Advancing a facile one-pot synthetic approach for the fabrication of a hybrid heterojunction photocatalyst remains a significant challenge in research pursuits. Herein, a microsphere-like trinary hybrid nanocomposite has been synthesized (NH/PIn/MAA/Ag). It comprises exfoliated single- and a few-layered Ni(OH)2 (NH nanosheets), mercaptoacetate-functionalized polyindole (PIn/MAA), and Ag nanoparticles (AgNPs) through an in situ approach. The formation mechanism is based on the exfoliation of stacked Ni(OH)2 multilayers [i.e., Ni(OH)2 microflowers] and stabilization of NH nanosheets through host-guest formation of PIn/MAA, followed by the adsorption-reduction of Ag+ ions in a one-pot reaction at low temperature. Surface morphological analyses of hybrid nanocomposite microspheres have exhibited that highly dense Ni(OH)2 microflowers have been transformed into low-density layered forms (NH nanosheets) within the polymeric platform (PIn/MAA) with deposited AgNPs. An interfacial heterojunction has been developed between the components in the depletion region, leading to an improvement in photocatalytic efficiency through a synergistic effect over the components for charge separation and transfer through the heterojunction interface via solid-state mediator Ag-based Z-scheme charge transfer dynamics. The superior photocatalytic degradation of tetracycline (98.2%) by trinary hybrid microspheres can be attributed to the deteriorated recombination rate of electron-hole pairs with reduced charge transfer resistance of the heterojunction in the photocatalyst, as obvious from photoluminescence, electrochemical impedance spectroscopy, chronoamperometry, and time-resolved photoluminescence (TRPL) analyses. Moreover, the antibacterial properties of microspheres against Bacillus pumilus (Gram-positive) and Escherichia coli (Gram-negative) bacteria have validated their potential as promising materials for the overall purification of aquatic systems.
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