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This work demonstrated the development of nanofiber templated metal oxide nanocomposites by hydrothermal and calcination methods for photocatalytic degradation using Congo red (CR) as model pollutant. Herein, we developed PAN/CuO-ZnO nanocomposites by the electrospinning technique followed by heat treatment process i.e hydrothermal and calcination. The obtained nanofibrous composites were characterized by various analytical techniques such as X-Ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Thermogravimetric analys