Magnesium (Mg) - based alloys are becoming attractive materials for medical applications as temporary bone implants for support of fracture healing, e.g. as a suture anchor. Due to their mechanical properties and biocompatibility, they may replace titanium or stainless-steel implants, commonly used in orthopedic field. Nevertheless, patient safety has to be assured by finding a long-term balance between metal degradation, osseointegration, bone ultrastructure adaptation and element distribution in organs. In order to determine the implant behavior and its influence on bone and tissues, we investigated two Mg alloys with gadolinium contents of 5 and 10 wt percent in comparison to permanent materials titanium and polyether ether ketone. The implants were present in rat tibia for 10, 20 and 32 weeks before sacrifice of the animal. Synchrotron radiation-based micro computed tomography enables the distinction of features like residual metal, degradation layer and bone structure. Additionally, X-ray diffraction and X-ray fluorescence yield information on parameters describing the bone ultrastructure and elemental composition at the bone-to-implant interface. Finally, with element specific mass spectrometry, the elements and their accumulation in the main organs and tissues are traced. The results show that Mg-xGd implants degrade in vivo under the formation of a stable degradation layer with bone remodeling similar to that of Ti after 10 weeks. No accumulation of Mg and Gd was observed in selected organs, except for the interfacial bone after 8 months of healing. Thus, we confirm that Mg-5Gd and Mg-10Gd are suitable material choices for bone implants.

Osteogenesis imperfecta (OI) is a skeletal dysplasia characterized by low bone mass and frequent fractures. Children with OI are commonly treated with bisphosphonates to reduce fracture rate, but treatment options for adults are limited. In the Phase 2b ASTEROID trial, setrusumab (a sclerostin neutralizing antibody, SclAb) improved bone density and strength in adults with type I, III, and IV OI. Here, we investigate bone matrix material properties in tetracycline-labeled trans iliac biopsies from 3 groups: (1) control: individuals with no metabolic bone disease, (2) OI: individuals with OI, (3) SclAb-OI: individuals with OI after 6 mo of setrusumab treatment (as part of the ASTEROID trial). In addition to bone histomorphometry, bone mineral and matrix properties were evaluated with nanoindentation, Raman spectroscopy, second harmonic generation imaging, quantitative backscatter electron imaging, and small-angle X-ray scattering. Spatial locations of fluorochrome labels were identified to differentiate inter-label bone of the same tissue age and intra-cortical bone. No difference in collagen orientation was found between the groups. The bone mineral density distribution and analysis of Raman spectra indicate that OI groups have greater mean mineralization, greater relative mineral content, and lower crystallinity than the control group, which was not altered by SclAb treatment. Finally, a lower modulus and hardness were measured in the inter-label bone of the OI-SclAb group compared to the OI group. Previous studies suggest that even though bone from OI has a higher mineral content, the extracellular matrix (ECM) has comparable mechanical properties. Therefore, fragility in OI may stem from contributions from other yet unexplored aspects of bone organization at higher length scales. We conclude that SclAb treatment leads to increased bone mass while not adversely affecting bone matrix properties in individuals with OI.

Magnesium alloys are some of the most convenient biodegradable materials for bone fracture treatment due to their tailorable degradation rate, biocompatibility, and mechanical properties resembling those of bone. Despite the fact that magnesium-based implants and ZX00 (Mg-0.45Zn-0.45Ca in wt.%), in particular, have been shown to have suitable degradation rates and good osseointegration, knowledge gaps remain in our understanding of the impact of their degradation properties on the bone’s ultrastructure. Bone is a hierarchically structured material, where not only the microstructure but also the ultrastructure are important as properties like the local mechanical response are determined by it. This study presents the first comparative analysis of bone ultrastructure parameters with high spatial resolution around ZX00 and Ti implants after 6, 12, and 24 weeks of healing. The mineralization was investigated, revealing a significant decrease in the lattice spacing of the (002) Bragg’s peak closer to the ZX00 implant in comparison to Ti, while no significant difference in the crystallite size was observed. The hydroxyapatite platelet thickness and osteon density demonstrated a decrease closer to the ZX00 implant interface. Correlative indentation and strain maps obtained by scanning X-ray diffraction measurements revealed a higher stiffness and faster mechanical adaptation of the bone surrounding Ti implants as compared to the ZX00 ones. Thus, the results suggest the incorporation of Mg²⁺ ions into the bone ultrastructure, as well as a lower degree of remodeling and stiffness of the bone in the presence of ZX00 implants than Ti.

