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In the present study, a green, scalable, and environmentally friendly approach was developed for the fabrication of Bi2S3-decorated CdS nanoparticles with an efficient hydrogen generation ability from the water. As a sulfur source, thiourea was used. The process was completed in two stages: mechanical activation and thermal annealing. The presence of spherical CdS nanoparticles and Bi2S3 nanorods in the CdS/Bi2S3 nanocomposite was confirmed and proved by XRD, Raman spectroscopy, SEM-EDS, and TEM. The synthesized CdS/Bi2S3 nanocomposites were evaluated for their photocatalytic hydrogen evolution capabilities. The CdS/Bi2S3 photocatalyst exhibited 25% higher photocatalytic activity compared to CdS, reaching a hydrogen evolution rate of 996.68 μmol h−1g−1 (AQE 0.87%) after 3.5 h under solar-light irradiation.

CdS nanoparticles were successfully synthesized using cadmium acetate and sodium sulfide as Cd and S precursors, respectively. The effect of using sodium thiosulfate as an additional sulfur precursor was also investigated (combined milling). The samples were characterized by XRD, Raman spectroscopy, XPS, UV-Vis spectroscopy, PL spectroscopy, DLS, and TEM. Photocatalytic activities of both CdS samples were compared. The photocatalytic activity of CdS, which is produced by combined milling, was superior to that of CdS, and was obtained by an acetate route in the degradation of Orange II under visible light irradiation. Better results for CdS prepared using a combined approach were also evidenced in photocatalytic experiments on hydrogen generation. The antibacterial potential of mechanochemically prepared CdS nanocrystals was also tested on reference strains of E. coli and S. aureus. Susceptibility tests included a 24-h toxicity test, a disk diffusion assay, and respiration monitoring. Bacterial growth was not completely inhibited by the presence of neither nanomaterial in the growth environment. However, the experiments have confirmed that the nanoparticles have some capability to inhibit bacterial growth during the logarithmic growth phase, with a more substantial effect coming from CdS nanoparticles prepared in the absence of sodium thiosulfate. The present research demonstrated the solvent-free, facile, and sustainable character of mechanochemical synthesis to produce semiconductor nanocrystals with multidisciplinary application.