By ultrasonic wave irradiation, the metallic ions in aqueous solution are reduced to metallic nanoparticles. Using the mixture solution of Au and Pd ions, core(Au)-shell(Pd) structured nanoparticles are prepared. Au-197 Mossbauer spectra of core-shell structured nanoparticles contains two components, one is pure Au component due to the inner part of the Au core and the other is the positive isomer shift component due to the alloy layer at the interface of Au core and Pd shell. The thickness of the alloy layer is 0.5similar to0.7 nm.