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Ultra-high-speed synchrotron-based hard X-ray (i.e. above 10 keV) imaging is gaining a growing interest in a number of scientific domains for tracking non-repeatable dynamic phenomena at spatio-temporal microscales. This work describes an optimized indirect X-ray imaging microscope designed to achieve high performance at micrometre pixel size and megahertz acquisition speed. The entire detector optical arrangement has an improved sensitivity within the near-ultraviolet (NUV) part of the emitted spectrum (i.e. 310-430 nm wavelength). When combined with a single-crystal fast-decay scintillator, such as LYSO:Ce (Lu 2-x Y x SiO 5 :Ce), it exploits the potential of the NUV light-emitting scintillators. The indirect arrangement of the detector makes it suitable for high-dose applications that require high-energy illumination. This allows for synchrotron single-bunch hard X-ray imaging to be performed with improved true spatial resolution, as herein exemplified through pulsed wire explosion and superheated near-nozzle gasoline injection experiments at a pixel size of 3.2 µm, acquisition rates up to 1.4 MHz and effective exposure time down to 60 ps., (open access.)

The ID10 beamline of the SESAME (Synchrotron-light for Experimental Science and Applications in the Middle East) synchrotron light source in Jordan was inaugurated in June 2023 and is now open to scientific users. The beamline, which was designed and installed within the European Horizon 2020 project BEAmline for Tomography at SESAME (BEATS), provides full-field X-ray radiography and microtomography imaging with monochromatic or polychromatic X-rays up to photon energies of 100 keV. The photon source generated by a 2.9 T wavelength shifter with variable gap, and a double-multilayer monochromator system allow versatile application for experiments requiring either an X-ray beam with high intensity and flux, and/or a partially spatial coherent beam for phase-contrast applications. Sample manipulation and X-ray detection systems are designed to allow scanning samples with different size, weight and material, providing image voxel sizes from 13 µm down to 0.33 µm. A state-of-the-art computing infrastructure for data collection, three-dimensional (3D) image reconstruction and data analysis allows the visualization and exploration of results online within a few seconds from the completion of a scan. Insights from 3D X-ray imaging are key to the investigation of specimens from archaeology and cultural heritage, biology and health sciences, materials science and engineering, earth, environmental sciences and more. Microtomography scans and preliminary results obtained at the beamline demonstrate that the new beamline ID10-BEATS expands significantly the range of scientific applications that can be targeted at SESAME., (open access.)

Laser-driven dynamic compression experiments of plastic materials have found surprisingly fast formation of nanodiamonds (ND) via X-ray probing. This mechanism is relevant for planetary models, but could also open efficient synthesis routes for tailored NDs. We investigate the release mechanics of compressed NDs by molecular dynamics simulation of the isotropic expansion of finite size diamond from different P-T states. Analysing the structural integrity along different release paths via molecular dynamic simulations, we found substantial disintegration rates upon shock release, increasing with the on-Hugnoiot shock temperature. We also find that recrystallization can occur after the expansion and hence during the release, depending on subsequent cooling mechanisms. Our study suggests higher ND recovery rates from off-Hugoniot states, e.g., via double-shocks, due to faster cooling. Laser-driven shock compression experiments of polyethylene terephthalate (PET) samples with in situ X-ray probing at the simulated conditions found diamond signal that persists up to 11 ns after breakout. In the diffraction pattern, we observed peak shifts, which we attribute to thermal expansion of the NDs and thus a total release of pressure, which indicates the stability of the released NDs., (© 2024. The Author(s).)

