Flower-like NiAl-LDH/BiVO ₄ Z-scheme photocatalysts for sunlight-driven degradation of azo dye: performance and mechanistic insights

Layered double hydroxide (LDH)-based materials have garnered significant attention as versatile photocatalysts for environmental remediation, particularly for the abatement of dye-laden wastewater, owing to their structural tunability, chemical robustness, and facile synthetic routes. In this context, a series of NiAl-LDH/BiVO₄ (NAL/BV) Z-scheme heterojunction nanocomposites were constructed by loading 5-15% (wt%) of BiVO₄ onto LDH <i>via</i> an <i>ex situ</i> fabrication method, and evaluated for photocatalytic degradation of Congo red (CR), a typical azo dye, under solar irradiation. The structural, morphological, and optical attributes of the nanocomposites were meticulously elucidated through comprehensive analyses, including XPS, FTIR, PL, UV-DRS, FESEM, HRTEM, and BET surface area measurements. The optimized 5-NAL/BV composite exhibited a flower-like morphology with an augmented surface area, promoting efficient charge separation and enhanced photocatalytic activity. At a catalyst loading of 0.3 g L^-1, it achieved 94.3% CR degradation within 2 hours, with an apparent kinetic rate constant of 0.01673 min^-1 and a synergy factor of 5.67. The effects of contaminant concentration, catalyst dose, pH, and light source on activity were systematically studied. TOC analysis confirmed 50% mineralization, while scavenging studies identified superoxide radicals as the primary reactive species. HRMS analysis elucidated degradation intermediates, and post-cycle characterization confirmed structural stability over six cycles. Moreover, a comparative analysis with previously reported studies demonstrates that this hybrid acts as a superior photocatalyst for the decomposition of hazardous dyes, highlighting the potential of NAL/BV nanocomposites for solar-driven wastewater treatment and environmental remediation.