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In this study, we present an innovative ion-beam doping technique for the controlled modification of the near-surface region of multi-walled carbon nanotubes (MWCNTs) aimed at creating pyridinic and pyrrolic nitrogen defects in their walls. This method involves the irradiation of MWCNTs with nitrogen ions using a high-dose ion implanter, resulting in the incorporation of nitrogen atoms into the nanotube structure. The structural and chemical changes induced by the ion-beam treatment were thoroughly characterized. Scanning electron microscopy (SEM) analysis revealed subtle changes in nanotube morphology, while X-ray diffraction (XRD) measurements exhibited altered peak intensities and a shift in the (002) reflection peak, indicating structural modifications, which correlates with transmission electron microscopy (TEM) data. X-ray photoelectron spectroscopy (XPS) analysis confirmed the successful embedding of nitrogen, mainly in pyridinic and pyrrolic configurations, as evidenced by the presence of corresponding lines in the N1s spectrum. Our findings demonstrate the feasibility of precisely engineering nitrogen defects in MWCNTs using the ion-beam doping technique. This approach is expected to be promising for the use of carbon nanotubes surface-functionalized with nitrogen atoms in the development of new devices for electronics, electrochemistry, catalysis, etc. Full article

Using a set of microscopic, spectroscopic, and electrochemical methods, a detailed study of the interrelation between the structural and electrochemical properties of the as-prepared nitrogen-containing multi-walled carbon nanotubes (N-MWCNTs) and their modified derivatives is carried out. It was found that after treatment of nanotubes with hydrochloric acid, their structure is improved by removing amorphous carbon from the outer layers of N-MWCNTs. On the contrary, ion bombardment leads to the formation of vacancy-type structural defects both on the surface and in the bulk of N-MWCNTs. It is shown that the treated nanotubes have an increased specific capacitance (up to 27 F·g⁻¹) compared to the as-prepared nanotubes (13 F·g⁻¹). This is due to an increase in the redox capacitance. It is associated with the reversible Faraday reactions with the participation of electrochemically active pyridinic and pyrrolic nitrogen inclusions and oxygen-containing functional groups (OCFG). Based on the comparison between cyclic voltammograms of N-MWCNTs treated in HCl and with an ion beam, the peaks on these curves were separated and assigned to specific nitrogen inclusions and OCFGs. It is shown that the rate of redox reactions with the participation of OCFGs is significantly higher than that of reactions with nitrogen inclusions in the pyridinic and pyrrolic forms. Moreover, it was established that treatment of N-MWCNTs in HCl is accompanied by a significant increase in the activity of nitrogen centers, which, in turn, leads to an increase in the rate of redox reactions involving OCFGs. Due to the significant contribution of redox capacitance, the obtained results can be used to develop supercapacitors with increased total specific capacitance. Full article