This article presents the effect of NiO, a transitional metal oxide substitution on dielectric and magnetic studies of zinc ferrite (ZnFe2O4). NiO was substituted in pure zinc ferrite (ZnFe2O4) samples with the basic composition (1-x) ZnFe2O4 + (x) NiO (here, x= 0.0, 0.05, 0.1, and 0.15), were synthesized by wet chemical method using auto-combustion method with the help of the precursors such as nitrates and an organic fuel such as citrate in this case