Hostname: page-component-cd9895bd7-q99xh Total loading time: 0 Render date: 2024-12-27T22:55:05.735Z Has data issue: false hasContentIssue false
  • English
  • Français

Study on Quantitative Analysis of Carbon and Nitrogen in Stoichiometric θ-Fe3C and γ′-Fe4N by Atom Probe Tomography

Published online by Cambridge University Press:  05 March 2020

Jun Takahashi Open the ORCID record for Jun Takahashi [Opens in a new window] ,
Kazuto Kawakami  and
Yukiko Kobayashi
Jun Takahashi*
Affiliation:
Advanced Technology Research Laboratories, Nippon Steel Corporation, 20-1 Shintomi, Futtsu, Chiba293-8511, Japan
Kazuto Kawakami
Affiliation:
Nippon Steel Technology Co. Ltd., 20-1 Shintomi, Futtsu, Chiba293-0011, Japan
Yukiko Kobayashi
Affiliation:
Advanced Technology Research Laboratories, Nippon Steel Corporation, 20-1 Shintomi, Futtsu, Chiba293-8511, Japan
*
*Author for correspondence: Jun Takahashi, E-mail: takahashi.3ct.jun@jp.nipponsteel.com
Get access

Abstract

The quantitative analysis performance of carbon and nitrogen was investigated using stoichiometric θ-Fe3C (25 at% C) and γ′-Fe4N (~20 at% N) precipitates in pulsed voltage and pulsed laser atom probes. The dependencies of specimen temperature, pulse fraction, and laser pulse energy on the apparent concentrations of carbon and nitrogen were measured. Good coincidence with 25 at% carbon concentration in θ-Fe3C was obtained for the pulsed voltage atom probe by considering the mean number of carbon atoms per ion at 24 Da and the detection loss of iron, while better coincidence was obtained for the pulsed laser atom probe by considering only the mean number of carbon at 24 Da. On the other hand, a lack of nitrogen concentration in γ′-Fe4N was observed for the two atom probes. In particular, the pulsed laser atom probe showed a significant lack of nitrogen concentration. This implies that a large amount of 14N2+ was obscured by the main iron peak of 56Fe2+ at 28 Da in the mass-to-charge spectrum. Regarding preferential evaporation or retention, carbon in θ-Fe3C exhibited little of either, but nitrogen in γ′-Fe4N exhibited definite preferential retention. This result can be explained by the large difference in ionization energy between carbon and nitrogen.

Keywords

γ′-Fe4Nθ-Fe3Catom probecarbonnitrogen
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 26 , Issue 2 , April 2020 , pp. 185 - 193
Copyright
Copyright © Microscopy Society of America 2020

