High-temperature deformation followed in situ by X-ray microtomography: a methodology to track features under large strain.

Metallic materials processing such as rolling, extrusion or forging often involves high-temperature deformation. Usually under such conditions the samples are characterized post mortem, under pseudo in situ conditions with interrupted tests, or in situ with a limited strain rate. A full in situ 3D characterization, directly during high-temperature deformation with a prescribed strain-rate scheme, requires a dedicated sample environment and a dedicated image-analysis workflow. A specific sample environment has been developed to enable highly controlled (temperature and strain rate) high-temperature deformation mechanical testing to be conducted while performing in situ tomography on a synchrotron beamline. A dedicated digital volume correlation algorithm is used to estimate the strain field and track pores while the material endures large deformations. The algorithm is particularly suitable for materials with few internal features when the deformation steps between two images are large. An example of an application is provided: a high-temperature compression test on a porous aluminium alloy with individual pore tracking with a specific strain-rate scheme representative of rolling conditions.

A deformation rig for synchrotron microtomography studies of geomaterials under conditions down to 10†km depth in the Earth.

A hard X-ray transparent triaxial deformation apparatus, called HADES, has been developed by Sanchez Technologies and installed on the microtomography beamline ID19 at the European Radiation Synchrotron Facility (ESRF). This rig can be used for time-lapse microtomography studies of the deformation of porous solids (rocks, ceramics, metallic foams) at conditions of confining pressure to 100 MPa, axial stress to 200 MPa, temperature to 250°C, and controlled aqueous fluid flow. It is transparent to high-energy X-rays above 60 keV and can be used for in situ studies of coupled processes that involve deformation and chemical reactions. The rig can be installed at synchrotron radiation sources able to deliver a high-flux polychromatic beam in the hard X-ray range to acquire tomographic data sets with a voxel size in the range 0.7-6.5 µm in less than two minutes.

Morphometric analysis of chameleon fossil fragments from the Early Pliocene of South Africa: a new piece of the chamaeleonid history.

The evolutionary history of chameleons has been predominantly studied through phylogenetic approaches as the fossil register of chameleons is limited and fragmented. The poor state of preservation of these fossils has moreover led to the origin of numerous nomen dubia, and the identification of many chameleon fossils remains uncertain. We here examine chameleon fossil fragments from the Early Pliocene Varswater formation, exposed at the locality of Langebaanweg "E" Quarry along the southwestern coast of South Africa. Our aim was to explore whether these fossil fragments could be assigned to extant genera. To do so, we used geometric morphometric approaches based on microtomographic imaging of extant chameleons as well as the fossil fragments themselves. Our study suggests that the fossils from this deposit most likely represent at least two different forms that may belong to different genera. Most fragments are phenotypically dissimilar from the South African endemic genus Bradypodion and are more similar to other chameleon genera such as Trioceros or Kinyongia. However, close phenetic similarities between some of the fragments and the Seychelles endemic Archaius or the Madagascan genus Furcifer suggest that some of these fragments may not contain enough genus-specific information to allow correct identification. Other fragments such as the parietal fragments appear to contain more genus-specific information, however. Although our data suggest that the fossil diversity of chameleons in South Africa was potentially greater than it is today, this remains to be verified based on other and more complete fragments.

Fragmentation and limits to dynamical scaling in viscous coarsening: an interrupted in situ x-ray tomographic study.

X-ray microtomography was used to follow the coarsening of the structure of a ternary silicate glass experiencing phase separation in the liquid state. The volumes, surfaces, mean, and Gaussian curvatures of the domains of minority phase were measured after reconstruction of the 3D images and segmentation. A linear growth law of the characteristic length scale ℓ∼t was observed. A detailed morphological study was performed. While dynamical scaling holds for most of the geometrical observables under study, a progressive departure from scaling invariance of the distributions of local curvatures was evidenced. The latter results from a gradual fragmentation of the structure in the less viscous phase that also leads to a power-law size distribution of isolated domains.

Slow but tenacious: an analysis of running and gripping performance in chameleons.

