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Extensive utilisation and manufacture of pigments and dyes have a substantial adverse effect on the ecosystem; hence, there is an immediate need for the methods to cleanse dye effluent. By utilising the Fe(II) complex of the salicyl-thiosemicarbohydrazone ligand, we suggest the synthesis of Fe2O3−FeS nanoparticles in this study. The ligand and the respective Fe(II) complex were synthesized using reported methods. The Fe2O3−FeS nanoparticles were prepared by thermal decomposition method. All the compounds were duly characterized by using UV-visible, IR, PXRD spectroscopy and SEM-EDX analysis. The synthesized Fe2O3−FeS nanoparticles were further investigated for their efficiency in the photocatalytic degradation of the dye methylene blue in the aqueous solution and the average time required for the complete photodegradation process is determined to be 25 minutes. The basic pH conditions were found to be more suitable for the catalytic dye-degradation by the current system. [ABSTRACT FROM AUTHOR]