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Angseryd, J, Liu, F, Andrén, H-O, Gerstl, SSA & Thuvender, M (2011). Quantitative APT analysis of Ti(C,N). Ultramicroscopy 111, 609–614.CrossRefGoogle Scholar
Cheng, L, Stark, I, Korevaar, BM, Mittemeijer, EJ & Smith, GDM (1988). The initial stage of aging iron-nitrogen martensite. In Proceedings of the International Conference on High Nitrogen Steels, pp. 97–101. London: The Institute of Metals.Google Scholar
Cottrell, AH (1993). A theory of cementite. Mater Sci Technol 9, 277–280.CrossRefGoogle Scholar
Forbes, G (1995). Field evaporation theory: A review of basic idea. Appl Surf Sci 87/88, 1–11.CrossRefGoogle Scholar
Geuser, FD, Gault, B, Bostel, A & Vurpillot, F (2007). Correlated field evaporation as seen by atom probe tomography. Surf Sci 601, 536–543.CrossRefGoogle Scholar
Göhring, H, Fabrichnaya, O, Leineweber, A & Mittemeijer, EJ (2016). Thermodynamics of the Fe-N and Fe-N-C systems: The Fe-N and Fe-N-C phase diagrams revisited. Metall Mater Trans A 47, 6173–6186.CrossRefGoogle Scholar
Gruber, M, Vurpillot, F, Bostel, A & Deconihout, B (2011). Field evaporation: A kinetic Monte Carlo approach on the influence of temperature. Surf Sci 605, 2025–2031.CrossRefGoogle Scholar
Haydock, R & Kingham, DR (1980). Post-ionization of field-evaporation ions. Phys Rev Lett 44, 1520–1523.CrossRefGoogle Scholar
Huheey, JE, Keiter, EA & Keiter, RL (1993). Inorganic Chemistry: Principles of Structure and Reactivity, 4th ed. New York, NY: Harper Collins.Google Scholar
Jessner, P, Danoix, R, Hannoyer, B & Danoix, F (2009). Investigations of the nitride subsurface layers of and Fe-Cr-model alloy. Ultramicroscopy 109, 530–534.CrossRefGoogle ScholarPubMed
Jiang, S, Xu, H, Sun, Y & Song, T (2019). Performance analysis of Fe-N compounds based on valence electron structure. J Alloy Compounds 779, 427–432.CrossRefGoogle Scholar
Kayser, FX & Sumitomo, Y (1997). On the composition of cementite in equilibrium with ferrite at room temperature. J Phase Equilibria 18, 458–464.CrossRefGoogle Scholar
Kinno, T, Kitamoto, K, Takeno, S & Tomita, M (2015). Laser-assisted atom probe tomography of 15N-enriched nitride thin films for analysis of nitrogen distribution in silicon-based structure. Appl Surf Sci 34, 89–92.CrossRefGoogle Scholar
Kitaguchi, HS, Lozano-Peres, S & Moody, MP (2014). Quantitative analysis of carbon in cementite using pulsed laser atom probe. Ultramicroscopy 147, 51–60.CrossRefGoogle ScholarPubMed
Kobayashi, Y, Takahashi, J & Kawakami, K (2011). Anomalous distribution in atom map of solute carbon in steel. Ultramicroscopy 111, 600–603.CrossRefGoogle ScholarPubMed
Langelier, B, Van Landeghem, HP, Botton, GA & Zurob, HS (2017). Interface segregation and nitrogen measurement in Fe-Mn-N steel by atom probe tomography. Microsc Microanal 23, 385–395.CrossRefGoogle ScholarPubMed
Leslie, WC (1981). The Physical Metallurgy of Steels. New York, NY: MacGrill-Hill.Google Scholar
Liu, F & Andrén, H-O (2011). Effect of laser pulsing on analysis of steels by atom probe tomography. Ultramicroscopy 111, 633–641.CrossRefGoogle Scholar
Liu, HF, Liu, HM & Tsong, TT (1986). Numerical calculation of the temperature distribution and evolution of the field-ion emitter under pulsed and continuous-wave laser irradiation. J Appl Phys 59, 1334–1340.CrossRefGoogle Scholar
Lundin, L & Andrén, H-O (1996). Observation of molybdenum-nitrogen clustering in highly alloyed martensite. Appl Surf Sci 94/95, 320–325.CrossRefGoogle Scholar
Marceau, RKW, Choi, P & Raabe, D (2013). Understanding the detection of carbon in austenitic high-Mn steel using atom probe tomography. Ultramicroscopy 132, 239–247.CrossRefGoogle ScholarPubMed
