Herein, we report a novel composite material of Nb2O5@MIL–125 that exhibited enhanced photoreduction of hexavalent chromium. The composite material was fabricated through an impregnation approach, which comprised of a two-step hydrothermal synthesis. As-prepared Nb2O5 nanospheres exhibited very poor charge separation; MIL–125 (Ti) which is a Ti-based metal-organic framework was introduced into the lattice of the spheres to improve charge recombination rate. The synthesized material’s phase, crystallinity, textural and morphological studies were investigated utilizing XRD, Raman, TEM, SEM, and EDS, respectively. While the optical and photoelectrochemical behavior of the samples were obtained from UV–vis–DRS, PL, and EIS data. This data combined, illustrated the successful formation of a functional and effective heterointerface between Nb2O5 and MIL–125 (Ti). Ti introduced as the MOF in the lattice of Nb2O5 had an essential synergetic effect as the composite bearing the highest mole ratio of Ti showed higher effective photoreduction of hexavalent chromium. This was further complemented the PL and XPS data which highlighted the Nb–MIL–125 (2–3) composite to have excellent charge separation and rapid photoreduction of chromium.
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