The major objective of this study was to examine the viability of using 5, 10, or 15 mass% of Activated Alum Sludge waste (AAS) instead of Ordinary Portland Cement (OPC) as a pozzolanic ingredient in concrete. This fundamental inquiry framed the investigation and OPC-AAS-hardened composites were studied to see whether they may benefit from inexpensive nanocomposites in terms of improved physical properties, mechanical strength, and resistance to heat and flame. The investigation set out to see how inexpensive nanocomposite might be put to use and the nanoparticles of CuFe2O4 spinel with an average size of less than 50 nm were successfully manufactured. Many different OPC-AAS-hardened composites benefit from the addition of CuFe2O4 spinel, which increases the composites' resistance to fire and enhances their physicomechanical properties at roughly average curing ages. Synthesized CuFe2O4 spinel was shown to have desirable characteristics by TGA/DTG and XRD. By using these methods, we were able to identify a broad variety of hydration yields, including C–S–Hs, C–A–S–Hs, C–F–S–Hs, and Cu–S–Hs, that enhance the physicomechanical properties and thermal resistivity of OPC-AAS-hardened composites as a whole. The composite material comprising 90% OPC, 10% AAS waste, and 2% CuFe2O4 has several positive economic and environmental outcomes.