Marquis, EA & Gault, B (2008). Determination of the tip temperature in laser assisted atom-probe tomography using charge state distributions. J Appl Phys 104, 084914.CrossRefGoogle Scholar
Meisenkothen, F, Steel, EB, Prosa, TJ, Henry, KT & Kolli, RP (2015). Effects of detector dead-time on quantitative analyses involving boron and multi-hit detection events in atom probe tomography. Ultramicroscopy 159, 101–111.CrossRefGoogle ScholarPubMed
Miller, MK (2000). Atom Probe Tomography: Analysis at the Atomic Level. New York, NY: Kluwer Academic/Plenum Publishers.CrossRefGoogle Scholar
Miller, MK, Russel, KF & Thompson, GB (2005). Strategies for fabrication atom probe specimens with a dual beam FIB. Ultramicroscopy 102, 287–298.CrossRefGoogle ScholarPubMed
Miyamoto, G, Shinbo, K & Furuhara, T (2012). Quantitative measurement of carbon content in Fe-C binary alloys by atom probe tomography. Scripta Mater 67, 999–1002.CrossRefGoogle Scholar
Müller, EW & Tsong, TT (1969). Field ion Microscopy: Principles and Applications. New York, NY: Elsevier.CrossRefGoogle Scholar
Ohtani, H, Hasebe, M & Nishizawa, T (1984). Calculation of Fe-C, Co-C and Ni-C phase diagrams. Transactions ISIJ 24, 857–864.CrossRefGoogle Scholar
Sha, W, Chang, L, Smith, GDW, Cheng, L & Mittemeijer, EJ (1992). Some aspects of atom-probe analysis of F-C and F-N systems. Surf Sci 266, 416–423.CrossRefGoogle Scholar
Takahashi, J & Kawakami, K (2014). A quantitative model of preferential evaporation and retention for atom probe tomography. Surf Interface Anal 46, 535–543.CrossRefGoogle Scholar
Takahashi, J, Kawakami, K & Kobayashi, Y (2011). Quantitative analysis of carbon content in cementite in steel by atom probe tomography. Ultramicroscopy 111, 1233–1283.CrossRefGoogle ScholarPubMed
Takahashi, J, Kawakami, K & Raabe, D (2017). Comparison of the quantitative analysis performance between pulsed voltage atom probe and pulsed laser atom probe. Ultramicroscopy 175, 105–110.CrossRefGoogle ScholarPubMed
Takahashi, J, Kawakami, K, Yamaguchi, Y & Sugiyama, M (2007). Development of atom probe specimen preparation techniques for specific regions in steel materials. Ultramicroscopy 107, 744–749.CrossRefGoogle ScholarPubMed
Takahashi, J, Tarui, T & Kawakami, K (2009). Three-dimensional atom probe analysis of heavily drawn steel wires by probing perpendicular to the pearlitic lamellae. Ultramicroscopy 109, 193–199.CrossRefGoogle ScholarPubMed
Thuvander, M, Kvist, A, Johnson, LJS, Weidow, J & Andrén, H-O (2013). Reduction of multiple hits in atom probe tomography. Ultramicroscopy 132, 81–85.CrossRefGoogle ScholarPubMed
Thuvander, M, Weidow, J, Angseryd, J, Falk, LKL, Liu, F, Sonestedt, M, Stiller, K & Andrén, H-O (2011). Quantitative atom probe analysis of carbides. Ultramicroscopy 111, 604–608.CrossRefGoogle ScholarPubMed
Umemoto, M & Tsuchiya, K (2002). Fundamental properties of cementite and their present understanding. Tetsu-to-Hagané 88, 117–128.CrossRefGoogle Scholar
Wang, J, Toloczko, MB, Kruska, K, Schreiber, DK, Edwards, DJ, Zhu, Z & Zhang, J (2017). Carbon contamination during ion irradiation-accurate detection and characterization of its effect on microstructure of ferritic/martensitic steels. Sci Rep 7, 15813.CrossRefGoogle ScholarPubMed
Yamaguchi, Y, Takahashi, J & Kawakami, K (2009). The study of quantitativeness in atom probe analysis of alloying elements in steel. Ultramicroscopy 109, 541–544.CrossRefGoogle Scholar
Yao, L, Gault, B, Cairny, JM & Ringer, SP (2010). On the multiplicity of field evaporation events in atom probe: A new dimension to the analysis of mass spectra. Philos Mag Lett 90, 121–129.CrossRefGoogle Scholar