Failure-resistant designs are particularly crucial for bones subjected to rapid loading, as is the case for the ambush-hunting northern pike (Esox lucius). These fish have slim and low-density osteocyte-lacking bones. As part of the swallowing mechanism, the cleithrum bone opens and closes the jaw. The cleithrum needs sufficient strength and damage tolerance, to withstand years of repetitive rapid gape-and-suck cycles of feeding. The thin wing-shaped bone comprises anisotropic layers of mineralized collagen fibers that exhibit periodic variations in mineral density on the mm and micrometer length scales. Wavy collagen fibrils interconnect these layers yielding a highly anisotropic structure. Hydrated cleithra exhibit Young's moduli spanning 3-9 GPa where the yield stress of ∼40 MPa increases markedly to exceed ∼180 MPa upon drying. This 5x observation of increased strength corresponds to a change to brittle fracture patterns. It matches the emergence of compressive residual strains of ∼0.15% within the mineral crystals due to forces from shrinking collagen layers. Compressive stresses on the nanoscale, combined with the layered anisotropic microstructure on the mm length scale, jointly confer structural stability in the slender and lightweight bones. By employing a range of X-ray, electron and optical imaging and mechanical characterization techniques, we reveal the structure and properties that make the cleithra impressively damage resistant composites. STATEMENT OF SIGNIFICANCE: By combining structural and mechanical characterization techniques spanning the mm to the sub-nanometer length scales, this work provides insights into the structural organization and properties of a resilient bone found in pike fish. Our observations show how the anosteocytic bone within the pectoral gridle of these fish, lacking any biological (remodeling) repair mechanisms, is adapted to sustain natural repeated loading cycles of abrupt jaw-gaping and swallowing. We find residual strains within the mineral apatite nanocrystals that contribute to forming a remarkably resilient composite material. Such information gleaned from bony structures that are different from the usual bones of mammals showcases how nature incorporates smart features that induce damage tolerance in bone material, an adaptation acquired through natural evolutionary processes., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

Background: The stability of implant-abutment connection is crucial to minimize mechanical and biological complications. Therefore, an assessment of the microgap behavior and abutment displacement in different implant-abutment designs was performed., Methods: Four implant systems were tested, three with a conical implant-abutment connection based on friction fit and a cone angle < 12 ° (Medentika, Medentis, NobelActive) and a system with an angulated connection (< 40°) (Semados). In different static loading conditions (30 N - 90º, 100 N - 90º, 200 N - 30º) the microgap and abutment displacement was evaluated using synchrotron-based microtomography and phase-contrast radioscopy with numerical forward simulation of the optical Fresnel propagation yielding an accuracy down to 0.1 μm., Results: Microgaps were present in all implant systems prior to loading (0.15-9 μm). Values increased with mounting force and angle up to 40.5 μm at an off axis loading of 100 N in a 90° angle., Conclusions: In contrast to the implant-abutment connection with a large cone angle (45°), the conical connections based on a friction fit (small cone angles with < 12°) demonstrated an abutment displacement which resulted in a deformation of the outer implant wall. The design of the implant-abutment connection seems to be crucial for the force distribution on the implant wall which might influence peri-implant bone stability., (© 2024. The Author(s).)

Porosity in directed energy deposition (DED) deteriorates mechanical performances of components, limiting safety-critical applications. However, how pores arise and evolve in DED remains unclear. Here, we reveal pore evolution mechanisms during DED using in situ X-ray imaging and multi-physics modelling. We quantify five mechanisms contributing to pore formation, migration, pushing, growth, removal and entrapment: (i) bubbles from gas atomised powder enter the melt pool, and then migrate circularly or laterally; (ii) small bubbles can escape from the pool surface, or coalesce into larger bubbles, or be entrapped by solidification fronts; (iii) larger coalesced bubbles can remain in the pool for long periods, pushed by the solid/liquid interface; (iv) Marangoni surface shear flow overcomes buoyancy, keeping larger bubbles from popping out; and (v) once large bubbles reach critical sizes they escape from the pool surface or are trapped in DED tracks. These mechanisms can guide the development of pore minimisation strategies., (© 2024. The Author(s).)

X-ray multi-projection imaging (XMPI) has the potential to provide rotation-free 3D movies of optically opaque samples. The absence of rotation enables superior imaging speed and preserves fragile sample dynamics by avoiding the centrifugal forces introduced by conventional rotary tomography. Here, we present our XMPI observations at the ID19 beamline (ESRF, France) of 3D dynamics in melted aluminum with 1000 frames per second and 8 µm resolution per projection using the full dynamical range of our detectors. Since XMPI is a method under development, we also provide different tests for the instrumentation of up to 3000 frames per second. As the high-brilliance of 4th generation light-sources becomes more available, XMPI is a promising technique for current and future X-ray imaging instruments.

In this study, we use synchrotron-based multi-modal X-ray tomography to examine human cerebellar tissue in three dimensions at two levels of spatial resolution (2.3 µm and 11.9 µm). We show that speckle-based imaging (SBI) produces results that are comparable to propagation-based imaging (PBI), a well-established phase-sensitive imaging method. The different SBI signals provide complementary information, which improves tissue differentiation. In particular, the dark-field signal aids in distinguishing tissues with similar average electron density but different microstructural variations. The setup's high resolution and the imaging technique's excellent phase sensitivity enabled the identification of different cellular layers and additionally, different cell types within these layers. We also correlated this high-resolution phase-contrast information with measured dark-field signal levels. These findings demonstrate the viability of SBI and the potential benefit of the dark-field modality for virtual histology of brain tissue., Competing Interests: The authors declare no conflicts of interest., (© 2023 Optica Publishing Group under the terms of the Optica Open Access Publishing Agreement.)

