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Graphene oxide (GO)/polyvinyl butyral (PVB) nanofibers were prepared by a simple electrospinning technique with PVB as matrix and GO as a functional nanomaterial. GO/PVB nanofibers on glassy carbon electrode (GCE) were reduced through electrochemical method to form reduced graphene oxide (RGO)/PVB nanofibers. The morphology and structure of GO/PVB nanofiber were studied by scanning election microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR). RGO/PVB modified GCE was used for fabricating an electrochemical sensor for detecting Cu (II) in water. The analysis results showed that RGO/PVB modified GCE had good analytical results with the linear range of 0.06–2.2 μM, detection limit of 4.10 nM (S/N=3), and the sensitivity of 103.51 μA·μM−1·cm−2.