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Nanocomposites of multiwalled carbon nanotubes (MWCNTs) in epoxy resin and polypropylene (PP) are studied. The effect of matrix viscosity on the degree of dispersion of nanotubes is determined by rheological methods. Rheology and microwave properties are correlated to estimate the optimal limits of nanofiller content required for improving the performance of nanocomposites. Rheological percolation threshold is determined for both types nanocomposites, ϕp=0.27% for the epoxy/MWCNT and; ϕp=1.5% for the PP/MWCNT, as found critical for achieving a network structure of interacting nanotubes in the matrix polymer. Good electromagnetic shielding efficiency was obtained for nanocomposites at nanotube contents above the rheological percolation. Low viscosity matrix facilitates contacts between MWCNTs, resulting in appearance of electromagnetic shielding at very low percolation threshold.