X ray fluorescence ghost imaging (XRF-GI) was recently demonstrated for x ray lab sources. It has the potential to reduce the acquisition time and deposited dose by choosing their trade-off with a spatial resolution while alleviating the focusing constraints of the probing beam. Here, we demonstrate the realization of synchrotron-based XRF-GI: we present both an adapted experimental setup and its corresponding required computational technique to process the data. This extends the above-mentioned potential advantages of GI to synchrotron XRF imaging. In addition, it enables new strategies to improve resilience against drifts at all scales and the study of previously inaccessible samples, such as liquids.

Introduction: Recently, efforts towards the development of patient-specific 3D printed scaffolds for bone tissue engineering from bioactive ceramics have continuously intensified. For reconstruction of segmental defects after subtotal mandibulectomy a suitable tissue engineered bioceramic bone graft needs to be endowed with homogenously distributed osteoblasts in order to mimic the advantageous features of vascularized autologous fibula grafts, which represent the standard of care, contain osteogenic cells and are transplanted with the respective blood vessel. Consequently, inducing vascularization early on is pivotal for bone tissue engineering. The current study explored an advanced bone tissue engineering approach combining an advanced 3D printing technique for bioactive resorbable ceramic scaffolds with a perfusion cell culture technique for pre-colonization with mesenchymal stem cells, and with an intrinsic angiogenesis technique for regenerating critical size, segmental discontinuity defects in vivo applying a rat model. To this end, the effect of differing Si-CAOP (silica containing calcium alkali orthophosphate) scaffold microarchitecture arising from 3D powder bed printing (RP) or the Schwarzwalder Somers (SSM) replica fabrication technique on vascularization and bone regeneration was analyzed in vivo . In 80 rats 6-mm segmental discontinuity defects were created in the left femur. Methods: Embryonic mesenchymal stem cells were cultured on RP and SSM scaffolds for 7d under perfusion to create Si-CAOP grafts with terminally differentiated osteoblasts and mineralizing bone matrix. These scaffolds were implanted into the segmental defects in combination with an arteriovenous bundle (AVB). Native scaffolds without cells or AVB served as controls. After 3 and 6 months, femurs were processed for angio-µCT or hard tissue histology, histomorphometric and immunohistochemical analysis of angiogenic and osteogenic marker expression. Results: At 3 and 6 months, defects reconstructed with RP scaffolds, cells and AVB displayed a statistically significant higher bone area fraction, blood vessel volume%, blood vessel surface/volume, blood vessel thickness, density and linear density than defects treated with the other scaffold configurations. Discussion: Taken together, this study demonstrated that the AVB technique is well suited for inducing adequate vascularization of the tissue engineered scaffold graft in segmental defects after 3 and 6 months, and that our tissue engineering approach employing 3D powder bed printed scaffolds facilitated segmental defect repair., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest., (Copyright © 2023 Knabe, Stiller, Kampschulte, Wilbig, Peleska, Günster, Gildenhaar, Berger, Rack, Linow, Heiland, Rendenbach, Koerdt, Steffen, Houshmand, Xiang-Tischhauser and Adel-Khattab.)

Despite a century of research, our understanding of cement dissolution and precipitation processes at early ages is very limited. This is due to the lack of methods that can image these processes with enough spatial resolution, contrast and field of view. Here, we adapt near-field ptychographic nanotomography to in situ visualise the hydration of commercial Portland cement in a record-thick capillary. At 19 h, porous C-S-H gel shell, thickness of 500 nm, covers every alite grain enclosing a water gap. The spatial dissolution rate of small alite grains in the acceleration period, ∼100 nm/h, is approximately four times faster than that of large alite grains in the deceleration stage, ∼25 nm/h. Etch-pit development has also been mapped out. This work is complemented by laboratory and synchrotron microtomographies, allowing to measure the particle size distributions with time. 4D nanoimaging will allow mechanistically study dissolution-precipitation processes including the roles of accelerators and superplasticizers., (© 2023. The Author(s).)

