Synchrotron X-ray Microtomography Research Articles

Dental cementum virtual histology of Neanderthal teeth from Krapina (Croatia, 130-120 kyr): an informed estimate of age, sex and adult stressors.

The evolution of modern human reproductive scheduling is an aspect of our life history that remains vastly uncomprehended. The present work aims to address this gap by validating a non-destructive cutting-edge methodology to infer adult life-history events on modern teeth with known life history and then applying it to fossil specimens. We use phase-contrast synchrotron X-ray microtomography to visualize the dental cementum of 21 specimens: nine contemporary humans; 10 Neanderthals from Krapina (Croatia, 130-120 kyr); one Neolithic Homo sapiens from Ajmana (Serbia); and one Mesolithic H. sapiens from Vlasac (Serbia). We were able to correctly detect and time (root mean square error = 2.1 years; R2 = 0.98) all reproductive (menarche, parturition, menopause) and other physiologically impactful events in the modern sample. Nonetheless, we could not distinguish between the causes of the events detected. For the fossil specimens, we estimated age at death and age at occurrence of biologically significant events. Finally, we performed an exploratory analysis regarding possible sexual dimorphism in dental cementum microstructure, which allowed us to correctly infer the sex of the Neolithic specimen, for which the true value was known via DNA analysis.

Time-resolved 3D characterisation of early-age microstructural development of Portland cement

Time-resolved in-situ synchrotron X-ray microtomography reveals new levels of detail about the chemical and physical processes that take place as Portland cement hardens. The conversion of a fluid paste into a hardened product can be monitored on a sub-minute time-scale, and with sample movement/settlement corrections applied to enable individual particles to be tracked as they react, hydrate, and become interconnected into a single strong monolith. The growth of the strength-giving hydrate phases surrounding cement grains, and of the fluid-filled pore network that surrounds them, is able to be directly viewed at the level of individual cement particles through the application of this tracking protocol. When cement is brought into contact with water, a layer which differs in density from the bulk of the cement grains becomes observable on the grain surfaces during the induction period (during which time the heat evolution from the paste is relatively low). As hydration continues, reaction products grow both from particle surfaces into the initially fluid-filled region, and also into the space originally occupied by the cement particles, forming a density gradient within the microstructure. As the reaction accelerates and larger volumes of solid phases precipitate, the newly-formed solid structure percolates via interconnection of agglomerated low-density outer hydrates, which then densify as hydration continues. This eventually leads to solidification of the structure into a hardened porous matrix.Graphical abstract

Redescription of the Planthopper Bursinia genei (Dufour, 1849), with a New Record from Greece (Hemiptera: Fulgoromorpha: Dictyopharidae).

Bursinia genei (Dufour, 1849) is the most widespread species of the planthopper subfamily Orgeriinae (Hemiptera: Fulgoromorpha: Dictyopharidae) in Europe, found from the Iberian Peninsula to the Western Balkans. However, its diagnostically important genitalia and biology have been insufficiently described. We employ state-of-the-art synchrotron X-ray microtomography and photomicrography to re-describe B. genei, and to study the morphology of both its sexes in unprecedented detail. By examining specimens from across the distribution of B. genei, we find that they probably belong to a single, broadly distributed morphospecies. Our morphological examination allowed us to make inferences on its jumping mechanism and capacity for vibrational communication. We also record B. genei for the first time from Greece, further extending the range of this elusive species. Detailed information on the habitat of B. genei is also provided.

