Solution combustion synthesis has been used for the preparation of finely dispersed copper oxide, copper and copper-nickel bimetallic particles. The structure and morphology of the materials are studied by XRD and SEM techniques. The fuel content in the combustion mixture is found to be a crucial factor in controlling the formation of oxide and metal particles. Starting with copper nitrate trihydrate as oxidizer (O) and carbohydrazide as fuel (F), we obtained CuO (F/O=0.75-1), mixed valence copper oxides, CuO+Cu2O, (F/O=1.0-1.5) and metallic Cu (F/O=2). At very low fuel content (F/O=0.5), a polymeric phase of copper hydroxide nitrate is isolated from the combustion residue. We also report the use of a new organic fuel N-tertiarybutoxy-carbonylpiperazine for the preparation of Cu, Ni and CuNi bimetallic particles. (C) 2004 Elsevier B.V. All rights reserved.