Nanocomposites built from silicon oxycarbonitride amorphous materials and ZrO2 (t) nanocrystals were obtained by pyrolysis of sol-gel derived nanostructured hybrids in the Si-O-C-N-Zr system. The structure of the hybrid materials before and after pyrolysis was investigated by XRD, SEM, FTIR, Si-29 MAS NMR. Based on the data of the analyses pointed out it has been proposed a most probable cross-linking mechanism in the derived gels. The results from the preliminary experiments carried out motivate our research team to continue the study in direction of deposition of the obtained materials on metal substrates in order to improve their resistance toward oxidation and corrosion or to modify their surface properties. (c) 2005 Elsevier B.V. All rights reserved.