The grazing incidence diffraction (GID) method in side inclination mode, described by Ma et al. in 2002, of polycrystalline thin-film residual stress was revisited and explained using simple geometric relations. To overcome the issue of decreasing peak intensity of this method, which is induced by the decreasing incident angle because of the Eulerian cradle Chi-tilt, an improvement of Omega (ω)–Phi (φ) compensation was devised and applied to a NiFe thin-film sample. The geometry of this improved ω–φ compensated GID method in side inclination mode is detailed in this paper. This improvement guarantees a constant incident angle on the sample surface and a fixed sample illumination volume during measurement. The measured data were analysed using parametric refinement in DIFFRAC.TOPAS v6 software in Launch Mode, and details of the input file (.INP) are explained in this paper. The tensile stress of the NiFe thin-film sample was measured to be 1181 ± 85 MPa using this improved method.

In this study, the application of (an)isotropic size determination using a recently proposed model for the double-Voigt approach is demonstrated and validated against line profile simulations using the Whole Powder Pattern Modelling approach. The fitting of simulated line profiles demonstrates that the attained crystallite sizes and morphologies are in very reasonable agreement with the simulated values and thus demonstrate that even in routine application scenarios credible size and morphology information can be obtained using the double-Voigt approximation. The aim of this contribution is to provide a comprehensive introduction to the problem, address the practical application of the developed model, and discuss the accuracy of the double-Voigt approach and derived size parameters. Mathematical formulations for the visualization of modeled morphologies, supporting the application of the recently developed macros, are additionally provided.

Two applications of parametric Rietveld refinement employing a newly developed robust computer program are presented. The first application focuses on the parametric kinetic analysis of the reactions involving phase transitions of various polymorphic forms of copper phthalocyanine pigments. The second application concerns the parameterization of crystallite size with respect to experimental temperature. XRPD data for nanocrystalline titanium dioxide measured in dependence on temperature are used in this case study. Both the applications were realized with the help of the developed program in combination with the launch mode of topas® software.