Solute Distributions in Tantalum-Containing Zirconium Diboride Ceramics

Solute segregation was examined in zirconium diboride and zirconium-tantalum diboride solid solution ceramics that were produced by reactive hot pressing. Microstructural analysis demonstrated that the ZrB2 and (Zr,Ta)B2 ceramics reached nearly full relative density and were nominally phase-pure. X-ray diffraction was consistent with full incorporation of Ta into solid solution within the ZrB2 structure, and energy-dispersive spectroscopy demonstrated that tantalum was well distributed throughout the bulk of the Ta-doped specimens. The weak characteristic X-rays for B led to inaccurate results for total atom concentrations in boride ceramics by energy-dispersive spectroscopy. Atom probe tomography was used to analyze the amount and spatial distribution of Ta species. No obvious Ta segregation was observed in grains or grain boundaries. However, nitrogen strongly segregated to a grain boundary. This study demonstrated that atom probe tomography is an accurate method for characterizing the amount and spatial distribution of metallic and nonmetallic species in ZrB2 ceramics

Visualizing the Nanoscale Oxygen and Cation Transport Mechanisms during the Early Stages of Oxidation of Fe–Cr–Ni Alloy Using In Situ Atom Probe Tomography

Understanding the early stages of interactions between oxygen and material surfaces—especially at very high spatial resolutions—is highly beneficial for fields ranging from materials degradation, corrosion, geological sciences, forensics, and catalysis. The ability of in situ atom probe tomography (APT) is demonstrated to track the diffusion of oxygen and metal ions at nanoscale spatial resolution during the early stages of oxidation of a model Fe–Cr–Ni alloy. Using 18O isotope tracers in these in situ APT experiments and complementary ex situ multimodal microscopy, spectroscopy, and computational simulations allows to precisely analyze the kinetics of oxidation and determine that outward cation diffusion to oxide/air interface is the primary mechanism for intragranular oxide growth in this alloy at 300 °C. This unique in situ isotopic tracer APT approach and the insights gained can be highly beneficial for studying early stages of gas–surface reactions in a broad array of materials