Highly porous nitrogen-doped carbon nanomaterials have distinct advantages in energy storage and conversion technologies. In the present work, hydrothermal treatments in water or ammonia solution were used for modification of mesoporous nitrogen-doped graphitic carbon, synthesized by deposition of acetonitrile vapors on the pyrolysis products of calcium tartrate. Morphology, composition, and textural characteristics of the original and activated materials were studied by transmission electron microscopy, X-ray photoelectron spectroscopy, near-edge X-ray absorption fine structure spectroscopy, infrared spectroscopy, and nitrogen gas adsorption method. Both treatments resulted in a slight increase in specific surface area and volume of micropores and small mesopores due to the etching of carbon surface. Compared to the solely aqueous medium, activation with ammonia led to stronger destruction of the graphitic shells, the formation of larger micropores (1.4 nm vs. 0.6 nm), a higher concentration of carbonyl groups, and the addition of nitrogen-containing groups. The tests of nitrogen-doped carbon materials as electrodes in 1M H₂SO₄ electrolyte and sodium-ion batteries showed improvement of electrochemical performance after hydrothermal treatments especially when ammonia was used. The activation method developed in this work is hopeful to open up a new route of designing porous nitrogen-doped carbon materials for electrochemical applications.

The structural and chemical composition of the surface layer (100–140 nm) of niobium radiofrequency cavities operating at cryogenic temperature has enormous impact on their superconducting characteristics. During the last years, cavities treated with a new thermal processing recipe, so-called nitrogen infusion, have demonstrated an increased efficiency and high accelerating gradients. The role and importance of nitrogen gas has been a topic of many debates. In the present work we employ variable-energy synchrotron x-ray photoelectron spectroscopy (XPS), to study the niobium surface subjected to the following treatments: vacuum annealing at 800 °C, nitrogen infusion, and vacuum heat treatment as for the infusion process but without nitrogen supply. Careful analysis of XPS energy-distribution curves revealed a slightly increased thickness of the native oxide Nb₂O₅ for the infused samples (∼3.8 nm) as compared to the annealed one (∼3.5 nm) which indicates insignificant oxygen incorporation into niobium during 120 °C baking and no effect of nitrogen on the formation of oxides or other niobium phases. By conducting an additional in-situ annealing experiment and analyzing the niobium after the failed infusion process, we conclude that the vacuum furnace hygiene particularly during the high-temperature stage is the prerequisite for success of any treatment recipe.

Filling of single-walled carbon nanotubes (SWCNTs) and extraction of the encapsulated species from their cavities are perspective treatments for tuning the functional properties of SWCNT-based materials. Here, we have investigated sulfur-modified SWCNTs synthesized by the ampoule method. The morphology and chemical states of carbon and sulfur were analyzed by transmission electron microscopy, Raman scattering, thermogravimetric analysis, X-ray photoelectron and near-edge X-ray absorption fine structure spectroscopies. Successful encapsulation of sulfur inside SWCNTs cavities was demonstrated. The peculiarities of interactions of SWCNTs with encapsulated and external sulfur species were analyzed in details. In particular, the donor–acceptor interaction between encapsulated sulfur and host SWCNT is experimentally demonstrated. The sulfur-filled SWCNTs were continuously irradiated in situ with polychromatic photon beam of high intensity. Comparison of X-ray spectra of the samples before and after the treatment revealed sulfur transport from the interior to the surface of SWCNTs bundles, in particular extraction of sulfur from the SWCNT cavity. These results show that the moderate heating of filled nanotubes could be used to de-encapsulate the guest species tuning the local composition, and hence, the functional properties of SWCNT-based materials.