The studies of the synthesis of uranium carbide from uranyl-ascorbate gels using the complex sol-gel process (CSGP) have been carried out. The synthesis of uranyl-ascorbate mixture as liquid sol from uranium trioxide and ascorbic acid and solid gel by extraction of water from sol were carefully examined. Ascorbic acid was used as a complexing agent in complex sol-gel process and as a carbon source. The crucial step to obtain final uranium carbides from the aforementioned substrates is the carbonization process. The thermal behavior of ascorbic acid and uranyl-ascorbate gels in a nitrogen atmosphere in the temperature range of 25-900°C were investigated using TG-DTG. Furthermore, the products of the carbonization of uranyl-ascorbate gels in nitrogen, argon and vacuum atmosphere were identified by X-ray diffraction. TG-DTG was used also as a method for determining of carbon residues in the samples.