This study was aimed to study the effect of Zn content on the hyperfine parameters and the structural variation of Ni_1-xZn_xFe₂O₄ for x = 0, 0.2, 0.4, 0.6, and 0.8. To achieve this, a sol–gel route was used for the preparation of samples and the obtained ferrites were investigated by X-ray diffraction, scanning electron microscopy, and Mössbauer spectroscopy. The formation of spinel phase without any impurity peak was identified by X-ray diffraction of all the samples. Moreover, the estimated crystallite size by X-ray line broadening indicates a decrease with increasing Zn content. This result was in agreement with the scanning electron microscopy result, indicating the reduction in grain growth with further zinc substitution. The room-temperature Mössbauer spectra show that the hyperfine fields at both the A and B sites decreased with increasing Zn content; however, the rate of reduction is not the same for different sites. Moreover, the best fit parameter showed that the quadrupole splitting values of B site increased from the pure nickel ferrite to the sample with x = 0.8.