A radically new innovation was established for development of electromagnetic interference shielding. The innovation emphasis synthesis of carboxymethyl cellulose (CMC), carboxymethyl cellulose composite containing different metal nanoparticles (CMC-MNPs), and carboxymethyl cellulose nanofiber mat (CMC-NF) and carboxymethyl cellulose containing metal nanofiber mat (CMC-MNPs nanofiber mat) by electrospinning technique. Metal nanoparticles used include copper nanoparticles, iron nanoparticles, zinc nanoparticles, cadmium nanoparticles, and cobalt nanoparticles. Synthesized CMC-MNPs were characterized by using scanning electron microscopy coupled with high-energy dispersive X-ray and UV-visible spectroscopy that was used for confirmation of nanoparticles formation. The scanning electron microscopy images clearly showed regular flat shape with semiporous surface. All metal nanoparticles were well distributed inside the backbone of the cellulose without aggregation. The average particle diameter was 29-39nm for zinc nanoparticles, 29-33nm for cadmium nanoparticles, 25-33nm for cobalt nanoparticles, 23-27nm for copper nanoparticles, and 22-26nm for iron nanoparticles. Electrospun carboxymethyl cellulose and CMC-MNPs nanofiber mats were synthesized by electrospinning technique and characterized using scanning electron microscopy, energy dispersive X-ray, and transmission electron microscopy. Scanning electron microscopy images of electrospun carboxymethyl cellulose and CMC-MNPs nanofibers reveal smooth and uniformly distributed nanofibers without bead formation with average fiber diameters in the range of 300-450nm. Moreover, the diameters of electrospun carboxymethyl cellulose nanofiber mat were not affected by the presence of metal nanoparticles. Metal nanoparticles' content inside the electrospun CMC-MNPs nanofibers was investigated by using atomic absorption spectroscopy. Electromagnetic interference shielding of electrospun carboxymethyl cellulose and CMC-MNPs nanofiber mats was evaluated. Data showed that the EMI-SE was increased in presence of metal nanoparticles and depending on both the metal nanoparticle contents and the electrical conductivity of metal nanoparticles.