The CHP technique is applied for evaluating of hydrogen storage capacity of the Fe 2 O 3 −CeO 2 nanocomposite oxide. The Fe 2 O 3 −CeO 2 nanocomposite oxide has been synthesized via a thermal decomposition route using different solvents. To achieve better morphology, various parameters were studied such as calcination temperature, type of solvent, and the changing molar ratio of Ce:Fe. Then, XRD, EDS, FT-IR, SEM, TEM, and BET have been applied to characterize the prepared nanocomposite oxide. The electrochemical hydrogen storage capacity of the proposed nanocomposite oxide was studied for two samples, 4 and 7. The discharge capacity of samples at the 1st and 20th cycles was observed at 940 mAh/g (≈3.1 wt %) and 6450 mAh/g (≈21.5 wt %) for sample 4 and from 850 mAh/g (≈2.8 wt %) to 5450 mAh/g (≈18.2 wt %) for sample 7. The enhancement of their electrochemical hydrogen storage capacity is owing to the creation of new sites during charge and discharge process in the working electrode (Fe 2 O 3 −CeO 2 nanocomposite oxide).