Disk-like Cu microcrystals were successfully synthesized with assistance of ultrasonic irradiation. The products were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), selected area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS), and thermogravimetric/differential thermal analysis (TGA/DTA). It was found that as-prepared Cu microcrystals were single crystals in nature and had a high crystallinity. They were mainly composed of disk-like and triangular Cu microcrystals with an average diameter of about 1 mu m. There existed CuO on the outermost surface of the products, while a thin layer of Cu2O was found between CuO and inner Cu microcrystals. Moreover. CTAB molecules were adsorbed on the surface of Cu microcrystals and they were desorbed while heated during TGA analysis. In addition, the influences of magnetic stirring, stillness, concentration of hexadecyltrimethylammonium bromide (CTAB) surfactant, and starting Cu salts on the morphology and size distribution of the final products have also been studied. (C) 2010 Elsevier B.V. All rights reserved.