Atom Probe Tomography‐Based Analysis of Residual Trace Elements in Advanced Metallic Materials

ABSTRACT Residual trace elements inherited from raw materials strongly influence the mechanical and environmental performance of advanced metallic alloys and recycling materials due to preferable boundary/interface segregation and resultant embrittlement effects, yet their parts per million level concentrations pose significant challenges to conventional characterization techniques. Although the atom probe tomography (APT) technique, which uniquely combines single‐atom sensitivity with sub‐nanometer spatial resolution, enables discerning the distribution of these trace species, the quantification of the local trace elements is strongly affected by trajectory aberrations resulting from structure/chemistry heterogeneity. In this paper, we present a comprehensive APT‐based workflow covering multiscale characterization and atomic‐scale analysis, and demonstrate its application across representative alloy systems. By integrating electron microscopy for crystallographic guidance and interface‐width calibration, we further solved the localization‐limited and quantification‐inaccuracy in typical alloys and uncovered the atomistic origins of property degradation quantitatively. The combined approach provides a rigorous protocol for characterizing residual trace elements and establishes a benchmark for elucidating structure‐composition‐properties relationships in high‐performance metallic materials.