NiZn ferrites have been commercially used for many years as high frequency materials. Dielectric properties of Ni-Zn ferrites mainly depend on microstructure and stoichiometry. To use these materials in modern technology there is a need to obtain fine-grained structure what can be provided by selection of appropriate synthesis method. The lattice parameter increases with increase in Z n 2 + content. Surface microstructure of the sintered pellets was investigated by using atomic force microscopy. From electrical measurements it is observed that resistivity increase with decreasing zinc content. Obtained resistivity values are comparatively higher than resistivity of ferrites prepared by the conventional ceramic method due to fine grained microstructure and chemical homogeneity.