Chameleons are highly specialized and mostly arboreal lizards characterized by a suite of derived characters. The grasping feet and tail are thought to be related to the arboreal lifestyle of chameleons, yet specializations for grasping are thought to exhibit a trade-off with running ability. Indeed, previous studies have demonstrated a trade-off between running and clinging performance, with faster species being poorer clingers. Here we investigate the presence of trade-offs by measuring running and grasping performance in four species of chameleon belonging to two different clades (Chamaeleo and Bradypodion). Within each clade we selected a largely terrestrial species and a more arboreal species to test whether morphology and performance are related to habitat use. Our results show that habitat drives the evolution of morphology and performance but that some of these effects are specific to each clade. Terrestrial species in both clades show poorer grasping performance than more arboreal species and have smaller hands. Moreover, hand size best predicts gripping performance, suggesting that habitat use drives the evolution of hand morphology through its effects on performance. Arboreal species also had longer tails and better tail gripping performance. No differences in sprint speed were observed between the two Chamaeleo species. Within Bradypodion, differences in sprint speed were significant after correcting for body size, yet the arboreal species were both better sprinters and had greater clinging strength. These results suggest that previously documented trade-offs may have been caused by differences between clades (i.e. a phylogenetic effect) rather than by design conflicts between running and gripping per se.

Comparison of the 3D-microstructure of human alveolar and fibula bone in microvascular autologous bone transplantation: a synchrotron radiation µ-CT study.

Introduction: Autologous bone transplantation is successfully used in reconstructive surgery of large/critical-sized bone defects, whereby the microvascular free fibula flap is still regarded as the gold standard for the reconstruction of such defects in the head and neck region. Here, we report the morphological and lacunar properties of patient-paired bone samples from eight patients from the jaw (AB; recipient site) and the fibula (FB; donor site) on the micron length-scale using Synchrotron µ-CT. Insights into differences and similarities between these bone structures could offer a better understanding of the underlying mechanism for successful surgical outcomes and might clear the path for optimized, nature-inspired bone scaffold designs. Methods: Spatial vessel-pore arrangements, bone morphology, fluid-simulation derived permeability tensor, osteocyte lacunar density, and lacunar morphology are compared. Results: The orientation of the vessel system indicates a homogenous vessel orientation for AB and FB. The average mineral distance (50%) to the closest vessel boundary is higher in AB than in FB (the mean is 96 µm for AB vs. 76 µm for FB; p = 0.021). Average osteocyte lacunar density is found to be higher in AB than in FB (mean 22,874 mm3 vs. 19,376 mm3 for FB; p = 0.038), which might compensate for the high distance from the mineral to the nearest vessel. No significant differences in lacunar volume are found between paired AB and FB. Discussion: A comparable vessel network and similar distribution of vessel porosity between AB and FB may allow the FB graft to exhibit a high regeneration potential when connected to AB, and this might correlate with a high osteoinductive and osteoconductive potential of FB when connected to AB. Since widely used and potent synthetic bone grafts exist, new insight into the bone structure of well-established autologous bone grafts, such as the free fibula flap, could help to improve the performance of such materials and therefore the design of 3D scaffolds.

Nanoscale imaging of the bone cell network with synchrotron X-ray tomography: optimization of acquisition setup.

PURPOSE: The fundamental role of the osteocyte cell network in regulating the bone remodeling has become evident in the last years. This has raised the necessity to explore this complex three-dimensional interconnected structure, but the existing investigation methods cannot provide an adequate assessment. The authors propose to use parallel beam synchrotron radiation computed tomography at the nanoscale to image in three dimensions the osteocyte lacunocanalicular network. To this aim, the authors study the feasibility of this technique and present an optimized imaging protocol suited for the bone cell network. Moreover, they demonstrate the multifaceted information provided by this method. METHODS: The high brilliance of synchrotron radiation combined with state of art detectors permits reaching nanoscale spatial resolution. With a nominal pixel size of 280 nm, the parallel beam computed tomography setup at the ID19 experimental station of the ESRF is capable of imaging the bone lacunocanalicular network, considering that the reported diameter of canaliculi is in the range 300-600 nm. However, the actual resolution is limited by the detector and by the radiation dose causing sample damage during the scan. The authors sought to overcome these limitations by optimizing the imaging setup and the acquisition parameters in order to minimize the necessary radiation dose to create the images and to improve the spatial resolution of the detector. RESULTS: The authors achieved imaging of the osteocyte cell network in human bone. Due to the optimization of the imaging setup and acquisition parameters, they obtained simultaneously a radiation dose reduction and an increase of the signal to noise ratio in the images. This permitted the authors to generate the first three-dimensional images of the lacunocanalicular network in an area covering several osteons, the fundamental functional units in the bone cortex. The method enables assessment of both architectural parameters of the microporosity and of mineralization degree in the bone matrix. The authors found that the cell network is dense and connected inside osteonal tissue. Conversely, the cell lacunae are sparse, unorganized, and disconnected in interstitial tissue. CONCLUSIONS: The authors show that synchrotron radiation computed tomography is a feasible technique to assess the lacunocanalicular network in three dimensions. This is possible due to an optimal imaging setup in which the detector plays an important role. The authors could establish two valid setups, based on two different insertion devices. These results give access to new information on the bone cell network architecture, covering a number of cells two orders of magnitude greater than existing techniques. This enables biomedical studies on series of samples, paving the way to better understanding of bone fragility and to new treatments for bone diseases.

