Pt nanoparticles and Pt/spherical carbon (SC) were prepared in a heterogeneous (PtO2/SC, water/ethanol) solid-liquid system without dispersant using ultrasound and microwave irradiation. The Pt nanoparticles and Pt/SC were characterized using X-ray diffraction (XRD), transmission electron microscopy-energy-dispersive X-ray spectroscopy (TEM-EDX), and dynamic light scattering method for particle size determination. The average size of the Pt nanoparticles prepared by only ultrasound irradiation was smaller than that prepared by microwave irradiation. Pt nanoparticles were successfully prepared by microwave irradiation with a reaction time of several minutes at a specific concentration of diluted ethanol. Pt/SC prepared by combined ultrasound and microwave irradiation resulted in fine particles with good homogeneous distribution.