The NiCo ferrite has been prepared using sol-gel combustion technique making use of source materials like metal nitrates of Ni, Co and Fe. In order to reduce agglomeration, the polyvinyl alcohol has been added as a reducing agent. The characterisation studies such as XRD and TEM have been carried out to explore the particle size. An increase in particle size with an increase in calcination temperature was noticed. Similarly, the FTIR study confirms the presence of metal oxide. The above studies reveal that the sol-gel combustion technique can be used to produce a wide range of nanoparticles for different applications. © 2006 Elsevier B.V. All rights reserved.