Producing nanostructured materials through metastable phases is interesting in the field of ceramic materials. Metastable phases can be obtained by the Atmospheric Plasma Spray (APS) technique which, is a well-known technique to produce coatings. The initial powders are melted during the spraying obtaining a homogenized phase due to their solubility in the liquid state. Afterwards, the molten droplets are quenched in a cooled medium, producing the sought metastable phases. Finally, during material consolidation, the metastable structure evolves due to a dual structure. A suppression of the grain growth is produced as a consequence of the immiscibility of both phases in the solid state. Due to their small grain size and uniform structure, these nanostructured materials exhibit very interesting properties such as higher hardness and toughness. The aim of this research has been to produce nanostructured Al2O3-TiO2 ceramic powders through APS + quenching route, starting from commercially available micron-sized powders. A complete characterization of the obtained structures using XRD, SEM, FESEM and EDS has been carried out in the Thermal Spray Center (CPT) of the University of Barcelona.