The development and characterization of synthesis techniques for oxide materials based on ceria is a subject of extensive study with the objective of their wide-ranging applications in pursuit of sustainable development. The present study demonstrates the feasibility of controlled synthesis of Ce1−xMxO2−δ (M = Fe, Ni, Co, Mn, Cu, Ag, Sm, Cs, x = 0.0–0.3) in combustion reactions from precursors comprising glycine, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, and cellulose as organic components. Controlled synthesis is achieved by varying the composition of the precursor, the type of organic component, and the amount of organic component, which allows for the influence of the generation of high-density electrical charges and outgassing during synthesis. The intensity of charge generation is quantified by measuring the value of the precursor–ground potential difference. It has been demonstrated that an increase in the intensity of charge generation results in a more developed morphology, which is essential for the practical implementation of ceria as a catalyst to enhance contact with gases and solid particles. The maximum value of the potential difference, equal to 68 V, is obtained during the synthesis of Ce0.7Ni0.3O2−δ with polyvinyl alcohol in stoichiometric relations, which corresponds to a specific surface area of 21.7 m2 g−1. A correlation is established between the intensity of gas release for systems with different organic components, the intensity of charge generation, morphology, and the value of the specific surface area of the samples.