A kind of bimetallic Cu/Co zeolitic imidazole frameworks (CuCo-ZIFs) has been successfully synthesized in ethanol solvent by ultrasound method. The morphology, structural features and physicochemical properties of CuCo-ZIFs were analyzed by several techniques including powder X-ray diffraction, thermo-gravimetric analysis, Fourier-transform infrared spectroscopy,, energy-dispersive X-ray spectroscopy, scanning electron microscope, and nitrogen physisorption measurements. The results showed that CuCo-ZIFs nanocrystals demonstrated a ZIF-67-like polyhedral morphology with high thermal stability. The Brunauer-Emmett-Teller surface areas of CuCo-ZIFs were achieved approximately 1172 m²/g, while its Langmuir surfaces areas were achieved approximately 1907 m²/g.