This study presents the synthesis, structural tailoring, and photocatalytic evaluation of zinc oxide nanoparticles (ZnO NPs) immobilized within an aluminium-silica aerogel matrix derived from aluminium waste. Nanocomposites with varying aluminium-silica aerogel loadings were prepared and denoted as ASZ1, ASZ2, ASZ3, and ASZ4, corresponding to 10 %, 20 %, 30 %, and 40 % (wt), respectively, of Al–SiO2 aerogel incorporated onto ZnO NPs. This approach addresses ZnO intrinsic photo-corrosion and the mechanical fragility of conventional silica aerogels, integrating a high-porosity, mechanically robust framework with an optically active semiconductor. The composites (ASZ1–ASZ4) were systematically characterized using XRD, FTIR, FESEM, BET-BJH analysis, UV–Vis spectroscopy, and (PL) spectroscopy to elucidate correlations between crystallinity, defect states, optical bandgap, and nanostructured morphology. BET analysis revealed a large surface area of approximately 769 m2/g for the aluminium -silica aerogel. As for the optimal formulation, ASZ3, exhibited the largest interplanar spacing (0.1845 nm), balanced lattice strain (0.004096), a red-shifted bandgap (2.82 eV), and the lowest PL emission intensity, indicative of suppressed electron-hole recombination. Morphological analysis confirmed uniform ZnO dispersion within a highly porous aerogel network with the smallest particle size of 25–40 nm for sample ASZ3, promoting efficient light harvesting and pollutant adsorption. The photocatalytic performance of the ASZ3 nanocomposite far surpassed that of pristine ZnO, achieving rapid and nearly complete MB degradation. These findings demonstrate the potential of aluminium-silica aerogel-supported ZnO as a scalable, eco-friendly platform for high-performance photocatalytic wastewater remediation.
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