spinels were measured by means of powder X - ray diffraction As there are not any influence of other minerals on the diffraction peaks of spinels, the precision of most lattice parameters obtained can be determined as±0.008. At the same time,we calculated theoretically the lattice parameters of the same spinels by adjusting the cation distribution in Ni(1-x)ZnxFe2O4spinels. Finally, by comparing the lattice parameters of spinels measured from powder XRD and those obtained from calculation, we obtained the cation distribution of Ni2+, Zn2+and Fe3+in Ni(1-x)ZnxFe2O4spinel at different temperatures. The results show that, at temperatures≤1400℃, the tetrahedral sites in Ni(1-x)ZnxFe2O4spinel are occupied by Zn2+and Fe3+, whereas the octahedral sites by Ni2+and Fe3+. But at temperatures≥1600℃, it seems that the cation distribution of Ni2+, Zn2+and Fe3+in different sites are in random.The site occupancies of Fe3+in a spinel was reexamined by M ssbauer spectroscopy,which gave the result consistent with that obtained by theoretical calculation within acceptable errors (2%).