The cobalt carbonate cuboids are prepared by adopting a simple solvothermal approach by using diethylene glycol and water in specific ratio as solvent. The prepared cobalt carbonate is subjected to different instrumentation to investigate its morphology and other properties. It is clear from the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the product is distinct cuboid in shape with a size of approximately 3 mu m from each face of the cube. Each particle of cuboid cobalt carbonate seems to comprise of layer by layer assembly of unit cells that consequently leads to a cuboid geometry. The cuboid cobalt carbonate was calcined at 700 degrees C in a furnace under argon atmosphere that decompose cobalt carbonate into porous Co3O4 with the loosely packed arrangement of nano architectures. The gas sensing properties and catalytic activity of porous cuboids Co3O4 are also investigated. (C) 2013 Elsevier Ltd. All rights reserved.