In this work, an improved methodology of cross-sectional scanning electron microscopy (SEM) analysis of thin-film Ti/V/Ti multilayers was described. Multilayers with various thicknesses of the vanadium middle layer were prepared by magnetron sputtering. The differences in cross sections made by standard fracture, focused ion beam (FIB)/Ga, and plasma focused ion beam (PFIB)/Xe have been compared. For microscopic characterization, the Helios NanoLab 600i microscope and the Helios G4 CXe with the Quanta XFlash 630 energy dispersive spectroscopy detector from Bruker were used. The innovative multi-threaded approach to the SEM preparation itself, which allows us to retain information about the actual microstructure and ensure high material contrast even for elements with similar atomic numbers was proposed. The fracture technique was the most noninvasive for microstructure, whereas FIB/PFIB results in better material contrast (even than EDS). There were only subtle differences in cross sections made by FIB-Ga and PFIB-Xe, but the decrease in local amorphization or slightly better contrast was in favor of Xe plasma. It was found that reliable information about the properties of modern nanomaterials, especially multilayers, can be obtained by analyzing a two-part SEM image, where the first one is a fracture, while the second is a PFIB cross section.

Nonstoichiometric (Ti,Co)Ox coatings were prepared using gas-impulse magnetron sputtering (GIMS). The properties of coatings with 3 at.%, 19 at.%, 44 at.%, and 60 at.% Co content were compared to those of TiO_x and CoO_x films. Structural studies with the aid of GIXRD indicated the amorphous nature of (Ti,Co)Ox. The fine-columnar, homogeneous microstructure was observed on SEM images, where cracks were identified only for films with a high Co content. On the basis of XPS measurements, TiO₂, CoO, and Co₃O₄ forms were found on their surface. Optical studies showed that these films were semi-transparent (T > 46%), and that the amount of cobalt in the film had a significant impact on the decrease in the transparency level. A shift in the absorption edge position (from 337 to 387 nm) and a decrease in their optical bandgap energy (from 3.02 eV to more than 2.60 eV) were observed. The hardness of the prepared films changed slightly (ca. 6.5 GPa), but only the CoO_x film showed a slightly lower hardness value than the rest of the coatings (4.8 GPa). The described studies allowed partial classification of non-stoichiometric (Ti,Co)Ox thin-film materials according to their functionality.