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A simple and easily operated supercritical CO 2 dryer was designed and manufactured with the aim of producing high-surface-area mesoporous α-Fe 2 O 3 (hematite) and NiO aerogels. The gels were synthesized by a sol−gel method with the aid of propylene oxide (PO), as the gelation agent, and then dried and calcined at different conditions. The effects of drying and calcination conditions on the physicochemical properties of the final aerogels were investigated using X-ray diffraction (XRD), N 2 adsorption-desorption, Fourier-transformed infrared spectroscopy (FT-IR), and field emission scanning electron microscopy (FE-SEM) analyses. It was demonstrated that α-Fe 2 O 3 and NiO aerogels with high surface areas and mesoporosities could be successfully synthesized using the home-made supercritical CO 2 dryer. Supercritical drying of the gels resulted in α-Fe 2 O 3 (186 m2/g) and NiO (178 m2/g) aerogels with 186% and 34% higher surface areas, respectively, than xerogels obtained via simple drying at 80°C using a laboratory oven. In addition, the results showed that supercritical CO 2 drying could enhance preservation of the porous network of the oxide nanostructures at high calcination temperatures via suppression of sintering phenomenon. Calcination of α-Fe 2 O 3 and NiO aerogels at 600°C yielded 225% and 53% higher surface areas than the corresponding xerogel, confirming the significance of drying step in the sol − gel method. Asphaltene adsorption from a model oil with asphaltene concentration of 3000 ppm indicated that the aerogels possessed higher adsorption capacities for the bulky asphaltene molecules than xerogels calcined at the same temperature of 600°C, which was due to their enhanced textural properties. [ABSTRACT FROM AUTHOR]