Ammonium perchlorate (AP) is known as the most important oxidizer in solid composite propellants and its thermal decomposition plays an important role in the burning behavior of composite propellants [1]. Thermal decomposition of AP is very sensitive to various additives such as metal oxides, mixed metal oxides spinels [2] and other types of nanomaterials. In recent years, spinel nanostructures have attracted much attention for their use as catalyst in the thermal decomposition of ammonium perchlorate [3]. ZnAl2O4 nanoparticles have high chemical and thermal resistance, high mechanical stability, and low surface acidity [4], which make it suitable candidate for a variety of applications [5]. Zinc manganite (ZnMn2O4) is known as the most attractive spinel due to its low potential of oxidation and low material cost [6]. Studies on the optical and catalytic properties of zinc aluminate and zinc manganite nanoparticles were carried out by many researchers, but to the best of our knowledge there is no report, so far, on their catalytic effect on thermal decomposition of ammonium perchlorate.In this worktwo nano spinels of zinc were synthesized by co-precipitation method and have been examined as a catalyst for thermal decomposition of ammonium perchlorate. The catalysts were mixed with AP in 97:3 ratios and examined via DSC and TGA techniques. The DSC results showed that ZnMn2O4 nanoparticles have better catalytic effect than ZnAl2O4 nanoparticles.