Solution combustion synthesized (SCS) cobalt oxide (Co3O4) powder has been studied as a catalyst precursor for the hydrolysis of sodium borohydride (NaBH4). Synthesis is completed in less than two minutes and results indicate SCS is capable of reproducibly synthesizing 98.5-99.5% pure Co3O4 nano-foam materials. SCS materials demonstrate an as-synthesized specific surface area of 24 m(2) g(-1), a crystallite size of 15.5 nm, and fine surface structures on the order of 4 nm. Despite having similar initial surface areas and sample purities, SCS-Co3O4 outperforms commercially available Co3O4 and elemental cobalt (Co) nano powders when used as a catalyst precursor for NaBH4 hydrolysis. Hydrogen generation rates (HGR) using 0.6 wt% NaBH4 in aqueous solution at 20 degrees C were observed to be 1.24 +/- 0.2 L min(-1) g(cat)(-1) for SCS nano-foam Co3O4 compared to 0.90 +/- 0.09 and 0.43 +/- 0.04 L min(-1) g(cat)(-1) for commercially available Co3O4 and Co, respectively. The high catalytic activity of SCS-Co3O4 is attributed to its nano-foam morphology and crystallinity. During the hydrolysis of NaBH4, the SCS-Co3O4 converts in-situ to an amorphous active catalyst with a specific surface area of 92 m(2) g(-1) and exhibits a honeycomb type morphology. Copyright (C) 2013, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.