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A controlled and successful high temperature calcination of PVDF was performed to synthesize high quality CQDs from polymeric membrane via electrospinning to control its shape and size. X-Ray Diffractograms show the formation of CQDs after thermal reduction of polymeric nanofibers with an average crystallite size of ~1.9 nm. Raman spectrum reveals the formation of intense G-band which confirms the presence of carbon nanomaterials in the form of CQDs with ratio of intensities I_G/I_D ~3.7. The variation of FTIR spectrum before and after calcination process supports the speculation of the suppression of oxygen containing functional groups. XPS and UV–Vis absorption spectrum confirms the highly stable and rich carbon content of Cdouble bondC group. FE-SEM and TEM demonstrates the spherical distribution of quantum dots with an average size of ~2.6 nm.