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Transmission Electron Microscopy Investigation on the Electron-stimulated Oxidation of Iron Nitrides by 2-MeV Electron Irradiation

Published online by Cambridge University Press:  01 July 2005

Z.Q. Liu ,
H. Hashimoto ,
T. Sakata ,
H. Mori ,
M. Song ,
K. Mitsuishi  and
K. Furuya
Z.Q. Liu*
Affiliation:
High Voltage Electron Microscopy Station, National Institute for Materials Science, Tsukuba 305-0003, Japan
H. Hashimoto
Affiliation:
Department of Mechanical Engineering, Okayama University of Science, Okayama 700-0005, Japan
T. Sakata
Affiliation:
Research Center for Ultra-High Voltage Electron Microscopy, Osaka University, Osaka 565-0871, Japan
H. Mori
Affiliation:
Research Center for Ultra-High Voltage Electron Microscopy, Osaka University, Osaka 565-0871, Japan
M. Song
Affiliation:
High Voltage Electron Microscopy Station, National Institute for Materials Science, Tsukuba 305-0003, Japan
K. Mitsuishi
Affiliation:
High Voltage Electron Microscopy Station, National Institute for Materials Science, Tsukuba 305-0003, Japan
K. Furuya
Affiliation:
High Voltage Electron Microscopy Station, National Institute for Materials Science, Tsukuba 305-0003, Japan
*
a)Address all correspondence to this author. e-mail: liu.zhiquan@nims.go.jp
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Abstract

An iron nitride sample was irradiated by 2-MeV electrons intermittently for 2100 s with a dose rate of 6.3 × 1024 e.m.−2 s−1 inside a 3-MV high-voltage transmission electron microscope. The electron-stimulated oxidation of Fe4N and Fe2–3N was investigated in situ and ex situ using conventional transmission electron microscopy and high-resolution electron microscopy. It was found that both Fe4N and Fe2–3N nitrides were oxidized by the residual gas in the vacuum chamber to form Fe3O4 oxides. The orientation relationship between Fe4N (γ′) and Fe3O4 (o) was (110)γ′//(220)o, [001]γ′//[001]o, and that between Fe2–3N (ϵ) and Fe3O4 (o) was (110)ϵ//(−220)o, [1–11]ϵ//[001]o. Crystal lattice deformation from iron nitride to iron oxide took place during the dynamic oxidation process. Structural models were proposed to understand the oxide formation, and the models were confirmed by experimental observations. The irradiation effects of Fe4N and Fe2–3N crystals were compared. The results show that Fe4N is more sensitive than Fe2–3N to electron irradiation. These results are important not only for the fabrication of insulating iron oxide film, but also in the field of the surface modification of iron nitride to improve its mechanical properties.

Keywords

Phase transformationRadiation effectsTransmission electron microscopy (TEM)
Type
Articles
Information
Journal of Materials Research , Volume 20 , Issue 7 , July 2005 , pp. 1918 - 1926
Copyright
Copyright © Materials Research Society 2005

