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Summary:The synthesis and characterization of porous nanostructured cobalt oxide (Co 3 O 4 ) aerogels using epoxide addition method is described. Cobalt-containing monoliths were obtained by sol-gel processing of an alcoholic cobalt chloride solution with propylene oxide as the gelation agent. The alcogels were dried by supercritical CO 2 fluid extraction to obtain the highly porous amorphous cobalt (II) aerogels. To enhance and control the structural properties of the aerogels, single-walled carbon nanotubes (SWCNT) were incorporated into the cobalt (II) aerogel network to form a homogenous composite material. The resulting materials were characterized using powder X-ray diffraction and nitrogen adsorption/desorption analysis. The detailed microstructure of aerogel networks was investigated using scanning and transmission electron microscopy, which showed significant structural changes induced by the incorporation of SWCNT to the cobalt aerogel. Annealing of the aerogel materials at 6001C yields a highly crystalline well-faceted Co 3 O 4 network SCANNING 31: 132-138, 2009. r