This work reports the synthesis and microstructural characterization of a powdered composite comprised of tetragonal yttria-stabilized zirconia and cubic magnetite, fabricated using the aerosol-assisted chemical vapor deposition technique. Extensive characterization of the microstructure confirmed the formation of a powdered composite, which exhibited a spherical morphology with an irregular topography. Small amounts of monoclinic ZrO2 and Fe2O3 were also found as components of the particles. The particles exhibited a crystallite size of about 2 ± 0.5 nm. Additionally, several testing probes were prepared to assess the improvement of the mechanical properties of an Al-based metal matrix nanocomposite. The probes were prepared by mixing Al with different amounts of the particles (0.5–2.5 wt%). The addition of 1 wt% of particles exhibited the most significant results, with hardness and Yield Strength values of nearly 3 times higher than those for pure Al, while an increase of 119% in the elastic modulus was measured.
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