In this contribution, in-situ high-temperature high-energy synchrotron grazing incidence transmission X-ray diffraction technique will be introduced as a unique and powerful tool for characterization of microstructure, stress state and thermo-mechanical properties of nanostructured thin film materials. The method will be demonstrated for metastable AlCrN films, which undergo decomposition of the cubic structure into cubic and hexagonal constituents at temperatures above 800°C. The experiment performed at the German Synchrotron (DESY) at PETRA III allowed to study thermal stability of the film/substrate system and to describe stress-temperature-dependent decomposition routes of the metastable AlCrN solid solution.
Additionally, a newly developed synchrotron focusing setup based on Multilayer Laue Lenses at the beamline ID13 of the European Synchrotron Radiation Facility in Grenoble will be introduced, allowing to focus the X-ray beam down to 30 nm in diameter and to resolve depth gradients of microstructure and residual stresses within individual sublayers of multi-layered thin films with thicknesses below 50 nm. The capability of the focusing setup will be demonstrated for a 3 m-thick sculptured multi-layered TiN/SiOx film consisted of ~230 nm thick nano-crystalline TiN sublayers with zig-zag columnar grain morphology separated by amorphous SiOx sublayers, both prepared by oblique magnetron sputtering. The cross-sectional X-ray nanodiffraction analysis of the film revealed an oscillatory variation of the microstructure and compressive residual stresses across the film and gradually decreasing densities of structural defects within each TiN sublayer, exhibiting a sawtooth-like depth profile across the film.