Hematite (α-Fe2O3), magnetite (Fe3O4), and maghemite (γ-Fe2O3) are only a few of the polymorphic forms of iron oxide, a mineral component. Hematite and maghemite, solid propulsion technology nanoparticulate materials, perform exceptionally well during the thermal degradation of ammonium perchlorate. Due to their larger particle size, more active sites, and increased surface area, which encourages more gas adsorption during thermal oxidation reactions, metallic iron oxide nanoparticles have an enhanced catalytic impact. Currently, a variety of techniques, including co-precipitation, sol–gel, microemulsion, and thermal decomposition, can be used to create metallic iron nanoparticles. The literature contains information on these synthetic processes, but there is a dearth of information on nanoparticulate oxides and the methods used to characterise them. The methods for generating nanoparticulate iron oxides, the key features of the various characterization techniques, as well as information regarding the breakdown properties of these nanomaterials are presented in this concise review based on scientific papers, containing data from the last two decades. Transmission electron microscopy, scanning electron microscopy, X-ray powder diffraction, and Fourier transform infrared spectroscopy can all be used to describe the morphologies and structures of iron oxides. Physical adsorption techniques are typically used to determine the textural qualities.