Five Cu–Fe/SiO₂ catalysts were prepared by deposition–precipitation, solid state impregnation, solid-state chemical reaction, citric acid combustion, and ultrasound-assisted wet impregnation, and their physicochemical and catalytic properties for higher alcohols synthesis were investigated. The results showed that the Cu–Fe/SiO₂ catalyst prepared by ultrasound-assisted impregnation had a higher dispersion and reducibility of active metal oxides, and the largest S_Cu, which increased the amount of adsorbed CO and the ability for CO dissociation. As a result, the CO conversion and space time yield of total alcohols of the catalyst reached 14.04% and 104.3 g kg⁻¹ h⁻¹, respectively, which were better than the other catalysts.