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Heterostructured SnO2/CuO nanofibers with a hollow morphology were successfully fabricated by a one-step electrospinning method. The electrospun nanofibers were transformed into hollow nanostructures in the presence of camphene after a calcination process, and the obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflection spectroscopy (DRS), photoluminescence spectra (PL), and photodegradation measurements. The scanning electron microscopy (SEM) images displayed a rough and hollow structure for the obtained nanofibers. X-ray photoelectron spectroscopy (XPS) and energy-dispersive X-ray spectroscopy (EDX) identified the molecular composition and chemical interactions of the nanofibers. Photoluminescent (PL) measurements indicated that a recombination of the photoinduced electrons and holes was further inhibited due to the hollow nanostructure. Furthermore, the photodegradation of methylene blue suggested that the heterostructured SnO2/CuO hollow nanofibers possessed higher charge separation and photodegradation abilities than those of the other samples under visible light irradiation. This work can be potentially applied to the fabrication of other inorganic oxide photocatalysts with enhanced photodegradation activity in the field of environmental remediation. [ABSTRACT FROM AUTHOR]