X-rays are invaluable for imaging and sterilization of bones, yet the resulting ionization and primary radiation damage mechanisms are poorly understood. Here we monitor in-situ collagen backbone degradation in dry bones using second-harmonic-generation and X-ray diffraction. Collagen breaks down by cascades of photon-electron excitations, enhanced by the presence of mineral nanoparticles. We observe protein disintegration with increasing exposure, detected as residual strain relaxation in pre-stressed apatite nanocrystals. Damage rapidly grows from the onset of irradiation, suggesting that there is no minimal 'safe' dose that bone collagen can sustain. Ionization of calcium and phosphorous in the nanocrystals yields fluorescence and high energy electrons giving rise to structural damage that spreads beyond regions directly illuminated by the incident radiation. Our findings highlight photoelectrons as major agents of damage to bone collagen with implications to all situations where bones are irradiated by hard X-rays and in particular for small-beam mineralized collagen fiber investigations., (© 2022. The Author(s).)

Polymer based composites are widely used for treatment, for example as biofilm resistant seals of root canal fillings. Such clinical use, however, fails more frequently than other dental composite restorations, due to stress-related misfits. The reason for this is that the biomaterials used are inserted as viscous masses that may bond to the substrate, yet shrinkage stresses arising during setting of the cross-linking polymer, work against durable adhesion. Here we combine phase contrast enhanced time-lapse radiography (radioscopy), digital image correlation (DIC) and submicrometer resolution phase-contrast enhanced microtomography (PCE-CT), to reveal the spatial and temporal dynamics of composite polymerization and strain evolution. Radioscopy of cavities located in the upper part of human root canals demonstrates how the composite post-gelation "densification" is dominated by viscous flow with quantifiable motion of both particles and entrapped voids. Thereafter, these composites enter a "stress-relaxation" stage and exhibit several structural adaptations, induced by residual shrinkage stresses. Consequently critical alterations to the final biomaterial geometry emerge: (i) entrapped bubbles expand; (ii) microscopic root filling pull-out occurs; (iii) the cavity walls deform inwards, and (iv) occasionally delamination ensues, propagating out from the root canal filling along buried restoration-substrate interfaces. Our findings shed new light on the interactions between confined spaces and biomedical composites that cross-link in situ, highlighting the crucial role of geometry in channeling residual stresses. They further provide new insights into the emergence of structural flaws, calling attention to the need to find new treatment options. STATEMENT OF SIGNIFICANCE: This work quantifies recurring spatial and temporal material redistribution in composites used clinically to fill internal spaces in teeth. This knowledge is important for both promoting biomaterial resistance against potentially pathologic biofilms and for improving structural capacity to endure years of mechanical function. Our study demonstrates the significant role of geometry and the need for improved control over stress raisers to develop better treatment protocols and new space filling materials. The use of high-brilliance X-rays for time-lapse imaging at submicrometer resolution provides dynamic information about the damaging effects of stress relaxation due to polymerization shrinkage., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021. Published by Elsevier Ltd.)

Synchrotrons and free electron lasers are unique facilities to probe the atomic structure and electronic properties of matter at extreme thermodynamical conditions. In this context, 'matter at extreme pressures and temperatures' was one of the science drivers for the construction of low emittance 4th generation synchrotron sources such as the Extremely Brilliant Source of the European Synchrotron Radiation Facility and hard x-ray free electron lasers, such as the European x-ray free electron laser. These new user facilities combine static high pressure and dynamic shock compression experiments to outstanding high brilliance and submicron beams. This combination not only increases the data-quality but also enlarges tremendously the accessible pressure, temperature and density space. At the same time, the large spectrum of available complementary x-ray diagnostics for static and shock compression studies opens unprecedented insights into the state of matter at extremes. The article aims at highlighting a new horizon of scientific opportunities based on the synergy between extremely brilliant synchrotrons and hard x-ray free electron lasers., (Creative Commons Attribution license.)