Metakaolin-based geopolymers: Efflorescence and its effect on microstructure and mechanical properties

Efflorescence in geopolymers results from mobility of excess alkali and consequent crystallization of alkali carbonates. Efflorescence potential of various geopolymers has been reported previously but the knowledge regarding the effect of efflorescence on the microstructure and mechanical properties of geopolymers remains limited. In this work, metakaolin-based geopolymers were exposed to air, partially immersed in water, and fully immersed, to simulate different processes involved in efflorescence formation. The mechanical properties were assessed by compressive, splitting tensile and flexural strengths, and linear deformation. The microstructural features were investigated by SEM, synchrotron XRD, multinuclear MAS NMR, MIP and synchrotron X-ray microtomography. Extensive efflorescence resulted in a reduction of mechanical strength and changes in the nanostructure and microstructure, which is different from observations for Portland cement-based materials, where efflorescence is usually regarded as a surface or aesthetic problem. The understanding of the relationship between efflorescence formation, the synthesis and exposure conditions provides important insight into the manufacturing and application conditions of geopolymer related materials.

Pore-Scale Investigation of Dynamic Immiscible Displacement in Layered Media using Synchrotron X-ray Microtomography.

Understanding the dynamics of immiscible fluid in a porous media is critical in many chemical and environmental engineering processes. However, the geological heterogeneity effect on multiphase flow behavior remains unclear. Here, the dynamics of immiscible fluid displacement and entrapment were experimentally demonstrated at pore-level using time-lapse synchrotron X-ray microtomography. A drainage-imbibition experiment was designed using an unconsolidated layered sand pack that comprised coarse sand and fine sand zones. There were significant differences between the two zones, with regard to the temporal variations in fluid saturation and morphological evolution of nonwetting fluid (oil) during imbibition. Highly connected oil clusters in the coarse zone broke up into many small fragments, whereas the cluster in the fine zone remained connected while spanning multiple pores. To further understand the impacts of pore size and connectivity on multiphase fluid dynamics, a new approach that tracks the temporal variation of immiscible fluid in individual pores was conducted. The surface area at the oil-water interface increased during imbibition, which is expected to facilitate mass transfer and surface interactions. Understanding immiscible fluid displacement in layered porous media at the pore-level could lead to more effective environmental remediation.

3D Characterization of Sponge Cake as Affected by Freezing Conditions Using Synchrotron X-ray Microtomography at Negative Temperature.

In this study, the microstructural evolution of a non-reactive porous model food (sponge cake) during freezing was investigated. Sponge cake samples were frozen at two different rates: slow freezing (0.3 °C min−1) and fast freezing (17.2 °C min−1). Synchrotron X-ray microtomography (µ-CT) and cryo-scanning electron microscopy (Cryo-SEM) were used to visualize and analyze the microstructure features. The samples were scanned before and after freezing using a specific thermostated cell (CellStat) combined with the synchrotron beamline. Cryo-SEM and 3D µ-CT image visualization allowed a qualitative analysis of the ice formation and location in the porous structure. An image analysis method based on grey level was used to segment the three phases of the frozen samples: air, ice and starch. Volume fractions of each phase, ice local thickness and shape characterization were determined and discussed according to the freezing rates.

3D characterisation of hydrogen environmentally assisted cracking during static loading of AA7449-T7651

In this investigation, synchrotron X-ray microtomography was used to perform 3D in situ observations of crack initiation and growth during hydrogen environmentally assisted cracking (HEAC) in tensile samples of AA7449-T7651. Two smooth tensile samples with a 1 mm diameter gauge section were held at a fixed displacement (approx 30% of yield stress) in warm, moist air (approx 76,^circ C, 73% relative humidity). The samples were then imaged repeatedly using X-ray tomography until they fractured completely. The tomograms showing the nucleation and evolution of intergranular cracks were correlated with electron microscopy fractographs. This enabled the identification of crack initiation sites and the characterisation of the crack growth behaviour relative to the microstructure. The samples were found to fracture within an environmental exposure time of 240 min. Some cracks in both samples nucleated within an exposure time of 80 min (33–40% of the total lifetime). Many cracks were found to nucleate both internally and at the sample surface. However, only superficial cracks contributed to the final fracture surface as they grew faster owing to the direct environmental exposure and the larger crack opening. HEAC occurred prominently via brittle intergranular cracking, and cracks were found to slow down when approaching grain boundary triple junctions. Additionally, crack shielding from nearby cracks and the presence of coarse Al–Cu–Fe particles at the grain boundaries were also found to temporarily reduce the crack growth rates. After prolonged crack growth, the HEAC cracks displayed ductile striations and transgranular fracture, revealing a change in the crack growth mechanism at higher stress intensity factors.

