Nanocrystalline Y2BaCuO5 was prepared by a co-precipitation method with aid of ultrasonic irradiation using Y2O3, CuCl2 and BaCl2 as source materials. The crystallization and morphology of the prepared nanoparticles were characterized by X-ray diffraction and transmission electron microscopy. Results showed that Y2BaCuO5 monophase can be prepared at 900°C with NaOH + NaCO3 mixture as precipitator. Particle size of Y2BaCuO5 crystallites decreases with the increase of sonicating power. Around 30 nm Y2BaCuO5 crystallites could be achieved when sonicating power increased to 300 W.