Multiple myeloma (MM) bone disease is characterized by osteolytic bone tissue destruction resulting in bone pain, fractures, vertebral collapse, and spinal cord compression in patients. Upon initial diagnosis of MM, almost 80% of patients suffer from bone disease. Earlier diagnosis and intervention in MM bone disease would potentially improve treatment outcome and patient survival. New preclinical models are needed for developing novel diagnostic markers of bone structural changes as early as possible in the disease course. Here, we report a proof-of-concept, syngeneic, intrafemoral MOPC315.BM MM murine model in skeletally mature BALB/c mice for detection and characterization of very early changes in the extracellular matrix (ECM) of MM-injected animals. Bioluminescence imaging (BLI) in vivo confirmed myeloma engraftment in 100% of the animals with high osteoclast activity within 21 days after tumor cell inoculation. Early signs of aggressive bone turnover were observed on the outer bone surfaces by high-resolution microcomputed tomography (microCT). Synchrotron phase contrast-enhanced microcomputer tomography (PCE-CT) revealed very local microarchitecture differences highlighting numerous active sites of erosion and new bone at the micrometer scale. Correlative backscattered electron imaging (BSE) and confocal laser scanning microscopy allowed direct comparison of mineralized and nonmineralized matrix changes in the cortical bone. The osteocyte lacunar-canalicular network (OLCN) architecture was disorganized, and irregular-shaped osteocyte lacunae were observed in MM-injected bones after 21 days. Our model provides a potential platform to further evaluate pathological MM bone lesion development at the micro- and ultrastructural levels. These promising results make it possible to combine material science and pharmacological investigations that may improve early detection and treatment of MM bone disease., Competing Interests: The authors declare no conflicts of interest., (Copyright © 2020 Fani Ziouti et al.)

Ahead of Print article withdrawn by publisher.

State-of-the art, two-piece dental implants made from titanium alloys exhibit a complex micromechanical behavior under dynamical load. Its understanding, especially the formation of microgaps, is of crucial importance in order to predict and improve the long-term performance of such implants. Microgap formation in a loaded dental implant with a conical implant-abutment connection can be studied and quantified by synchrotron radiography with micrometer accuracy. Due to the high costs and limited access to synchrotron radiation sources, alternative approaches are needed in order to depict the microgap formation. Therefore, synchrotron radiography is used in this article to validate a simple finite element model of an experimental conical implant design. Once validated, the model is in turn employed to systematically study the microgap formation developed in a variety of static load scenarios and the influence of the preload of abutment screw on the microgap formation. The size of the microgap in finite element analysis (FEA) simulations is consistent with that found in in-vitro experiments. Furthermore, the FE approach gives access to more information such as the von-Mises stresses. It is found that the influence of the abutment screw preload has only a minor effect on the microgap formation and local stress distribution. The congruence between FE simulations and in-vitro measurements at the micrometer scale underlines the validity and relevance of the simple FE method applied to study the micromovement of the abutment and the abutment screw preload in conical implant-abutment connections under load.

Severe plastic deformation of solids is relevant to many materials processing techniques as well as tribological events such as wear. It results in microstructural refinement, redistribution of phases, and ultimately even mixing. However, mostly due to inability to experimentally capture the dynamics of deformation, the underlying physical mechanisms remain elusive. Here, we introduce a strategy that reveals details of morphological evolution upon shearing up to ultrahigh strains. Our experiments on metallic multilayers find that mechanically stronger layers either fold in a quasi-regular manner and subsequently evolve into periodic vortices, or delaminate into finer layers before mixing takes place. Numerical simulations performed by treating the phases as nonlinear viscous fluids reproduce the experimental findings and reveal the origin for emergence of a wealth of morphologies in deforming solids. They show that the same instability that causes kilometer-thick rock layers to fold on geological timescales is acting here at micrometer level.

The purpose of this study was to evaluate bone-to-implant contact (BIC) in two-dimensional (2D) histology compared to high-resolution three-dimensional (3D) synchrotron radiation micro computed tomography (SR micro-CT). High spatial resolution, excellent signal-to-noise ratio, and contrast establish SR micro-CT as the leading imaging modality for hard X-ray microtomography. Using SR micro-CT at voxel size 5 μm in an experimental goat mandible model, no statistically significant difference was found between the different treatment modalities nor between recipient and reconstructed bone. The histological evaluation showed a statistically significant difference between BIC in reconstructed and recipient bone (p < 0.0001). Further, no statistically significant difference was found between the different treatment modalities which we found was due to large variation and subsequently due to low power. Comparing histology and SR micro-CT evaluation a bias of 5.2% was found in reconstructed area, and 15.3% in recipient bone. We conclude that for evaluation of BIC with histology and SR micro-CT, SR micro-CT cannot be proven more precise than histology for evaluation of BIC, however, with this SR micro-CT method, one histologic bone section is comparable to the 3D evaluation. Further, the two methods complement each other with knowledge on BIC in 2D and 3D., (Copyright © 2017 European Association for Cranio-Maxillo-Facial Surgery. Published by Elsevier Ltd. All rights reserved.)