4D microstructural changes in dentinal tubules during acid demineralisation

ObjectiveDental erosion is a common oral condition caused by chronic exposure to acids from intrinsic/extrinsic sources. Repeated acid exposure can lead to the irreversible loss of dental hard tissues (enamel, dentine, cementum). Dentine can become exposed to acid following severe enamel erosion, crown fracture, or gingival recession. Causing hypersensitivity, poor aesthetics, and potential pulp involvement. Improving treatments that can restore the structural integrity and aesthetics are therefore highly desirable. Such developments require a good understanding of how acid demineralisation progresses where relatively little is known in terms of intertubular dentine (ITD) and peritubular dentine (PTD) microstructure. To obtain further insight, this study proposes a new in vitro method for performing demineralisation studies of dentine. MethodsAdvanced high-speed synchrotron X-ray microtomography (SXM), with high spatial (0.325 μm) and temporal (15 min) resolution, was used to conduct the first in vitro, time-resolved 3D (4D) study of the microstructural changes in the ITD and PTD phases of human dentine samples (∼0.8 × 0.8 × 5 mm) during 6 h of continuous acid exposure. ResultsDifferent demineralisation rates of ITD (1.79 μm/min) and PTD (1.94 μm/min) and their progressive width-depth profiles were quantified, which provide insight for understanding the mechanisms of dentine demineralisation. SignificanceInsights obtained from morphological characterisations and the demineralisation process of ITD and PTD during acid demineralisation would help understand the demineralisation process and potentially aid in developing new therapeutic dentine treatments. This method enables continuous examination of relatively large volumes of dentine during demineralisation and also demonstrates the potential for studying the remineralisation process of proposed therapeutic dentine treatments.

Pore-Scale Oil Connectivity and Displacement by Controlled-Ionic-Composition Waterflooding Using Synchrotron X-Ray Microtomography

Summary Controlled-ionic-composition waterflooding is an economic and effective method to improve oil recovery in carbonate oil reservoirs. Recent studies show controlling the salinity and ionic composition of injection water can alter the wettability of carbonate mineral surfaces. The pore-scale oil connectivity and displacement by controlled-ionic-composition waterflooding in heterogeneous carbonate reservoirs, especially at the early stage, is still unclear. The goal of this study is to examine the role of ion concentrations and types in the oil displacement efficiency and investigate the impact of the waterflooding on the pore-scale oil displacement using the national synchrotron facility. A carbonate rock sample was flooded with synthetic high-salinity water and other water solutions with different sulfate concentrations. The waterflooding processes were visualized with synchrotron X-ray microtomography to follow the evolution of pore-scale oil/brine interactions at typical field flow rates. Experimental results show that the water with lower sulfate concentration and higher salinity did not change the wettability of the pore surfaces. Higher sulfate ion concentrations in the water, in contrast, altered the wettability of carbonate pore surfaces from oil-wet to neutral-wet within the first few minutes of waterflooding. Novel insight was gained on the ability of water with high-sulfate concentration to displace oil in the small pores and through abundant oil channels, which could consequently lead to higher oil recovery from the carbonate rock.

Paleohistology of the Cretaceous resin-producing conifer Geinitzia reichenbachii using X-ray synchrotron microtomography.

