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Quantitative Analysis of Nitrogen by Atom Probe Tomography Using Stoichiometric γ′-Fe4N Consisting of 15N Isotope

Published online by Cambridge University Press:  26 November 2021

Jun Takahashi Open the ORCID record for Jun Takahashi [Opens in a new window] ,
Kazuto Kawakami ,
Koyo Miura ,
Mitsuhiro Hirano  and
Naofumi Ohtsu
Jun Takahashi*
Affiliation:
Advanced Technology Research Laboratories, Nippon Steel Corporation, 20-1 Shintomi, Futtsu, Chiba293-8511, Japan
Kazuto Kawakami
Affiliation:
Resource and Process Solution Dev., Nippon Steel Technology Co. Ltd., 20-1 Shintomi, Futtsu, Chiba293-0011, Japan
Koyo Miura
Affiliation:
School of Earth, Energy and Environmental Engineering, Kitami Institute of Technology, 165 Koen-cho, Kitami, Hokkaido090-8507, Japan
Mitsuhiro Hirano
Affiliation:
School of Earth, Energy and Environmental Engineering, Kitami Institute of Technology, 165 Koen-cho, Kitami, Hokkaido090-8507, Japan
Naofumi Ohtsu
Affiliation:
School of Earth, Energy and Environmental Engineering, Kitami Institute of Technology, 165 Koen-cho, Kitami, Hokkaido090-8507, Japan
*
*Corresponding author: Jun Takahashi, E-mail: [email protected]
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Abstract

The nitrogen deficiency in steels measured by atom probe tomography (APT) is considered to arise from the obscurement of singly charged dimer nitrogen ions (N2+) by the iron-dominant peak (56Fe2+) at 28 Da. To verify this by quantifying the amount of N2+ ions, γ′-Fe4N consisting of the 15N isotope was prepared on iron substrates by plasma nitriding using a nitrogen isotopic gas (15N2). Although considerable amounts of 15N2+ were observed at 30 Da without overlap with any iron peak, the observed nitrogen concentrations of γ′-Fe4N were clearly lower than the stoichiometric composition (19–20 at%), using both pulsed voltage and pulsed laser atom probes. The origin of the missing nitrogen, excluding nitrogen obscured by other ion species, was predicted to be the occurrence of neutral nitrogen or nitrogen gas molecules in field evaporation. The generation rate of iron nitride ions (FeN2+) for 15N was significantly lower than that for 14N in γ′-Fe4N, which affected the amount of the missing nitrogen. The isotope effect suggests that the isotopic ratio cannot always be determined from only one ion species among the multiple species observed in the APT analysis. We discuss the mechanism of the isotope effect in FeN2+ formation by field evaporation.

Keywords

atom probeγ′-Fe4Nisotope effectnitrogen deficiencynitrogen isotope
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 28 , Issue 1 , February 2022 , pp. 42 - 52
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Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

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