The purpose of the article is to discuss the process of oxidation of carbon nanotubes subsequently subjected to the process of decoration with rhenium nanoparticles. The influence of functionalization in an oxidizing medium is presented and the results of investigations using Raman spectroscopy and infrared spectroscopy are discussed. Multiwalled carbon nanotubes rhenium-type nanocomposites with the weight percentage of 10%, 20% and 30% of rhenium are also presented in the article. The structural components of such nanocomposites are carbon nanotubes decorated with rhenium nanoparticles. Microscopic examinations under transmission electron microscope and scanning transmission electron microscope using the bright and dark field confirm that nanocomposites containing about 20% of rhenium have the most homogenous structure.