In this research paper the dielectric properties such as Ddielectric loss (tan δ), AC conductivity, Dielectric constant (real part ε' and imaginary part ε") and dielectric loss tangent (tan δ) are reported for the series [Cox Ni(constant) Cu0.8-x Fe2O4] where constant=0.2 with x=0.2, 0.4 and 0.6 of ferrites, prepared by Sol-Gel autocombustion technique by using high purity metal nitrate, double distilled water and citric acid as a catalyst. The variation in the real part of dielectric constant(ε') , imaginary part of dielectric constant ( ε") , dielectric loss tangent (tan δ)and AC conductivity are studied at room temperature in the frequency range of 100 Hz to 5 MHz. Structural characterization of the annealed samples was done with the help of X-ray diffraction method. The particle size and single phase formation of CoNiCuFe2O4 ferrite was confirmed by X-ray diffraction analysis. The particle size of prepared sample was confirmed by Scherer's formula. The effect on Particle size (t) and lattice constant (Å) is observed due to substitution of Co2+ in Ni Cu. The impedance meter (LCR meter) is used to obtain the Dielectric properties of prepared pallets. The variations in the structural and dielectric properties of the prepared ferrite material are discussed.