High-Early-Strength Concrete Optimized with Hybrid Waste-Derived Nanomaterials: RSM-Based Design and Microstructural Analysis
High-Early-Strength Concrete (HESC) is increasingly required in accelerated construction, yet most existing studies focus on single nano-additives rather than hybrid waste-derived systems. This study investigates the individual and combined effects of nanoclay (NC), nanosilica (NS), and cellulose nanofibers (NCel)—each produced from industrial or agricultural waste—on the mechanical and microstructural properties of HESC. A Box–Behnken response surface methodology (RSM) design was employed to optimize nanomaterial dosages with respect to early-age compressive strength, while microstructural evaluation (SEM, EDS, elemental mapping) clarified the mechanisms of enhancement. The results demonstrate that NC, NS, and NCel play complementary roles in hydration acceleration, particle packing, pore refinement, and crack-bridging. The optimized hybrid system (1.64% NC, 0.115% NS, 0.027% NCel) achieved a 3-day compressive strength of 59.7 MPa, 7-day strength of 71.2 MPa, and 28-day strength of 94.6 MPa, representing increases of 42.14%, 36.92%, and 21.59%, respectively, over the control mixture. Microstructural observations confirmed matrix densification, reduced Ca/Si ratio (from 2.05 to 1.68), refined pore structure (<0.4 μm vs. 0.9–1.2 μm in control), and enhanced ITZ in the optimized mixtures. Statistical analysis yielded robust predictive models (R2 = 0.977–0.996) with significant interaction terms confirming synergistic effects among the three nanomaterials. This work demonstrates that waste-derived hybrid nano-systems offer a sustainable and effective strategy for producing high-performance HESC, with the RSM-derived optimum providing balanced early- and later-age strength while maintaining practical feasibility for field implementation.