This research aims toward an antibacterial and osteoconductive Ti₆Al₄V surface by chemical etching–oxidation treatment and in situ reduction of silver nanoparticles. Starting from a previously developed process, already proved to enhance the osteoinductive ability of titanium, different parameters are changed to tailor the amount of silver and its distribution across the surface oxide layer thickness. The samples are characterized by scanning and transmission electron microscopy, energy‐dispersive X‐ray spectroscopy, release of silver, biofilm formation (Staphylococcus aureus), and cytocompatibility toward human osteoblasts progenitor cells. The total amount of silver in the surface oxide layer depends only on the concentration of the silver precursor. The time of the addition of the silver precursor, during the oxidation treatment, affects the oxide layer thickness, dimension, and distribution of the nanoparticles across the surface oxide: they are larger and accumulate on the outermost layer, if the addition occurs early. The maximum ion release occurs after 24 h and lasts up to 14 days; the later addition of silver precursors leads to sustaining the silver release for a longer time. The samples prepared with the higher concentration of the silver precursor are bactericide, but highly cytotoxic, whereas the other ones are bacteriostatic and moderately cytotoxic.

The main strengthening mechanism for Inconel 718 (IN718), a Ni-based superalloy, is precipitation hardening by γ′ and γ″ particles. It is thus essential, for good alloy performance, that precipitates with the desired chemical composition have adequate size and dispersion. The distribution of the γ′ and γ″ phases and their chemical composition were investigated in the nickel-based Inconel 718 superalloy by taking advantage of the new capabilities of scanning transmission electron microscopy and energy-dispersive X-ray spectrometry using a windowless multiple detector, a high-brightness Schottky electron gun, and a spherical aberration corrector in the illumination probe optics. A small routine was developed to deconvolute the respective compositions of γ′ and γ″ nanoprecipitates embedded in the γ matrix. Keeping the electron probe current low enough—a few hundred pA—prevented excessive irradiation damage during the acquisition of element maps and brought their spatial resolution down to the atomic column level to track their element compositions. The present results agree with and complement atomic probe tomography observations and Thermo-Calc predictions from the literature. The presence of an Al enrichment at the γ′/γ″ interface—which may control the γ″ phase coarsening—is observed in the last row of Al-Nb-Ti columns along this interface. In addition, a few columns with similar composition changes are found randomly distributed in the γ′ phase.

The ATI 718Plus^® is a creep-resistant nickel-based superalloy exhibiting high strength and excellent oxidation resistance in high temperatures. The present study is focused on multiscale 2D and 3D characterization (morphological and chemical) of the scale and the layer beneath formed on the ATI 718Plus superalloy during oxidation at 850 °C up to 4000 h in dry and wet air. The oxidized samples were characterized using various microscopic methods (SEM, TEM and STEM), energy-dispersive X-ray spectroscopy and electron diffraction. The 3D visualization of the microstructural features was achieved by means of FIB-SEM tomography. When oxidized in dry air, the ATI 718Plus develops a protective, dense Cr₂O₃ scale with a dual-layered structure. The outer Cr₂O₃ layer is composed of coarser grains with a columnar shape, while the inner one features fine, equiaxed grains. The Cr₂O₃ scale formed in wet air is single-layered and features very fine grains. The article discusses the difference between the structure, chemistry and three-dimensional phase distribution of the oxide scales and near-surface areas developed in the two environments. Electron microscopy/spectroscopy findings combined with the three-dimensional reconstruction of the microstructure provide original insight into the role of the oxidation environment on the structure of the ATI 718Plus at the nanoscale.