A Critical Comparison Among High-Resolution Methods for Spatially Resolved Nano-Scale Residual Stress Analysis in Nanostructured Coatings

Residual stresses in multilayer thin coatings represent a complex multiscale phenomenon arising from the intricate interplay of multiple factors, including the number and thickness of layers, material properties of the layers and substrate, coefficient of thermal expansion (CTE) mismatch, deposition technique and growth mechanism, as well as process parameters and environmental conditions. A multiscale approach to residual stress measurement is essential for a comprehensive understanding of stress distribution in such systems. To investigate this, two AlGaN/GaN multilayer coatings with distinct layer architectures were deposited on sapphire substrates using metalorganic vapor phase epitaxy (MOVPE). High-resolution X-ray diffraction (HRXRD) was employed to confirm their epitaxial growth and structural characteristics. Focused ion beam (FIB) cross-sectioning and transmission electron microscopy (TEM) lamella preparation were performed to analyze the coating structure and determine layer thickness. Residual stresses within the multilayer coatings were evaluated using two complementary techniques: High-Resolution Scanning Transmission Electron Microscopy—Graphical Phase Analysis (HRSTEM-GPA) and Focused Ion Beam—Digital Image Correlation (FIB-DIC). HRSTEM-GPA enables atomic-resolution strain mapping, making it particularly suited for investigating interface-related stresses, while FIB-DIC facilitates microscale stress evaluation. The residual strain values obtained using the FIB-DIC and HRSTEM-GPA methods were −3.2 × 10⁻3 and −4.55 × 10⁻3, respectively. This study confirms that residual stress measurements at different spatial resolutions are both reliable and comparable at the required coating depths and locations, provided that a critical assessment of the characteristic scale of each method is performed.