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Ultrafine particles or nanoparticles (ranging from a few nanometers to 100 nm) are of considerable interest for a wide variety of applications, ranking from catalyst to luminescence ceramics, due to their unique and improved properties primarily determined by size, composition and structure. This study presents the preparation and characterization of nanostructured spherical alumina particles by the Spray Pyrolysis method for the application in reinforcements of metal-matrix composites (MMCs). Synthesis procedure includes aerosol formation ultrasonically from alumina nitrate water solution and its decomposition into a tubular flow reactor at 700 °C. The obtained particles are spherical, smooth, amorphous and in non-agglomerated state. Microstructural and morphological analyses were carried out using X-ray diffraction (XRD), scanning electron microscopy (SEM/EDS) and analytical and high resolution transmission electron microscopy (TEM/HRTEM).