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Hydrogen is the alternative renewable energy source for addressing the energy crisis, global warming, and climate change. Hydrogen is mostly obtained in the industrial process by steam reforming of natural gas. In the present work, CuCrO2 particles were attached to the surfaces of electrospun CeO2 nanofibers to form CeO2-CuCrO2 nanofibers. However, the CuCrO2 particles did not readily adhere to the surfaces of the CeO2 nanofibers, so a trace amount of SiO2 was added to the surfaces to make them hydrophilic. After the SiO2 modification, the CeO2 nanofibers were immersed in Cu-Cr-O precursor and annealed in a vacuum atmosphere to form CeO2-CuCrO2 nanofibers. The CuCrO2, CeO2, and CeO2-CuCrO2 nanofibers were examined by X-ray diffraction analysis, transmission electron microscopy, field emission scanning electron microscopy, scanning transmission electron microscope, thermogravimetric analysis, and Brunauer–Emmett–Teller studies (BET). The BET surface area of the CeO2-CuCrO2 nanofibers was 15.06 m2/g. The CeO2-CuCrO2 nanofibers exhibited hydrogen generation rates of up to 1335.16 mL min−1 g-cat−1 at 773 K. Furthermore, the CeO2-CuCrO2 nanofibers produced more hydrogen at lower temperatures. The hydrogen generation performance of these CeO2-CuCrO2 nanofibers could be of great importance in industry and have an economic impact.

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