Abstract

The growing demand for sustainable construction materials has intensified efforts to reduce the environmental impact of Portland cement. This study investigates the effect of partial substitution of cement with metakaolin (MK, 5–15 wt.%) and biosilica (BS, 5 wt.%) on the physical, mechanical, and microstructural properties of cementitious mortars. The influence of a polycarboxylate ether-based superplasticizer (Mf) and ultrasonic treatment (ULT) was also evaluated. The mortars were characterized through setting time, density, water absorption, flexural and compressive strength tests, as well as FTIR and SEM analyses. Water absorption decreased from 12.21% to 9.8%, indicating improved pore refinement and densification. Flexural strength of all modified mortars exceeded that of the control mix: from 10.0% to 89.9% at 7 days, and from 4.7% to 50.4% at 28 days. The compressive strength improved markedly with MK and BS incorporation, from 20.8% to 51.3% at 7 days and from 9.7% to 35.2% at 28 days compared to the control sample. FTIR and SEM results confirmed enhanced pozzolanic activity and formation of C–S–H gel. The synergistic use of MK, BS, and Mf—especially with ultrasonic dispersion—yielded denser, stronger, and more sustainable cementitious composites. © 2025 by the authors.