Nanocrystalline Cu3B2O6 particles were produced by ultrasonic spray pyrolysis (USP) method using aqueous solution of copper nitrate and boric acid in desired concentration. Particles obtained thermal decomposition of precursor under constant air flow rate at 1000 degrees C furnace temperature. Then samples were structurally characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS). The results show that nanocrystalline Cu3B2O6 particles in nearly spherical morphology were prepared successfully. Also, XRD analysis reveal that obtained Cu3B2O6 particles have anorthic crystal structure and their crystalline size are nearly 29 nm, which are calculated by Scherrer equation.