Structural, optical, and magnetic properties of ferrite series with chemical formula Zn0.5NixMg0.5-xFe2O4 (x = 0.0, 0.1, 0.2, 0.3 and 0.4) were investigated. Co-precipitation and sol-gel methods were used to synthesis the samples and to investigate further the influence of these preparation methods on the properties of Zn0.5NixMg0.5-xFe2O4 nano-ferrites. X-ray diffraction and Fourier-transform infrared spectroscopy revealed that the samples crystallize in a cubic spinel structure with space group Fd3m:1. The crystallite size of Zn0.5NixMg0.5-xFe2O4 nanoparticles was decreased from 19.15 to 11.65 nm with increasing Ni content for the samples of co-precipitation method, while the opposite behavior was observed in case of sol-gel method which was increased from 13.90 to 21.90 nm. Moreover, the optical investigation by UV-visible spectroscopy revealed that the energy band gap of the samples of co-precipitation method ranged (6.04 - 6.08) eV compared to (4.44 - 4.50) eV of sol-gel method. For both methods, substitution of Ni+2 by Mg+2 in Zn0.5NixMg0.5-xFe2O4 affects the remanent magnetization (Mr), coercivity (Hc) and saturation magnetization (Ms) suggesting the super-paramagnetic behavior of the samples. The substitution of Ni resulted in small values of coercivity ranged 0.758 to 164.62 Oe. The Ms was ranged 20.39 to 127.57 emu/g and an enhancement in magnetization was observed which increases the value of Ms that was found to be maximum with x=0.4 of co-precipitation method (127.57 emu/g). The magnetic behavior of synthesized Ni doped nanoparticles makes them suitable candidate for sensing and high-frequency applications and for use in hyperthermia treatment. The characterization outcomes may recommend that co-precipitation method is preferred over sol-gel method for refined structure and preferable properties of Zn0.5NixMg0.5-xFe2O4 nanoparticles.