The mechanical properties such as compressive strength and nanohardness were investigated for Pinctada margaritifera mollusk shells. The compressive strength was evaluated through a uniaxial static compression test performed along the load directions parallel and perpendicular to the shell axis, respectively, while the hardness and Young modulus were measured using nanoindentation. In order to observe the crack propagation, for the first time for such material, the in-situ X-ray microscopy (nano-XCT) imaging (together with 3D reconstruction based on the acquired images) during the indentation tests was performed. The results were compared with these obtained during the micro-indentation test done with the help of conventional Vickers indenter and subsequent scanning electron microscopy observations. The results revealed that the cracks formed during the indentation start to propagate in the calcite prism until they reach a ductile organic matrix where most of them are stopped. The obtained results confirm a strong anisotropy of both crack propagation and the mechanical strength caused by the formation of the prismatic structure in the outer layer of P. margaritifera shell.

The combination of near edge X‐ray absorption spectroscopy with nanoscale X‐ray imaging is a powerful analytical tool for many applications in energy technologies, catalysis, which are critical to combat climate change, as well as microelectronics and life science. Materials from these scientific areas often contain key elements, such as Si, P, S, Y, Zr, Nb, and Mo as well as lanthanides, whose X‐ray absorption edges lie in the so‐called tender photon energy range 1.5–5.0 keV. Neither conventional grazing incidence grating nor crystal monochromators have high transmission in this energy range, thereby yielding the tender photon energy gap. To close this gap, a monochromator setup based on a multilayer coated blazed plane grating and plane mirror is devised. The measurements show that this novel concept improves the photon flux in the tender X‐ray regime by two‐orders‐of‐magnitude enabling previously unattainable laboratory and synchrotron‐based studies. This setup is applied to perform nanoscale spectromicroscopy studies. The high photon flux provides sufficient sensitivity to obtain the electronic structure of Mo in platinum‐free MoNi₄ nanoparticles for electrochemical energy conversion. Additionally, it is shown that the chemical bonding of nano‐structures in integrated circuits can be distinguished by the electronic configuration at the Si‐K edge.

Laboratory transmission X-ray microscopy with a spatial resolution of about 100 nm was used to image 3D interconnect structures and failures in microchips during mechanical loading, applied by a microDouble Cantilever Beam (micro-DCB) test. High-resolution 3D image sequences based on nano X-ray computed tomography (nano-XCT) are used to visualize crack opening and propagation in fully integrated multilevel on-chip interconnect structures of integrated circuits. The nondestructive investigation of sub-micron cracks during the in-situ micro-DCB test allows one to identify the weakest layers and interfaces, to image delamination along Cu/dielectric interfaces (adhesive failure) and fracture in dielectrics (cohesive failure), as well as to evaluate the robustness of Backend-of-Line stacks against process-induced thermomechanical stress.

High-resolution imaging of buried metal interconnect structures in advanced microelectronic products with full-field X-ray microscopy is demonstrated in the hard X-ray regime, i.e., at photon energies > 10 keV. The combination of two multilayer optics—a side-by-side Montel (or nested Kirkpatrick–Baez) condenser optic and a high aspect-ratio multilayer Laue lens—results in an asymmetric optical path in the transmission X-ray microscope. This optics arrangement allows the imaging of 3D nanostructures in opaque objects at a photon energy of 24.2 keV (In-Kα X-ray line). Using a Siemens star test pattern with a minimal feature size of 150 nm, it was proven that features < 150 nm can be resolved. In-Kα radiation is generated from a Ga-In alloy target using a laboratory X-ray source that employs the liquid-metal-jet technology. Since the penetration depth of X-rays into the samples is significantly larger compared to 8 keV photons used in state-of-the-art laboratory X-ray microscopes (Cu-Kα radiation), 3D-nanopattered materials and structures can be imaged nondestructively in mm to cm thick samples. This means that destructive de-processing, thinning or cross-sectioning of the samples are not needed for the visualization of interconnect structures in microelectronic products manufactured using advanced packaging technologies. The application of laboratory transmission X-ray microscopy in the hard X-ray regime is demonstrated for Cu/Cu₆Sn₅/Cu microbump interconnects fabricated using solid–liquid interdiffusion (SLID) bonding.