Ceramic materials formed by complex metal oxides are assuming a very important role on the scientifically and technological development. The synthesis by reaction of combustion is of particular interest once it is a very quick and cheap method to obtain products with both levels of purity and excellent reproducibility. The method is based on a highly exothermic reaction that provides the necessary energy for the chemical transformation and the obtaining of reasonable ceramic products. This result must be confirmed by JCPDF 52-0279 chart, obtained products are monophasic. The present work aims to synthesize and characterize the Zn 0,5 Ni 0,5 Fe 2 O 4 in order to relate the micro-structural properties. The analysis of the thermal treatment effect generates a duplication of the crystallinity values related to material. The thermal treatment leading to a rising of the crystallinity of sample confirmed by the crystallite size of 422.4nm.