NixCo1−xFe2O4 (x = 0, 0.5, and 1) spinel nanoparticles (NPs) have been prepared using the ceramic method and
Ni0.5Co0.5Fe2O4 using green, microwave, and sol–gel routes. The as-prepared materials were characterized by XRD, FT-IR,
SEM TEM, and N2 adsorption/desorption techniques. The catalytic activity, thermal stability, and kinetic parameters of the
efect of synthesized materials upon thermal decomposition of ammonium perchlorate (AP) were studied through diferential scanning calorimetry (DSC) and thermogravimetric techniques (TG). The addition of 2 mass% of nanosized ferrites
to AP shifted the thermal degradation temperature of AP to lower temperatures. The catalytic activity for AP thermal degradation followed the order: NiCoF-gl>NiCoF-gr>NiCoF-mic>NiCoF-cer>NiF>CoF. The kinetic parameters for the
ferrite-catalyzed reaction, using the isoconversional methods for NiCoF-gl, showed a decrease in the activation energy and
preexponential factor of ammonium perchlorate thermal dissociation compared with the uncatalyzed one. The thermokinetic
parameters for the catalytic decomposition process were determined and a mechanism was suggested for the kinetic reaction. The DSC results showed that the decomposition temperatures of AP decreased with the addition of the ferrites. The
heat releases of the AP/ferrite mixtures were 0.82, 0.89, 0.91, 0.98, 1.04 and 1.23 kJ g−1 of AP, for CoF, NiF, NiCoF-cer,
NiCoF-gr, NiCoF-mic, and NiCoF-gl, respectively, compared to 0.72 kJ g−1 for neat AP.