The conifer Geinitzia reichenbachii was a common member of the Cretaceous Laurasian floras. However, the histology of G. reichenbachii leafy axes was never described in detail, and our knowledge of its paleoecology remains very limited. Using new and exquisitely preserved silicified material from the Upper Cretaceous of western France, we describe G. reichenbachii from the gross morphology to the cellular scale, then discuss paleoecological and taphonomical implications. We examined specimens from two localities in western France (Claix and Moragne) using propagation phase-contrast X-ray synchrotron microtomography. The cuticle and the inner tissues of leafy axes are preserved in three dimensions. Epidermis, hypodermis, palisade parenchyma, spongy parenchyma, transfusion tracheids, and most of tissues of the vascular cylinder are clearly discernible. The numerous resin ducts are sometimes filled by persisting resin. Additionally, surfaces of some leaves preserved drops and flows of resin. Depositional environmental context combined with histological features of G. reichenbachii suggest that this conifer was adapted to a range of marginal-littoral ecosystems including those open to the sea paleoenvironments and innermost ones influenced by strong continental inputs. Geinitzia reichenbachii was adapted to withstand intense sunlight, hot temperatures coupled with salty sea wind, and dry conditions. The frequent amber-bearing beds in the Cretaceous from western France with Geinitzia as a main component of the associated floras raises the possibility of a role for Geinitzia in the production of the "Charentese amber".

On the role of fibre bonds on the elasticity of low-density papers: a micro-mechanical approach

Fine prediction of the elastic properties of paper materials can now be obtained using sophisticated fibre scale numerical approaches. However, there is still a need, in particular for low-density papers, for simple and compact analytical models that enable the elastic properties of these papers to be estimated from the knowledge of various structural information about their fibres and their fibrous networks. For that purpose, we pursued the analysis carried out in Marulier et al. (Cellulose 22:1517–1539, 2015. https://doi.org/10.1007/s10570-015-0610-6) with low-density papers that were fabricated with planar random and orientated fibrous microstructures and different fibre contents. The fibrous microstructures of these papers were imaged using X-ray synchrotron microtomography. The corresponding 3D images revealed highly connected fibrous networks with small fibre bond areas. Furthermore, the evolutions of their Young’s moduli were non-linear and evolved as power-laws with the fibre content. Current analytical models of the literature do not capture these trends. In light of these experimental data, we developed a fibre network model for the in-plane elasticity of papers in which the main deformation mechanisms of the micromechanical model is the shear of the numerous fibre bonds and their vicinity, whereas the fibre parts far from these zones were considered as rigid bodies. The stiffness tensor of papers was then estimated both numerically using a discrete element code and analytically using additional assumptions. Both approaches nicely fit the experimental trends by adjusting a unique unknown micromechanical parameter, which is the shear stiffness of bonding zones. The estimate of this parameter is relevant in light of several recently reported experimental results.

Nondestructive Structural Investigation of Yttria-Stabilized Zirconia Fiber Insulation Tile by Synchrotron X-ray In-Line Phase-Contrast Microtomography

Zirconia (ZrO2) aerogels show excellent insulating performance and have been widely applied as a thermal protector in furnaces, nuclear reactors, and spacecraft. The nondestructive determination of their interior microstructure is significant for evaluating their mechanical and insulating performance. In this study, we performed nondestructive structural investigation of an yttria-stabilized ZrO2 fiber insulation tile using synchrotron X-ray in-line phase-contrast microtomography at a pixel resolution of 6.5 µm. Taking advantage of the edge enhancement of phase-contrast imaging, single yttria-stabilized ZrO2 fibers were clearly distinguished; furthermore, interior aggregates were nondestructively observed at this spatial resolution. This work demonstrates the advantages and potential of synchrotron X-ray microtomography for the structural analysis of porous ceramic materials. By combining higher-brilliance synchrotron radiation sources and CCD detectors with higher spatial and temporal resolutions, we anticipate that we can further understand the relationship between aerogel microstructure and function, especially under in-service conditions at high temperatures.

