Isoconcentration surfaces are commonly used to delineate phases in atom probe datasets. These surfaces then provide the spatial and compositional reference for proximity histograms, the number density of particles, and the volume fraction of particles within a multiphase system. This paper discusses the influence of the isoconcentration surface selection value on these quantitative outputs, using a simple oxide dispersive strengthened alloy, Fe91Ni8Zr1, as the case system. Zirconium reacted with intrinsic oxygen impurities in a consolidated ball-milled powder to precipitate nanoscale zirconia particles. The zirconia particles were identified by varying the Zr-isoconcentration values as well as by the maximum separation data mining method. The associated outputs mentioned above are elaborated upon in reference to the variation in this Zr isosurface value. Considering the dataset as a whole, a 10.5 at.% Zr isosurface provided a compositional inflection point for Zr between the particles and matrix on the proximity histogram; however, this value was unable to delineate all of the secondary oxide particles identified using the maximum separation method. Consequently, variations in the number density and volume fraction were observed as the Zr isovalue was changed to capture these particles resulting in a loss of the compositional accuracy. This highlighted the need for particle-by-particle analysis.

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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.