AbstractThe investigation focused on examining the impact of incorporating Fe‐carbon nanotubes (CNTs) on the valence state and oxygen vacancies, and the physicochemical parameters of the catalytic system. For the CeO2/TiO2 catalyst with Fe‐CNTs, no distinct X‐ray diffraction (XRD) peaks corresponding to Fe‐CNTs were observed. This indicated their uniform dispersion, supported by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) imaging. X‐ray photoelectron spectroscopy (XPS) analysis was conducted to observe the changes in the valence state due to the addition of Fe‐CNTs. The concentration of Ce3+ on catalyst surface increased from 19.90% to 29.48% with an increased concentration of the chemisorbed oxygen species (Oα). This suggests that the addition of Fe‐CNTs into CeO2/TiO2 catalyst reduced Ce4+ on the catalyst surface, resulting in the formation of oxygen vacancies. Oxygen temperature‐programmed desorption (O2‐TPD) and hydrogen temperature‐programmed reduction (H2‐TPR) analyses showed both the adsorbed oxygen species and H2 consumption increased with adding Fe‐CNTs. Furthermore, the onset temperatures for O2 desorption and H2 consumption became lower, confirming the enhancement of catalytic redox properties.