Foam-like nanocomposites of the Ce–Fe–O system with two (c-CeO2, am-F2O3), three (c-CeO2, o-CeFeO3, α-F2O3), or four phases (c-CeO2, o-CeFeO3, α-F2O3, am-Fe2O3) were synthesized using the RedOx reaction of glycine-nitrate combustion. The glycine/nitrate ratio (G/N) varied from deficient (0.2, 0.4) and stoichiometric (0.6) to excess ratios of glycine (0.8, 1.0, 1.2, 1.4). PXRD, 57Fe Mössbauer spectroscopy, N2-physisorption, TEM, H2-TPD, O2-TPD, and H2-TPR were used to examine the characteristics of the obtained samples. The average crystallite size of the obtained composites was in the range of 1.3–31.3 nm, 33.4–50.7 nm, and 10.1–33.9 nm for c-CeO2, o-CeFeO3, and α-Fe2O3, respectively. The lowest SBET (1.5 m2/g) belonged to the case of stoichiometric G/N, while the highest value (49.2 m2/g) was found in the case of the highest amount of glycine (G/N = 1.4); the latter case also had the largest total pore volume (Vp = 0.182 cm3/g) when compared to the others. Moreover, the advanced catalytic performance of foamy Ce–Fe–O-based nanocomposites toward H2 combustion in air was found with t10 = 275 °C, t50 = 345 °C, and Ea = 76.9 kJ/mol for sample G/N = 1.2. The higher activity of sample G/N = 1.2 in catalysis was attributed to different properties of the composite, including an appropriate component phase ratio, the smaller size of crystallites, higher specific surface area, higher reducibility,oxygen capacity, etc. The findings make it possible to carry out the directed synthesis of catalysts based on the Ce–Fe–O system with specific phases, dispersion, and morphological composition for efficient hydrogen oxidation at moderate temperatures. © 2023 Vietnam National University, Hanoi