Tailoring the stress-depth profile in thin films; the case of γ′-Fe4N1-x

Homogeneous gamma '-Fe4N1-x thin films were produced by gas through-nitriding of iron thin films (thickness 800 nm) deposited onto Al2O3 substrates by Molecular Beam Epitaxy. The nitriding parameters were chosen such that the nitrogen concentration within the gamma ' thin films was considerably lower (x approximate to 0.05) than the stoichiometric value (x = 0). X-ray diffraction stress analysis at constant penetration depths performed after the nitriding step revealed the presence of tensile stress parallel to the surface; the tensile stress was shown to be practically constant over the entire film thickness. For further nitriding treatments, the parameters were adjusted such that nitrogen enrichment occurred near the specimen surface. The depth-dependent nitrogen enrichment could be monitored by evaluating the strain-free lattice parameter of gamma ' as a function of X-ray penetration depth and relating it to the nitrogen concentration employing a direct relation between lattice parameter and nitrogen concentration. The small compositional variations led to distinct characteristic stress-depth profiles. The stress changes non-monotonously with depth in the film as could be shown by non-destructive X-ray diffraction stress analysis at constant penetration depths. This work demonstrates that by a specific choice of a first and a subsequent nitriding treatment (employing different nitriding potentials and/or different temperatures for both treatments) controlled development of residual stress profiles is possible in thin iron-nitride surface layers. (C) 2011 Elsevier B.V. All rights reserved.