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Iron-Nitride Compound Layers: Composition- and Stress-Depth Profiles Thomas Gressmann, Andreas Leineweber, Eric Jan Mittemeijer

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Iron-Nitride Compound Layers: Composition- and Stress-Depth Profiles Thomas Gressmann, Andreas Leineweber, Eric Jan Mittemeijer X-ray diffraction line-profile analysis of hexagonal ϵ-iron-nitride compound layers: composition- and stress-depth profiles Thomas Gressmann, Andreas Leineweber, Eric Jan Mittemeijer To cite this version: Thomas Gressmann, Andreas Leineweber, Eric Jan Mittemeijer. X-ray diffraction line-profile analysis of hexagonal ϵ-iron-nitride compound layers: composition- and stress-depth profiles. Philosophical Magazine, Taylor & Francis, 2008, 88 (02), pp.145-169. 10.1080/14786430701798936. hal-00513847 HAL Id: hal-00513847 https://hal.archives-ouvertes.fr/hal-00513847 Submitted on 1 Sep 2010 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Philosophical Magazine & Philosophical Magazine Letters For Peer Review Only X-ray diffraction line-profile analysis of hexagonal -iron-nitride compound layers: composition- and stress-depth profiles Journal: Philosophical Magazine & Philosophical Magazine Letters Manuscript ID: TPHM-07-Jul-0199.R1 Journal Selection: Philosophical Magazine Date Submitted by the 24-Oct-2007 Author: Complete List of Authors: Gressmann, Thomas; Max Planck Institute for Metals Research Leineweber, Andreas; Max Planck Institute for Metals Research Mittemeijer, Eric Jan; Max Planck Institute for Metals Research, Prof. Dr Ir. E.J. Mittemeijer metallic materials, microstructural characterization, nitrides, stress Keywords: analysis, X-ray diffraction line-profile analysis, grain interaction, anisotropic thermal Keywords (user supplied): expansion http://mc.manuscriptcentral.com/pm-pml Page 1 of 52 Philosophical Magazine & Philosophical Magazine Letters 1 2 3 4 X-ray diffraction line-profile analysis of hexagonal -iron-nitride compound 5 6 layers: composition- and stress-depth profiles 7 T. GRESSMANN, A. LEINEWEBER*, E. J. MITTEMEIJER 8 9 Max Planck Institute for Metals Research, Heisenbergstraße 3, D-70569 Stuttgart, Germany 10 11 *corresponding author 12 13 14 15 16 For Peer Review Only 17 18 Authors: 19 20 Thomas Gressmann 21 Tel.: +49 711 689 3369 22 E-mail: [email protected]; 23 24 Dr. Andreas Leineweber 25 Tel.: +49 711 689 3365 26 E-mail: [email protected]; 27 28 Prof. Dr. Ir. Eric Jan Mittemeijer 29 Tel.: +49 711 689 3311 30 31 E-mail: [email protected]; 32 33 34 Max Planck Institute for Metals Research, Heisenbergstrasse 3, D-70569 Stuttgart, Germany 35 36 Fax: +49 711 689 3312 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 - 1 - http://mc.manuscriptcentral.com/pm-pml Philosophical Magazine & Philosophical Magazine Letters Page 2 of 52 1 2 3 4 Abstract 5 6 Two hexagonal =-Fe3N1+x layers grown on >-Fe substrates by nitriding in NH3/H2 gas atmospheres 7 8 were investigated by high-resolution X-ray powder diffraction using synchrotron radiation 9 10 employing systematic tilting of the diffraction vector with respect to the specimen surface. The 11 12 13 obtained complicatedly shaped diffraction profiles, considering all recorded reflections 14 15 simultaneously, were analysed using a model incorporating hkl-dependent (anisotropic) and tilt- 16 For Peer Review Only 17 angle () dependent diffraction-line broadening and diffraction-line shifting. The diffraction-line 18 19 20 broadening is mainly ascribed to the nitrogen concentration-depth profile within the layers 21 22 causing depth-dependent strain-free lattice parameters, whereas the line shifts are predominantly 23 24 25 caused by the stress-depth profile originating from the concentration-dependence of the 26 27 coefficients of thermal expansion of the = phase, with stress parallel to the surface which is of 28 29 tensile nature at the surface and of compressive nature at the =/DE interface. This stress gradient 30 31 32 additionally leads to a -dependence of the line broadening. Fitting of the microstructure and 33 34 diffraction model led to determination of microstructure parameters, which can be related to the 35 36 different sets of treatment conditions applied for the =-iron-nitride layer growth. 