Aerogels have high porosity and specific surface area, as well as the ability to maintain textural stability at high temperatures, making them good heterogeneous catalysts. Catalytic performance can be enhanced by adding metal salts in the synthesis process. One application of great interest of catalytic aerogels is found in their potential to replace the environmentally unfriendly three-way-catalysts (TWCs) employed in automobile catalytic converters. Characterization can provide information about aerogels' microstructure (availability of catalyst sites), which can reveal ways to optimize catalytic efficiency. Alumina aerogels were synthesized by two different methods and with varying amounts of copper using the patented Union College rapid supercritical extraction (RCSE) method. These aerogels were then characterized using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). Copper(0) microrods and microparticles were identified, as well as microcrystals containing copper and chlorine (the latter from the alumina aerogel precursor). The catalytic activity of aerogels prepared with different copper loading was assessed using the Union Catalytic Aerogel Testbed (UCAT).