Abstract

Light element identification is necessary in materials research to obtain detailed insight into various material properties. However, reported techniques, such as scanning transmission electron microscopy (STEM)-energy dispersive X-ray spectroscopy (EDS) have inadequate detection limits, which impairs identification. In this study, we achieved light element identification with nanoscale spatial resolution in a multi-component metal alloy through unsupervised machine learning algorithms of singular value decomposition (SVD) and independent component analysis (ICA). Improvement of the signal-to-noise ratio (SNR) in the STEM-EDS spectrum images was achieved by combining SVD and ICA, leading to the identification of a nanoscale N-depleted region that was not observed in as-measured STEM-EDS. Additionally, the formation of the nanoscale N-depleted region was validated using STEM–electron energy loss spectroscopy and multicomponent diffusional transformation simulation. The enhancement of SNR in STEM-EDS spectrum images by machine learning algorithms can provide an efficient, economical chemical analysis method to identify light elements at the nanoscale.

Highlights

  • Light element identification is necessary in materials research to obtain detailed insight into various material properties

  • We investigated the correlation between the element distribution around the C­ r2N precipitate and the aging time of High-nitrogen stainless steel (HNS) using scanning transmission electron microscopy (STEM)-energy dispersive X-ray spectroscopy (EDS) spectrum images (SIs) with improved signal-to-noise ratio (SNR) via machine learning (ML) algorithms

  • In the specimen aged for 1­ 03 s (Fig. 1a), a cellular type of C­ r2N began to form within the grains, and the volume fraction of cellular C­ r2N increased with the aging time (Fig. 1b,c)

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Summary

Introduction

Light element identification is necessary in materials research to obtain detailed insight into various material properties. Analytical characterization techniques, strengthened by both a robust detection limit and nanometer spatial resolution, are required for researching and manufacturing materials with enhanced properties Analytical techniques such as scanning transmission electron microscopy (STEM)-electron energy loss spectroscopy (EELS) and 3D atom-probe tomography (3D-APT) have been widely used to characterize the chemical composition or a phase structure of materials due to their excellent detection limits (0.005–0.1 at%8–10 and 0.001 at%11,12, respectively) and spatial resolutions (0.1 ­nm[13,14] and 0.2–0.4 ­nm[15,16,17,18], respectively). It is difficult to detect a light element when alloyed with heavy element(s), because its characteristic X-ray energies are likely to be overlapped by the low-energy L and M peaks of the heavy e­ lement[26]

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