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References

REFERENCES

1Margoninski, Y., Segal, D. and Kirby, R.E.: The interference of an electron beam with the surface reaction between oxygen and germanium. Surf. Sci. 53, 488 (1975).CrossRefGoogle Scholar
2Antoniewicz, P.R.: Model for electron- and photo-stimulated desorption. Phys. Rev. B: Condens. Matter 21, 3811 (1980).CrossRefGoogle Scholar
3Park, J.W., Pedraza, A.J. and Allen, W.R.: Irradiation-induced decomposition of Al2O3 during Auger electron spectroscopy analysis. J. Vac. Sci. Technol., A 14, 286 (1996).CrossRefGoogle Scholar
4Xu, B. and Tanaka, S.I.: Formation and bounding of platinum nanoparticles controlled by high energy beam irradiation. Scripta Mater. 44, 2051 (2001).CrossRefGoogle Scholar
5Zhukov, V., Popova, I., Yates, J.T. Jr.: Electron-stimulated oxidation of Al(111) by oxygen at low temperatures: Mechanism of enhanced oxidation kinetics. Phys. Rev. B: Condens. Matter 65, 195409 (2002).CrossRefGoogle Scholar
6Heras, J.M. and Viscido, L.: Oxygen fixing on Cu due to electron-beam damage during Auger spectroscopy. J. Vac. Sci. Technol., A 15, 2051 (1997).CrossRefGoogle Scholar
7Li, W., Stirniman, M.J. and Sibener, S.J.: Inelastic electron scattering study of metallic oxidation: Synergistic effects involving electrons during the low temperature oxidation of Ni(111). J. Vac. Sci. Technol., A 13, 1574 (1995).CrossRefGoogle Scholar
8Xu, J., Choyke, W.J., Yates, J.T. Jr.: Enhanced silicon oxide film growth on Si(100) using electron impact. J. Appl. Phys. 82, 6289 (1997).CrossRefGoogle Scholar
9Olivier, J., Faulconnier, P. and Poirier, R.: Electron-stimulated oxidation of InP(100) surfaces studied by Auger electron spectroscopy and by low-energy-loss spectroscopy. J. Appl. Phys. 51, 4990 (1980).CrossRefGoogle Scholar
10Chen, Y., Luo, Y.S., Seo, J.M. and Weaver, J.H.: Role of O2 negative-ion formation in low-energy electron-induced oxidation of InP(110). Phys. Rev. B: Condens. Matter 43, 4527 (1991).CrossRefGoogle ScholarPubMed
11Jack, D.H. and Jack, K.H.: Invited review: Carbides and nitrides in steel. Mater. Sci. Eng. 11, 1 (1973).CrossRefGoogle Scholar
12Etchells, I.V.: A new approach to salt bath nitrocarburizing. Heat Treat. Met. 8, 85 (1981).Google Scholar
13Dawes, V. and Tranter, D.F.: Nitrotec surface-treatment technology. Heat Treat. Met. 12, 70 (1985).Google Scholar
14Somers, M.A.J., Kooi, B.J., Sloof, W.G. and Mittemeijer, E.J.: On the oxidation of γ′-Fe4N1–x layers: Redistribution of nitrogen. Surf. Interface Anal. 19, 633 (1992).CrossRefGoogle Scholar
15Graat, P.C.J., Somers, M.A.J. and Mittemeijer, E.J.: The initial oxidation of ϵ-Fe2N1–x: An XPS investigation. Appl. Surf. Sci. 136, 238 (1998).CrossRefGoogle Scholar
16Jutte, R.H., Kooi, B.J., Somers, M.A.J. and Mittemeijer, E.J.: On the oxidation of α-Fe and ϵ-Fe2N1–z: I. Oxidation kinetics and microstructural evolution of the oxide and nitride layers. Oxid. Met. 48, 87 (1997).CrossRefGoogle Scholar
17Kooi, B.J., Somers, M.A.J., Jutte, R.H. and Mittemeijer, E.J.: On the oxidation of α-Fe and ϵ-Fe2N1–z: II. Residual strains and blisters in the oxide layer. Oxid. Met. 48, 111 (1997).CrossRefGoogle Scholar
18Graat, P.C.J., Somers, M.A.J. and Mittemeijer, E.J.: The initial oxidation of ϵ-Fe2N1–x: Growth kinetics. Thin Solid Films 353, 72 (1999).CrossRefGoogle Scholar
