The goal of this research is to convert iron (Fe) and aluminum (Al) waste from metal workshops, as well as silicon (Si), into innovative intermetallic nanocomposites with different characteristics that are reinforced with various quantities of hybrid fly ash and vanadium carbide (VC) for industrial usage. The microstructure, physical integrity, tribo-mechanical performance, and thermal behavior of the resultant sintered materials were all carefully examined. FeSi, FeAl, Fe₃Si, and Fe₃Al₂Si₃ were among the intermetallic phases that were formed, according to post-milling XRD examination. The bulk density of the intermetallic alloy steadily dropped as the amount of hybrid ceramic reinforcements rose, although the apparent porosity in the sintered microstructure increased. Notably, as compared to the unreinforced intermetallic alloy, the microhardness increased by 8.11%, 23.62%, 47.10%, and 84.26% in quick succession when these reinforcements were added. In comparison to the intermetallic alloy, the sample containing 16 vol% of hybrid reinforcements (FV8) achieved a Young’s modulus of 84.1% and a compressive strength of 43.2% after the addition of reinforcements. The CTE value of the intermetallic alloy was 11.88 × 10−6/ ⁰C, whereas the nanocomposite samples FV1, FV2, FV4 and FV8 have values of 11.28 × 10−6, 10.61 × 10−6, 9.14 × 10−6, and 7.10 × 10−6/ ⁰C, respectively, which can be attributed to vanadium and silica, which have lower CTE values than the matrix. Moreover, the previous results are associated with improved tribological properties of the prepared nanocomposites, as their wear rate decreased by 4.6%, 10.9%, 22.8%, and 43.2% compared to the intermetallic alloy. The average fraction coefficient decreased by 5.3%, 11.9%, 22.4%, and 39.5% for the same samples. Based on the results, recycled materials can be used in industrial applications, reinforcing the importance of recycling metal waste.