Novel propeller-like multicomponent microstructures, which are actually self-assemblies of nanoparticles ofpoly(vinyl alcohol) (PVA)-coated Ag and/or Cu
2O, were synthesized in aqueous solution of amphiphilicpolyvinylacetone (PVKA) (ketalization degree
DH = 0.549), via one-step in situ reduction of Ag
+ and Cu
2+under
-ray irradiation, utilizing the low hydrolysis rate of PVKA in the dilute acidic solution. Herein, PVAchains are obtained from hydrolyzed PVKA. The reaction mechanism and the formation mechanism areproposed. The room temperature photoluminescence spectrum has also been applied to explore the opticalproperty.