Copper oxide (CuO) particles with loose agglomeration of porous flakes were treated by ultrasound in different solvents. CuO particles with completely discrete flakes were obtained with ultrasonic surface treatment in ethyl alcohol as a polar solvent while CuO particles with compacted flake agglomeration were found after ultrasonic treatment in diethyl ether as a non-polar solvent. CuO particles after ultrasonic treatment were characterized to investigate the effects of morphological appearance on size distribution, sedimentation velocity, specific surface area, ultraviolet-visible (UV-vis) absorption spectra, diffraction angle of X-ray diffraction (XRD) pattern, binding energy of X-ray photoelectron spectroscopy (XPS), Raman intensity and dissolution rate. CuO particles with completely discrete flakes exhibited a fastest dissolution rate of 7 s in 12.5 vol% H2SO4 for rapid complement of cupric ions so that the electrolyte for copper electrodepositon could meet the requirement of stable concentration of cupric ions to generate fine copper deposits in a plating system with insoluble anode.