37 38 39 40 41 42 43 Keywords: metallic materials, stress analysis, X-ray diffraction, nitrides, microstructural 44 45 characterization, line-profile analysis, grain interaction, anisotropic thermal expansion 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 - 2 - http://mc.manuscriptcentral.com/pm-pml Page 3 of 52 Philosophical Magazine & Philosophical Magazine Letters 1 2 3 4 5 6 1 Introduction 7 8 In the field of materials science there is a great demand for methods for depth-dependent 9 10 characterisation of the microstructure of polycrystalline thin films and surface layers, especially 11 12 13 recognising that in many specimens/workpieces the properties change with depth. Depth profiling 14 15 by determination of depth-dependent (micro-)structural features (e.g. lattice parameters – 16 For Peer Review Only 17 associated with composition, macrostresses, microstresses, crystallite size), is often realised in a 18 19 20 destructive manner either by cutting a piece out of the specimen/workpiece of interest and 21 22 investigation of the thus produced cross section (e.g. by electron probe microanalysis (EPMA)), or 23 24 25 by successive removal of sublayers of material from the surface by methods like polishing and 26 27 analysis of the occurring surface or near surface volume (e.g. by means of X-ray diffraction 28 29 (XRD)) [1]. These types of depth profiling are destructive and, moreover, upon removal of 30 31 32 material from the surface the characteristics of the investigated material may change, e.g. a 33 34 redistribution of stress in the remaining material occurs because of the requirement of mechanical 35 36 equilibrium and also stress may be induced by the removal of material. Hence, a non-destructive 37 38 39 method is desired. The method developed and applied in this work is based on non-destructive 40 41 high-resolution X-ray powder-diffraction analysis: The positions and full shapes of diffraction- 42 43 line profiles recorded under variation of the orientation of the diffraction vector with respect to the 44 45 46 surface are interpreted in terms of an absorption-weighted superposition of the diffraction effects 47 48 in the detected signal arising from different depths and as influenced by changes in composition 49 50 51 and stress. 52 53 54 55 [Insert Fig. 1 about here] 56 57 58 59 60 - 3 - http://mc.manuscriptcentral.com/pm-pml Philosophical Magazine & Philosophical Magazine Letters Page 4 of 52 1 2 3 The system iron-nitrogen is not only scientifically of great interest in metallurgy but also 4 5 6 plays an important role in technology [2, 3]: in particular iron-nitride phases as surface layers on 7 8 iron or steel workpieces are of great importance, since they can improve the corrosion resistance 9 10 and the tribological properties of the surface region [4, 5]. Iron-nitride phases are typically 11 12 13 generated by nitriding iron or steel in NH3/H2 gas mixtures at temperatures between 773 K and 14 15 863 K. During the nitriding process the >-iron substrate becomes enriched with nitrogen and, if 16 For Peer Review Only 17 18 the chemical potential of nitrogen in the applied gas mixture is sufficiently high, a compound 19 20 layer forms composed of an outer surface-adjacent =-Fe3N1+x sublayer (for the = phase also 21 22 formulas like Fe2N1-z and FeNy with y = (1 + x)/3 are used in literature) and an inner DE-Fe4N 23 24 1 25 sublayer adjacent to the >-iron substrate (Fig. 1) . Both, the = and the DE phase contain a close- 26 27 packed stacking of the iron atoms, with hcp for = and fcc for DE, in which the nitrogen atoms 28 29 occupy octahedral interstitial sites in a more or less long-range ordered fashion [6-10]. Especially 30 31 32 the = phase is of great interest, since its homogeneity range is quite large, e.g. at 823 K from about 33 34 24 at.% N to about 33 at.% N [11] (Fig. 2). These concentration variations are associated with 35 36 considerable variations of the lattice parameters a and c. It is well known that within the = layer a 37 38 39 concentration gradient builds up during the nitriding process due to the inward diffusion of 40 41 nitrogen from the gas atmosphere to the bulk [12], with higher nitrogen contents at the surface of 42 43 44 the specimen and with lower nitrogen contents at the =/DE interface, implying a strong depth 45 46 dependence of the lattice parameters. Various dependencies of the lattice parameters on the 47 48 composition of the = phase have been reported [7, 13-18]. The data from the different sources vary 49 50 51 considerably. Furthermore, it was shown recently that the lattice parameters depend not only on 52 53 the nitrogen content but also to a significant extent on the degree of nitrogen ordering induced by 54 55 the type of cooling procedure employed after nitriding or heat treatment [18]. 56 57 58 59 60 1 For nitriding steels, composed of many different alloying elements, often no clear distinction between the sublayers is possible. - 4 - http://mc.manuscriptcentral.com/pm-pml Page 5 of 52 Philosophical Magazine & Philosophical Magazine Letters 1 2 3 [Insert Fig. 2 about here] 4 5 6 7 8 Additional to the concentration gradient, a macrostress-depth profile will likely build up 9 10 within the = layer.
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