NiO-YSZ powder mixtures were prepared from reactive citrate-nitrate gels using the combustion route. The influence of the fuel/oxidant molar ratio in the citrate-nitrate precursor on the combustion dynamics was studied by chemical analysis and a thermoanalytical set-up combining evolved-gas analysis and thermogravimetry. It was found that the citrate-nitrate combustion reaction proceeds through several separate steps which strongly depend on the citrate/nitrate ratio prior to the combustion. The highest combustion rate and highest combustion temperature were obtained in the case of a sample with a citrate/nitrate molar ratio of 0.27. According to the EGA results, nitrate was reduced to NO and no nitrogen was formed during the combustion, while carbon from the citrate left the reaction system as a mixture of carbon dioxide and monoxide.