用能量色散x射线能谱扫描透射电子显微镜精确测量钢晶界偏析的溶质剖面

IF 2.2 3区工程技术 Q1 MICROSCOPY

Micron Pub Date : 2025-07-17 DOI:10.1016/j.micron.2025.103887

Yuya Murata , Taku Moronaga , Mariko Egami , Kazushi Hayashi , Shigenobu Nanba , Toru Hara , Ikuo Ohnuma , Takahito Ohmura

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引用次数: 0

摘要

本文介绍了一种利用扫描透射电子显微镜结合能量色散x射线能谱（STEM-EDS）精确测量晶界偏析溶质剖面的方法。STEM中溶质剖面的测量存在信号强度的计数误差和样品中电子束展宽引起的系统误差。在我们的测量方法中，采用大立体角EDS系统抑制了EDS信号强度的计数误差，并通过ζ-因子法估计样品厚度来修正样品中电子束展宽引起的系统误差。我们验证了电子束展宽误差修正的有效性，并证实了该方法可以测量在GB分离的溶质剖面的半最大值全宽度，误差为0.1 nm。测量方法应用于添加p的间隙型游离钢。P谱线与GB平面的距离呈衰减分布，而不是恒定分布。此外，发现晶内偏析宽度随晶内偏析取向的增加而增大。对GB偏析的溶质剖面的精确测量，将为研究GB偏析对材料性能的影响提供新的思路，有助于更好地理解和控制GB偏析对材料性能的影响。

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Accurate measurement of solute profile segregated at steel grain boundary by scanning transmission electron microscope with energy dispersive X-ray spectroscopy

This report describes a method for accurate measurement of solute profile segregated at grain boundary(GB) by scanning transmission electron microscope with energy dispersive X-ray spectroscopy (STEM-EDS). Measurement of solute profile in STEM has issues of a counting error of the signal intensity and a systematic error due to electron beam broadening in the sample. In our measurement method, the counting error of the EDS signal intensity was suppressed by using a large solid-angle EDS system, and the systematic error due to electron beam broadening in the sample was corrected with estimating the sample thickness by ζ-factor method. We verified the effectiveness of the error correction for electron beam broadening, and confirmed that the method can measure full width at half maximum of solute profile segregated at GB with an error of 0.1 nm. The measurement method was applied to P-added interstitial free steels. The P profile showed a decaying distribution rather than constant with respect to the distance from GB plane. In addition, it was found that the GB segregation width increases with the GB misorientation. The accurate measurement of solute profile segregated at GB will provide new insight into the structure of GBs, and lead to better understanding and controlling of the influence of GB segregation on material property.

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来源期刊

Micron 工程技术-显微镜技术

CiteScore

4.30

自引率

4.20%

发文量

100

审稿时长

31 days

期刊介绍： Micron is an interdisciplinary forum for all work that involves new applications of microscopy or where advanced microscopy plays a central role. The journal will publish on the design, methods, application, practice or theory of microscopy and microanalysis, including reports on optical, electron-beam, X-ray microtomography, and scanning-probe systems. It also aims at the regular publication of review papers, short communications, as well as thematic issues on contemporary developments in microscopy and microanalysis. The journal embraces original research in which microscopy has contributed significantly to knowledge in biology, life science, nanoscience and nanotechnology, materials science and engineering.