CuO-CoO-MnO/SiO2 nanocomposite aerogels were prepared by using tetraethyl orthosilicate (TEOS) as Si source, and aqueous solution of Cu, Co and Mn acetates as transition metal sources via sol-gel process and supercritical drying (SCD) technique. The effect of synthesis conditions on gelation was investigated. The composition of the nanocomposite aerogels was characterized by electron dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The specific surface area of the nanocomposite aerogels was determined by the Brunauer-Emmett-Teller (BET) method. The results show that the range of optimal temperature for gelation is 30-45 °C, and the pH is 3.0-4.5. CuO-CoO-MnO/SiO2 nanocomposite aerogels are porous with a specific surface area of 384.9-700.6 m2/g. Compared to CO2 SCD, ethanol SCD is even favorable to the formation of aerogel with high specific surface area. The transition metals content in the nanocomposite aerogels can be controlled to be 0.71-13.77 at.%.