19Kooi, B.J., Somers, M.A.J. and Mittemeijer, E.J.: Growth kinetics of thin oxide layers: Oxidation of Fe and Fe-N phases at room temperature. Thin Solid Films 282, 488 (1996).CrossRefGoogle Scholar
20Liu, Z.Q., Hashimoto, H., Song, M., Mitsuishi, K. and Furuya, K.: Phase transformation from Fe4N to Fe3O4 due to electron irradiation in the transmission electron microscope. Acta Mater. 52, 1669 (2004).CrossRefGoogle Scholar
21Liu, Z.Q., Hashimoto, H., Sukedai, E., Song, M., Mitsuishi, K. and Furuya, K.: In situ observation of the formation of Fe3O4 in Fe4N (001) due to electron irradiation. Phys. Rev. Lett. 90, 255504 (2003).CrossRefGoogle ScholarPubMed
22Liu, Z.Q., Hei, Z.K. and Li, D.X.: Microstructural investigation of four kinds of γ′-Fe4N nitrides in ion-nitrided pure iron. J. Mater. Res. 17, 2621 (2002).CrossRefGoogle Scholar
23Liu, Z.Q., Chen, Y.X., Hei, Z.K., Li, D.X. and Hashimoto, H.: Microstructural investigation on the precipitation of α″ nitrides and α′′ → γ′ nitride transformation in ion-nitrided pure iron. Metall. Mater. Trans. A 32, 2681 (2001).CrossRefGoogle Scholar
24Takaoka, A., Ura, K., Mori, H., Katsuta, T., Matsui, I. and Hayashi, S.: Development of a new 3 MV ultra-high voltage electron microscope at Osaka University. J. Electron Microsc. 46, 447 (1997).CrossRefGoogle Scholar
25Yoshida, K.: A. Takaoka, S. Hayashi, and I. Matsui: Development of a remote operation system for an ultra-high-voltage electron microscope. J. Electron Microsc. 48, 865 (1999).CrossRefGoogle Scholar
26Takaoka, A., Yoshida, K., Mori, H., Hayashi, S., Young, S.J. and Ellisman, M.H.: International telemicroscopy with a 3 MV ultrahigh voltage electron microscope. Ultramicroscopy 83, 93 (2000).CrossRefGoogle ScholarPubMed
27Hashimoto, H., Endoh, H., Tomita, M., Ajika, N., Kuwabara, M., Hata, Y., Tsubokawa, Y., Honda, T., Harada, Y., Sakurai, S., Etoh, T. and Yokota, Y.: Construction and application of a 400 kV analytical atom resolution electron microscope. J. Electron Microsc. Tech. 3, 5 (1986).CrossRefGoogle Scholar
28Somers, M.A.J. and Mittemeijer, E.J.: Phase transformation and stress relaxation in γ′-Fe4N1–x surface layers during oxidation. Metall. Mater. Trans. A 21, 901 (1990).CrossRefGoogle Scholar
29Liu, Z.Q., Li, D.X., Hei, Z.K. and Hashimoto, H.: Identification of ϵ′-Fe2N and ϵ′-Fe3N superstructures studied with high-resolution electron microscopy. Scripta Mater. 45, 455 (2001).CrossRefGoogle Scholar
30Liu, Z.Q., Li, D.X., Hei, Z.K. and Hashimoto, H.: Electron diffraction study on ϵ′′ superstructure in the compound layer of ion-nitrided pure iron. Scripta Mater. 46, 179 (2002).CrossRefGoogle Scholar
31Graat, P.C.J., Zandbergen, H.W., Somers, M.A.J. and Mittemeijer, E.J.: Constitution and crystallography of thin thermal-oxide layers on ϵ-Fe2N1–x: A HREM investigation. Oxid. Met. 53, 221 (2000).CrossRefGoogle Scholar
32Shannon, R.D.: Revised effective ionic radii and systematic studies of interatomic distances in halides and chalcogenides. Acta Crystallogr., Sect. A 32, 751 (1976).CrossRefGoogle Scholar
33Jack, K.H.: Binary and ternary interstitial alloys I. The iron-nitrogen system: The structures of Fe4N and Fe2N. Proc. R. Soc. London, Ser. A 195, 34 (1948).Google Scholar
34Chambers, S.A.: Epitaxial growth and properties of thin film oxides. Surf. Sci. Rep. 39, 105 (2000).CrossRefGoogle Scholar