Miniature laser powder bed fusion system for in situ synchrotron x-ray micro-computed tomography experiments at the European Synchrotron Radiation Facility.

We describe our miniature laser powder bed fusion (L-PBF) system for in situ synchrotron x-ray micro-computed tomography (XCT) at the European Synchrotron Radiation Facility. This replicator was designed to extend the characterization of L-PBF to 3D. This instrument fills in a technical gap because the existing replicators were mostly designed to shed light on the dynamic mechanisms involved in molten pool formation but, therefore, suffered from a lack of 3D information. Technical details regarding the setup and beamline integration are given. Experimental validations via post-mortem XCT scans and in situ scans acquired during experiments conducted at the BM05 beamline of the European Synchrotron Radiation Facility are provided. Based on a few illustrative examples, we show that such a replicator opens the path to collect key 3D information that to date could not be available. Our miniature instrument complements the other replicators developed in the world by other research groups that enable operando x-ray imaging (radiography) and operando x-ray diffraction.

Comparison of the 3D-Microstructure Between Alveolar and Iliac Bone for Enhanced Bioinspired Bone Graft Substitutes.

In oral- and maxillofacial bone augmentation surgery, non-vascularized grafts from the iliac crest demonstrate better clinical performance than alveolar bone grafts. The underlying mechanisms are not fully understood but are essential for the enhancement of bone regeneration scaffolds. Synchrotron Radiation µ-CT at a pixel size of 2.3 µm was used to characterize the gross morphology and the vascular and osteocyte lacuna porosity of patient-matched iliac crest/alveolar bone samples. The results suggest a difference in the spatial distribution of the vascular pore system. Fluid simulations reveal the permeability tensor to be more homogeneous in the iliac crest, indicating a more unidirectional fluid flow in alveolar bone. The average distance between bone mineral and the closest vessel pore boundary was found to be higher in alveolar bone. At the same time, osteocyte lacunae density is higher in alveolar bone, potentially compensating for the longer average distance between the bone mineral and vessel pores. The present study comprehensively quantified and compared the 3D microarchitecture of intraindividual human alveolar and iliac bone. The identified difference in pore network architecture may allow a bone graft from the iliac crest to exhibit higher regeneration potential due to an increased capacity to connect with the surrounding pore network of the residual bone. The results may contribute to understanding the difference in clinical performance when used as bone grafts and are essential for optimization of future scaffold materials.

Assisted walking in Malagasy dwarf chamaeleons.

Chamaeleons are well known for their unique suite of morphological adaptations. Whereas most chamaeleons are arboreal and have long tails, which are used during arboreal acrobatic manoeuvres, Malagasy dwarf chamaeleons (Brookesia) are small terrestrial lizards with relatively short tails. Like other chamaeleons, Brookesia have grasping feet and use these to hold on to narrow substrates. However, in contrast to other chamaeleons, Brookesia place the tail on the substrate when walking on broad substrates, thus improving stability. Using three-dimensional synchrotron X-ray phase-contrast imaging, we demonstrate a set of unique specializations in the tail associated with the use of the tail during locomotion. Additionally, our imaging demonstrates specializations of the inner ear that may allow these animals to detect small accelerations typical of their slow, terrestrial mode of locomotion. These data suggest that the evolution of a terrestrial lifestyle in Brookesia has gone hand-in-hand with the evolution of a unique mode of locomotion and a suite of morphological adaptations allowing for stable locomotion on a wide array of substrates.

Correction: 4D synchrotron microtomography and pore-network modelling for direct in situ capillary flow visualization in 3D printed microfluidic channels.

Correction for '4D synchrotron microtomography and pore-network modelling for direct in situ capillary flow visualization in 3D printed microfluidic channels' by Agnese Piovesan et al., Lab Chip, 2020, 20, 2403-2411, DOI: .

4D synchrotron microtomography and pore-network modelling for direct in situ capillary flow visualization in 3D printed microfluidic channels.