Lattice kinetic model of 3D flow characterization in core samples via synchrotron X-ray micro-tomography

Flow characterization using more accurate and robust numerical engine in the natural domains is a demanding subject in underground related surveys for an optimized performance. Primarily, we employed a more precise insight into constructing a proper three-dimensional rock model, the XCT. Representative samples were scanned with a synchrotron Micro-Tomography beamline. The reconstructed volumes were analyzed using iMorph and the fluid flow simulated by employing the novel Constant Speed Kinetic Lattice model (CSKM).In this approach, the 4D Fourier series have been employed to simulate 3D fluid flow taking into account thermodynamic consistency. Considering the recently proposed entropic model of Burg and Tsallis, the extended Boghosian distribution function model was substituted by the recently proposed 4D CSKM with Tsallis entropy, incorporating a new developed forcing term through modified Exact Difference Method (EDM). Compared earlier research, the results reveal more accuracy in making flow parameters consistent with the porous-media-related physical phenomena.

Synchrotron X-ray microtomography and multifractal analysis for the characterization of pore structure and distribution in softwood pellet biochar

Biochar pores in the micrometer range (1–100 µm) derive from cellular structures of the plant biomass subjected to pyrolysis or can be the result of mechanical processing, such as pelleting. In this study, synchrotron X-ray microtomography was used to investigate the internal pore structure of softwood pellet biochar produced by slow pyrolysis at 550 and 700 °C. The microtomographic data sets consisted of 2025 images of 2560 × 2560 voxels with a voxel side length of 0.87 µm. The three-dimensional reconstructions revealed that pelleting and pyrolysis significantly altered the pore structures of the wood feedstock, creating a network of connected pores between fragments that resembled the wood morphology. While higher pyrolysis temperature increased the specific surface area (as determined by BET nitrogen adsorption), it did not affect the total observed porosity. Multifractal analysis was applied to assess the characteristics of the frequency distribution of pores along each of the three dimensions of reconstructed images of five softwood pellet biochar samples. The resulting singularity and Rényi spectra (generalized dimensions) indicated that the distribution of porosity had monofractal scaling behavior, was homogeneous within the analyzed volumes and consistent between replicate samples. Moreover, the pore distributions were isotropic (direction-independent), which is in strong contrast with the anisotropic pore structure of wood. As pores at the scale analyzed in this study are relevant, for example, for the supply of plant accessible water and habitable space for microorganisms, our findings combined with the ability to reproduce biochar with such pore distribution offer substantial advantages in various biochar applications.

In situ quantification of crystallisation kinetics of plagioclase and clinopyroxene in basaltic magma: Implications for lava flow

Crystallisation is a complex process that significantly affects the rheology of magma, and thus the flow dynamics during a volcanic eruption. For example, the evolution of crystal fraction, size and shape has a strong impact on the surface crust formation of a lava flow, and accessing such information is essential for accurate modelling of lava flow dynamics. To investigate the role of crystallisation kinetics on lava flow behaviour, we performed real-time, in situ synchrotron X-ray microtomography, studying the influence of temperature-time paths on the nucleation and growth of clinopyroxene and plagioclase in an oxidised, nominally anhydrous basaltic magma. Crystallisation experiments were performed at atmospheric pressure in air and temperatures from 1250°C to 1100°C, using a bespoke high-temperature resistance furnace. Depending on the cooling regime (single step versus continuous), two different crystal phases (either clinopyroxene or plagioclase) were produced, and we quantified their growth from both global and individual 3D texture analyses. The textural evolution of charges suggests that suppression of crystal nucleation is due to changes in the melt composition with increasing undercooling and time. Using existing viscosity models, we inferred the effect of crystals on the viscosity evolution of our crystal-bearing samples to trace changes in rheological behaviour during lava emplacement. We observe that under continuous cooling, both the onsets of the pāhoehoe-‘a‘ā transition and of non-Newtonian behaviour occur within a shorter time frame. With varying both temperature and time, we also either reproduced or approached the clinopyroxene and plagioclase phenocryst abundances and compositions of the Etna lava used as starting material, demonstrating that real-time synchrotron X-ray tomography is an ideal approach to unravel the final solidification history of basaltic lavas. This imaging technology has indeed the potential to provide input into lava flow models and hence our ability to forecast volcanic hazards.