A compact voltage application setup has been developed for in situ electrical testing of organic field effect transistors in combination with X-ray scattering studies at a synchrotron beamlines. Challenges faced during real condition in-operando test of newly developed OFETs originated an idea of creation of a new setup which excludes number of factors that make experiments complicated. The application of the setup is demonstrated on a prototype of an organic transistors based on α,ω-dihexyl-α-quaterthiophene molecules. The new setup allows to monitor material structural changes by X-ray scattering under applied voltage conditions and their direct correlations. The versatile setup eliminates possible shadowing effects and short circuits due to misalignment of the contacts. The electrical stability of the prototypes was characterized by the application of different voltage values. Corresponding structural changes were monitored by grazing X-ray scattering technique before, during and after the voltage was applied. The selected oligothiophene material with proved transistor properties shows high stability and directional anisotropy under applied voltage conditions. Thanks to a compact and flexible design of the setup, different type of small dimension devices could be studied under external voltage conditions at various synchrotron beamlines. Graphical Abstract

A focused ion beam scanning electron microscope (FIB-SEM) is a powerful tool that is routinely used for scale imaging from the micro- to nanometer scales, micromachining, prototyping, and metrology. In spite of the significant capabilities of a FIB-SEM, there are inherent artefacts (e.g., structural defects, chemical interactions and phase changes, ion implantation, and material redeposition) that are produced due to the interaction of Ga⁺ or other types of ions (e.g., Xe⁺, Ar⁺, O⁺, etc.) with the sample. In this study, we analyzed lattice distortion and ion implantation and subsequent material redeposition in metallic micropillars which were prepared using plasma focus ion beam (PFIB) milling. We utilized non-destructive synchrotron techniques such as X-ray fluorescence (XRF) and X-ray nanodiffraction to examine the micropillars prepared using Xe⁺ ion energies of 10 keV and 30 keV. Our results demonstrate that higher Xe ion energy leads to higher density of implanted ions within the redeposited and milled material. The mixing of ions in the redeposited material significantly influences the lattice structure, causing deformation in regions with higher ion concentrations. Through an X-ray nanodiffraction analysis, we obtained numerical measurements of the strain fields induced in the regions, which revealed up to 0.2% lattice distortion in the ion bombardment direction.

Microstructural characterization of polycrystalline micropillars remains a significant challenge, particularly under time constraints such as those encountered during in situ or other time-sensitive experimental conditions, where appropriate data checks might assist in taking the right decision and have influence on the outcome of the experiment. In this study, we present a fast and efficient method for estimating local structural properties using scanning X-ray nanodiffraction—a technique widely employed in various dynamic and static micro- and nanoscale material investigations. The analysis targets the strongest diffraction peaks within the scattering pattern to extract essential information on grain orientation, size and lattice strain, while excluding weaker signals to streamline processing. As a case study, a γ-TiAl-based micropillar (Ti–46.5Al–5Nb), fabricated via Xe ⁺ plasma focused-ion-beam milling, was analyzed before and after 10% uniaxial compression. The micropillar's grain size significantly exceeded the X-ray beam size (∼300 nm ² ), and its known crystallographic orientation enabled accurate tracking of structural evolution. A direct point-to-point comparison between the undeformed and compressed states revealed localized microstructural changes associated with plastic deformation. This approach provides a rapid and reliable means of assessing microstructural evolution and demonstrates high potential for in situ and operando investigations of small-scale materials.