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The structural organization and thermomechanical properties of nanocomposites prepared from interpolyelectrolyte–metal complex (IMC) involving anionic polyelectrolyte, pectin and AgNO 3 , and cationic polyelectrolyte, poly(4-vinylpyridine), have been investigated using the methods of wide- and small-angle X-ray scattering and thermomechanical analysis. It is established that chemical reduction of Ag +  ions in the IMC by sodium borohydride results in formation of the nanocomposite based on the “pectin–poly(4-vinylpyridine)” interpolyelectrolyte complex (IPEC) and Ag 0  nanoparticles as well. At the same time, the level of nanocomposites’ structural heterogeneity is substantially enhancing, while effective size of the heterogeneity regions decreases. The nanocomposites IPEC–Ag 0  prepared are shown much bigger  T    g   value and enhanced ability for deformation than those for IMC.

X-ray Study of Structural Formation and Thermomechanical Properties of Silver-Containing Polymer Nanocomposites