Nickel zinc ferrite (Ni0.8Zn0.2Fe2O4) is a soft ferrite material and can be use in electromagnetic applications that require a high permeability, such as electromagnetic wave absorbers. However synthesizing nanosize Ni0.8Zn0.2Fe2O4remains a challenge. This work deals with preparation of Ni0.8Zn0.2Fe2O4nanoparticles by using self combustion technique. The mixtures were annealed at 800 ◦C, 900 ◦C and 1200 ◦C. Characterizations were done by using X-Ray Diffractions (XRD), Raman Spectra, Field Emission Scanning Electron Microscope (FESEM) and Transmission Electron Microscope (TEM). The XRD patterns showed a major peak of  plane of the spinel cubic structure for Ni0.8Zn0.2Fe2O4samples. The average crystallites size are 20- 50 nm. Raman Spectra patterns had shown two major peaks located in the range located at in the range of 400- 700 cm-1. FESEM morphology shown hexagon shape with average dimensions of 40-140 nm. From TEM morphologies, dimension of d-spacing are 2 nm and obtain the hexagon shape of Ni0.8Zn0.2Fe2O4. As a conclusion, the best morphology of Ni0.8Zn0.2Fe2O4 was obtained at temperature of 900 ◦C.