A Al
2O
3/Fe
2O
3 mesoporous composite has been prepared with a nanoscale casting process using activatedcarbon as template in supercritical carbon dioxide (SC CO
2). The composite precursor of iron(III)acetylacetonate (Fe(acac)
3) and aluminum acetylacetonate (Al(acac)
3) and acetone were dissolved in supercriticalCO
2 and then coated on activated carbon in the desired supercritical conditions. After removal of activatedcarbon template by calcination in air at 600
C, a Al
2O
3/Fe
2O
3 mesoporous composite was obtained.Temperature, pressure, and composite precursor ratio effects were studied. X-ray diffraction pattern provedthat the product was composed of
-Al
2O
3 and
-Fe
2O
3. Dendritic nanocrystals were observed from TEMgraphs. SEM results show that the porous structure of activated carbon template was well replicated bycomposite product. The product pore structure information was calculated from the nitrogen sorption isotherms.