A three-dimensional (3-D) metal-organic framework (MOF) with 3-D channels, i.e. Cu-3(BTC)(2) (HKUST-1, BTC = benzene-1,3,5-tricarboxylate), was synthesized by using ultrasonic method for the first time. The reaction of cupric acetate and H3BTC in a mixed solution of DMF/EtOH/H2O (3:1:2, v/v) under ultrasonic irradiation at ambient temperature and atmospheric pressure for short reaction times (5-60min) gave Cu-3(BTC)(2) in high yields (62.6-85.1%). These Cu-3(BTC)(2) nano-crystals have dimensions of a size range of 10-200 nm, which are much smaller than those synthesized using conventional solvothermal method. There were no significant differences in physicochemical properties, e.g. BET surface area, pore volume, and hydrogen storage capacity, between Cu-3(BTC)(2) nano-crystals prepared using ultrasonic method and the microcrystals obtained by using improved solvothermal method. Compared with traditional synthetic techniques, such as solvent diffusion technique, hydrothermal and solvothermal methods, ultrasonic method for the construction of porous MOFs was found to be highly efficient and environmentally friendly. (C) 2008 Elsevier B.V. All rights reserved.