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Unique functional properties of materials based on metal-polymer nanocomposites have been stimulating interests in the methods to their synthesis over the past three decades; meanwhile, the reduction of metal ions in the presence of macromolecular stabilizers is probably the most common way. In case one needs the high-purity nanocomposites with tunable size, the radiation-chemical approach becomes a particularly attractive method, since the irradiation of aqueous solutions leads to the generation of powerful and “clean” reducing species, such as hydrated electrons. The present work is concerned with the radiation-chemical synthesis of gold and silver nanoparticles in aqueous solutions and suspensions of Ag(I) and Au(III) ternary interpolymer complexes (IPC) based on poly(1-vinyl-1,2,4-triazole) (PVT) and poly(acrylic acid) (PAA), with the main attention being paid to studying the effects of the formation of such IPC on the kinetics of nanoparticle assembling and their resulting size distribution. In particular, we have shown, that ultrasmall AuNPs with an average size of 1.5 nm can be obtained by irradiation of PVT-PAA-Au(III) IPC [1]. The effective stabilization of AuNPs in this case is probably achieved due to a combination of both the electrostatic interaction of polymer units and the specific adsorption of functional groups on the nanoparticle surface.