Mn substituted ZnFe2O4 nanoparticles were prepared by the auto-combustion method using different fuel ratios of 50%, 75% and 100%.The powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectrum (EDX). Also, the dielectric behaviors of the samples were investigated for different annealing temperatures. The X-ray diffraction patterns indicated that the annealed samples resulted in the formation of crystalline powder and the presence of α-Fe2O3 as a secondary phase. The average crystallite sizes of the samples are from ~12 to 60nm. The external morphology and microstructure of the samples are tested by SEM and TEM. The effect of annealing temperature and particle size on dielectric properties such as dielectric constant (έ) and dielectric loss (D) of the spinel MnxZn1−xFe2O4 nanoparticles was measured using impedance analyzer in the frequency range 100kHz–5MHz.