The effect of ultrasonic treatment on methanol synthesis activity of a copper/zinc/aluminum oxide catalyst has been investigated. It has been found that insonation of the suspension during co-precipitation and aging steps appreciably enhanced the activity of the catalyst and along with the increase of the frequency of the ultrasound, the enhancement grew stronger. It has also been revealed that this enhancement is due to the promotion of the ultrasound for the formation of the hydrotalcite-like phase in the precursor of the catalyst. The surface area and the STY of methanol (expressed in g/g Cu h) is linearly related to the content of the hydrotalcite-like phase in the precursor, which resulted in highly dispersed Cu (Cu1+), ZnO and Al2O3 particles in the final catalyst.