Novel conductive PVA/CQDs nanocomposite films were synthesized through the casting technique for the electromagnetic (EM) wave protection at microwave band. The surface morphology, thermal and mechanical properties were briefly studied. The SEM micrograph showed an excellent distribution, dispersion and a high adhesion property of the CQDs in the PVA chains. Also, DSC analysis showed an increase in theglasstemperature(Tglass) from 83.2 °C for fresh PVA to 95.4 °C for 8 wt% of CQD and the increase in melting temperature from 215 °C for fresh PVA to 227.7 °C for the same CQDs concentration. It was found that Young's modulus is directly proportional to CQD nano-particles concentration in the nano-composites from 0.14 GPa for fresh PVA to 4.48 GPa for 8 wt% of CQDs. It was found that the strength at break increases, but the elongation declines with the increase of CQDs nano-particles. The EM shielding effectiveness (SE) of (PVA/CQDs) nanocomposite is measured in the microwave frequency range, and it is found around 36.8 dB with the CQDs concentration (8 wt%). Finally, the PVA/CQDs nano-composite is of promising potential applications in electronics and microwave devices at an affordable cost.