The work reports the synthesis and characterization of ternary nanoalloy catalysts of silver, bismuth, and rhenium from alkaline solutions containing L–cysteine as a complexing agent and sodium borohydride as a reducing agent. UV–Vis spectra and dynamic light scattering (DLS) analyses of the obtained colloids were performed. Additionally, high-resolution transmission electron microscope (HR–TEM) analysis assisted the former investigations. The influence of a stabilizer (PVA) was demonstrated for bismuth nanoparticles reaching an average size of 8 nm with PVA, whereas they grew large, 514 nm, in the case of synthesis without stabilizing agent. AgReBi nanoalloy particles reach an average size of 19 nm with PVA. The presence of two absorption maxima in the UV–Vis spectrum suggests shape anisotropy of these nanoparticles. TEM micrographs demonstrate the crystal structure of AgReBi nanoparticles. Cyclic voltamaperometry allows for deciphering of the catalytic properties for hydrogen peroxide electro-reduction. Both bismuth and AgReBi nanoalloy catalysts showed relatively high catalytic activity in H2O2 electro-reduction in the amperometric tests.