Pure and Ni-doped ZnFe2O4 nanoparticles, Zn1-xNixFe2O4 (x = 0.0, 0.1, 0.2, 0.3, 0.4 and 0.5) were synthesized by microwave combustion method (MCM). The structural, morphological and magnetic properties of the products were determined by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM) and vibrating sample magnetometer (VSM). X-ray analysis showed that all the compositions crystallize with cubic spinel structure. The broadband visible emission is observed in the entire photoluminescence (PL) spectrum and the estimated energy band gap is about 2.1 eV. VSM measurements shows superparamagnetic behavior for lower concentration of Ni (x ≤ 0.2), whereas for higher concentration (x ≥ 0.2), it becomes ferromagnetic. The saturation magnetization (Ms) varies considerably with Ni content to reach a maximum value for Ni0.5Zn0.5Fe2O4 composition, i.e. 57.89 emu/g.