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Transition metal sulphide-loaded fly ash–based EU-12 photocatalysts were synthesized by sono-hydrothermal method followed by ion exchange. The composites were characterized by XRD, FESEM, DSC-TGA, Raman spectroscopy, and BET surface area analysis. The XRD results imply 76.39% crystallinity of EU-12 and morphological studies by FESEM, and TEM revealed the shape and size of EU-12, i.e. rod-shaped with size ranging from 5 to 200 nm. Band gap of all synthesized photocatalysts were found to be?≤?3.44 eV. The photoactivities of the photocatalysts were examined by degrading rhodamine B (RhB). The results indicated that metal sulphide/EU-12 composite had the strong photoactivity under visible light compared to dark environment. Furthermore, the efficiency of photocatalysts was determined in terms of degradation efficiency towards RhB which was found to be maximum of 98.62% for 0.2 M CdS/EU-12 at 2 gL?1 of catalyst dosage and 10 ppm of dye concentration within 3 h under visible light source of 200 W.

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