A facile method utilizing microwave irradiation is described that accomplishes the cross‐linking reaction of PVA with metallic and bimetallic systems. Nanocomposites of PVA‐cross‐linked metallic systems such as Pt, Cu, and In and bimetallic systems such as Pt‐In, Ag‐Pt, Pt‐Fe, Cu‐Pd, Pt‐Pd and Pd‐Fe were prepared expeditiously by reacting the respective metal salts with 3 wt.‐% PVA under microwave irradiation, maintaining the temperature at 100 °C, a radical improvement over the methods for preparing cross‐linked PVA described in the literature. The general preparative procedure is versatile and provides a simple route to manufacturing useful metallic and bimetallic nanocomposites with various shapes, such as nanospheres, nanodendrites and nanocubes.