A novel ZrCO composite aerogel is synthesized using zirconium oxychloride and resorcinol-formaldehyde (RF) as precursors through the sol-gel route and carbothermal reduction process. The effects of different Zr/R molar ratios and calcination temperatures on the physical chemistry properties of ZrCO aerogels are investigated. The ZrCO composite aerogel consists of the C/ZrO2/ZrC ternary aerogel. The results show that with the increase of R/Zr molar ratios, the specific surface area and bulk density increase with calcination temperature up to 1300 A degrees C, but decrease at even temperature (1500 A degrees C). The specific surface area is as high as 637.4 m(2)/g for ZrCO composite aerogel (R:Zr = 2:1), which was higher than ever reported. As the heat-treatment temperature increases to 1500 A degrees C, the ZrC crystalline phase occurs and the t-ZrO2 phase still appears within the composite. The thermal conductivity of the carbon fiber mat-reinforced composite aerogel is as low as 0.057 W/m/K at room temperature (25 A degrees C). [GRAPHICS] .