In order to obtain cobalt oxides nanoparticles we have used the thermal decomposition of some carboxylate type precursors. These precursors were obtained by the redox reaction between cobalt nitrate and ethylene glycol, either bulk or dispersed in silica matrix. The redox reaction takes place by heating the Co(NO3)2·6H2O-C2H6O2 solution or the Si(OC2H5)4-Co(NO3)2·6H2O-C2H6O2 gels. Thermal analysis of the Co(NO3)2·6H2O-C2H6O2 solution and Si(OC2H5)-Co(NO3)2·6H2O-C2H6O2 gels allowed us to establish the optimal value for the synthesis temperature of the carboxylate precursors. By fast heating of the solution Co(NO3)2·6H2O-C2H6O2, the redox reaction is immediately followed by the decomposition of the precursor, which represents an autocombustion process. The product of this combustion contains CoO as unique phase. We have obtained a mixture of CoO and Co3O4 by annealing the synthesized carboxylate compounds for 2 h at 400°C. With longer annealing time (6 h), we have obtained Co3O4 as unique phase. The XRD study of the crystalline phases resulted by thermal decomposition of the precursors embedded in silica matrix, showed that the formation of Co2SiO4 and Co3O4, as unique phases, depends on the thermal treatment.