Achieving a combination of high strength and ductility in metal-based composites is still a difficult task, and it is especially challenging in a wide temperature range. Here, nanoAl2O3/nanoAl composites with high tensile and compressive strength and excellent ductility at 25 and 500 °C were obtained using Al and Al2O3 nanopowders via a combination of high-energy ball milling (HEBM) and spark plasma sintering (SPS). Being about three times lighter than conventional high-strength steel (with a density of 2.7 g/cm3 vs. that of 7.8 g/cm3 for steel), the nanoAl2O3/nanoAl materials demonstrated tensile strength and elongation before failure comparable with those of steel. The nanoAl2O3/nanoAl composites were strengthened with two types of Al2O3 NPs, in situ formed, and introduced into the powder mixture. The resulting materials had a bimodal microstructure consisting of Al with micron and submicron grains surrounded by an Al/Al2O3 framework whose structural components were all in the size range of 20–50 nm. Among the studied compositions (0, 1, 2, 3, 4, 5, 10, and 20 wt.% of Al2O3), the Al-3%Al2O3 material showed the best thermomechanical properties, such as a tensile strength of 512 MPa and 280 MPa and a compressive strength of 489 MPa and 344 MPa at 25 and 500 °C, respectively, with an elongation to failure of 15–18%. These results show the promise of nanoAl2O3/nanoAl composites for use as small items in the automotive and aviation industries.</p
