Reported are the synthesis and characterization of CuS composite nanowires and microspheres in the presence of amylose. The preparation involved first the complexation of amylose with Cu 2+ of CuCl 2 at 70°C. Cu 2+ complexation was confirmed by a conductivity reduction of CuCl 2 after amylose addition. Also, the aggregation state of the amylose changed after Cu 2+ as revealed by transmission electron microscopy (TEM) and dynamic light scattering (DLS). At the Cu 2+ to α-d-glucopyranosyl unit molar ratio r of 0.70 and 1.41, the amylose aggregated into microspheres that were approximately 150 and 250nm in diameter. Adding sodium thiosulfate resulted in the production of an amorphous precipitate consisting presumably of CuS 2 O 3 . At r=0.70 and 1.41, CuS 2 O 3 precipitated inside the template of Cu 2+ /amylose microspheres as nanoparticles, while a twisted nanowire-like structure was produced at r=0.92. CuS 2 O 3 decomposed under heating at 100°C to yield crystalline CuS nanoparticles.