Powder-based 3D printing was employed to produce porous, capillarity-based devices suitable for passive microfluidics. Capillary imbibition in such devices was visualized in situ through dynamic synchrotron X-ray microtomography performed at the European Synchrotron Radiation Facility (ESRF) with sub-second time resolution. The obtained reconstructed images were segmented to observe imbibition dynamics, as well as to compute the system effective contact angle and to generate a pore-network to model capillary imbibition. A contact angle gradient was observed resulting in a preferential wicking direction, with the central portion of the microfluidic channel filling faster than the edge areas. The contact angle analysis and the pore-network model results suggest that this is due to spatial variations in the material surface properties arising from both the 3D printing and the subsequent drying processes.

A peek into the origin of creep in sand.

This paper presents the results of an experimental study of the particle scale mechanisms that underpin creep, on-going deformations under constant external load, in dry non-cemented sand under 1D oedometric compression loading at 2500 kPa. Traditional observations on the boundary of the sample are complemented with simultaneous measurements of the 3D kinematics of both the entire grain assembly and details of grain-scale mechanisms using synchrotron based X-ray tomography at two different spatial resolutions. Both the continuum response and the local grain scale response are captured using two spatial resolutions, i.e.  6.5 µ m and 0.65 µ m respectively. The results, for the first time, illustrate that small displacements measured at the boundary can be the result of rather pronounced fracturing at the individual grain scale.

Revealing the Effect of Local Connectivity of Rigid Phases during Deformation at High Temperature of Cast AlSi12Cu4Ni(2,3)Mg Alloys.

The 3D microstructure and its effect on damage formation and accumulation during tensile deformation at 300 °C for cast, near eutectic AlSi12Cu4Ni2Mg and AlSi12Cu4Ni3Mg alloys has been investigated using in-situ synchrotron micro-tomography, complemented by conventional 2D characterization methods. An increase of Ni from 2 to 3 wt.% leads to a higher local connectivity, quantified by the Euler number χ, at constant global interconnectivity of rigid 3D networks formed by primary and eutectic Si and intermetallics owing to the formation of the plate-like Al-Ni-Cu-rich δ-phase. Damage initiates as micro-cracks through primary Si particles agglomerated in clusters and as voids at matrix/rigid phase interfaces. Coalescence of voids leads to final fracture with the main crack propagating along damaged rigid particles as well as through the matrix. The lower local connectivity of the rigid 3D network in the alloy with 2 wt.% Ni permits localized plastification of the matrix and helps accommodating more damage resulting in an increase of ductility with respect to AlSi12Cu4Ni3Mg. A simple load partition approach that considers the evolution of local connectivity of rigid networks as a function of strain is proposed based on in-situ experimental data.

3D multiscale imaging of human vocal folds using synchrotron X-ray microtomography in phase retrieval mode.

Human vocal folds possess outstanding abilities to endure large, reversible deformations and to vibrate up to more than thousand cycles per second. This unique performance mainly results from their complex specific 3D and multiscale structure, which is very difficult to investigate experimentally and still presents challenges using either confocal microscopy, MRI or X-ray microtomography in absorption mode. To circumvent these difficulties, we used high-resolution synchrotron X-ray microtomography with phase retrieval and report the first ex vivo 3D images of human vocal-fold tissues at multiple scales. Various relevant descriptors of structure were extracted from the images: geometry of vocal folds at rest or in a stretched phonatory-like position, shape and size of their layered fibrous architectures, orientation, shape and size of the muscle fibres as well as the set of collagen and elastin fibre bundles constituting these layers. The developed methodology opens a promising insight into voice biomechanics, which will allow further assessment of the micromechanics of the vocal folds and their vibratory properties. This will then provide valuable guidelines for the design of new mimetic biomaterials for the next generation of artificial larynges.

The Visible Cement Data Set.

With advances in x-ray microtomography, it is now possible to obtain three-dimensional representations of a material's microstructure with a voxel size of less than one micrometer. The Visible Cement Data Set represents a collection of 3-D data sets obtained using the European Synchrotron Radiation Facility in Grenoble, France in September 2000. Most of the images obtained are for hydrating portland cement pastes, with a few data sets representing hydrating Plaster of Paris and a common building brick. All of these data sets are being made available on the Visible Cement Data Set website at http://visiblecement.nist.gov. The website includes the raw 3-D datafiles, a description of the material imaged for each data set, example two-dimensional images and visualizations for each data set, and a collection of C language computer programs that will be of use in processing and analyzing the 3-D microstructural images. This paper provides the details of the experiments performed at the ESRF, the analysis procedures utilized in obtaining the data set files, and a few representative example images for each of the three materials investigated.