A zinc-based MOF has been prepared by utilizing adipic acid as an aliphatic ditopic linker via both solvothermal and sonochemical methods. The ultrasound irradiation has reduced the reaction time and has led to smaller particle size. The samples were evaluated for their catalytic efficiency by the electrochemical reduction of CO2, with carbon monoxide and hydrogen being the sole products. At lower potentials (-1.5 V to -1.7 V) the ultrasound sample achieved up to 10 % better faradaic efficiency towards CO (FECO). At more negative potentials (-1.8 V to -1.9 V) the FECO of the two samples start to equalize to a maximum of around 58 %.