The present article emphasizes the synthesis of Schiff base derived bis(1,2,3-triazolyl-γ-propyltriethoxysilanes) (3a-3d) by utilizing an efficient and biocompatible Cu(I) catalyzed 'Click Chemistry' approach. All the synthesized compounds 3a-3d have been well-characterized by IR, NMR (1H and 13C) and HRMS spectroscopic techniques. Further, 3a was immobilized over silica nanosphere and the resultant hybrid nanoparticles were thoroughly examined by IR, XRD, EDX, TGA, and SEM analysis. The photophysical properties of 3a and their hybrid nanoparticles were studied which showed dual recognition of Cu2+ and Fe3+ ions with negligible interference from other metal ions. Most importantly, hybrid nanoparticles have strong binding affinity towards Cu2+ and Fe3+ compared to compound 3a. All types of the binding interaction between chemosensors and metal ions, Cu2+ and Fe3+ got reversed upon addition of Na2EDTA. The interacting behaviour of 3a towards Cu2+ and Fe3+ ions has been studied by performing DFT calculations. © 2020 Elsevier B.V.