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The excellent properties of single-walled carbon nanotubes (SWNTs), mechanical, electrical, thermal, optical, have been studied, both experimentally and theoretically, in a much more details, compared with multiwalled carbon nanotubes (MWNTs). However, in development of new functional materials, MWNTs are used, as a filler, more often than the SWNTs, although the MWNTs parameters are normally weaker than those of SWNTs. To what extent these parameters are weaker depends on the type of MWNTs which determined by the method and regimes of CNTs synthesis. Here the Raman spectrometry is used to determine the relative concentration of defects in CNTs, produced by different methods and having different size and shapes, including vertically aligned (VA) CNTs. Further on, the methods of preparation of nanocomposites (PNC) with different polymers and different CNTs are described, including the polymer impregnation of a dense array of VACNTs and PNC with horizontally aligned (HA) CNTs. Raman spectra of CNTs in a polymer matrix are compared with those in a “ready-to-fill” form and a difference in D- and G-lines are discussed. The mechanical, electrical, thermal properties of PNCs are characterised by a number of tests. The most prominent change in the polymer properties are in the PNCs with VA and HA CNTs. As examples, the thermal conductivity is enhanced by a factor of more than 3 and electrical conductivity increased by a factor 109.