Influence of curing temperature on belite cement hydration: A comparative study with Portland cement

Belite cements (BCs) could be a more sustainable binder than Portland cements (PCs) but adequate knowledge of the hydration features has still to be built. In particular, the mild curing hydration temperature effects have been extensively studied for PCs but not for BCs. This research was triggered by a previous work reporting improved mechanical strengths of BCs at higher curing temperatures. Here, we report the hydration characteristics of a BC at 20, 40 and 60 °C and compared to those of a typical PC. We have corroborated previous findings and used a multi-technique approach including Rietveld phase analysis, thermal analysis, calorimetry, silicon MAS-NMR, mercury intrusion porosimetry and chiefly synchrotron X-ray microtomography, to thoroughly understand the different behavior. In a nutshell, the improved mechanical performances at mild curing temperatures for BCs are mainly due to a much larger belite degree of reaction, with lower porosity coarsening of belite cements also playing a role.

Four-dimensional imaging and free-energy analysis of sudden pore-filling events in wicking of yarns.

What are the mechanisms at play in the spontaneous imbibition dynamics in polyethylene terephthalate filament yarns at pore scale? Processes at pore scale such as waiting times between the filling of two neighboring pores, as observed in special irregular porous media, like yarns, may overrule the predicted behavior by well-known laws such as Washburn's law. While the imbibition physics are well known, classic models like Washburn's law cannot explain the dynamics observed for yarns. The stepwise dynamics is discussed in terms of the interplay of thermodynamic free energy and viscous dissipation. Time-resolved synchrotron x-ray microtomography documents water filling at pore scale. Spontaneous imbibition in yarns is characterized by a series of fast pore-filling events separated by long periods of low flux. Four-dimensional imaging allows the extraction of interface areas at the boundaries between water, air, and polymer and the calculation of free-energy evolution. It is found that the waiting periods correspond to quasistable water configurations of almost vanishing free-energy gradient. The distributions of pore filling event sizes and waiting times spread over several orders of magnitude, resulting in the pronounced stepwise uptake dynamics.

Poisson’s ratio of eTPU molded bead foams in compression via in situ synchrotron X-ray microtomography

In situ synchrotron X-ray microtomography was used to characterize the bulk deformation behavior by computing the Poisson’s ratio of expanded thermoplastic polyurethane (eTPU) molded bead foams used in footwear midsole during compression. Quantitative data on morphological characteristics were obtained using an iterative image processing workflow. Image correlation on the 4D datasets using DVC was performed to calculate the volumetric and axial strain to estimate the Poisson ratio. Strain maps from DVC showed the influence of variability in ligament thickness distribution on the global mechanical behavior exhibited which dominated the response seen in these bead foams. Finally, our results showed a strong correlation between Poisson ratio and distribution of ligament thickness in foams.

Fracture Shape and Orientation Contributions to P-Wave Velocity and Anisotropy of Alpine Fault Mylonites

P-wave anisotropy is significant in the mylonitic Alpine Fault shear zone. Mineral- and texture-induced anisotropy are dominant in these rocks but further complicated by the presence of fractures. Electron back-scattered diffraction and synchrotron X-ray microtomography (micro-CT) data are acquired on exhumed schist, protomylonite, mylonite, and ultramylonite samples to quantify mineral phases, crystal preferred orientations, microfractures, and porosity. The samples are composed of quartz, plagioclase, mica and accessory garnet, and contain 3–5% porosity. Based on the micro-CT data, the representative pore shape has an aspect ratio of 5:2:1. Two numerical models are compared to calculate the velocity of fractured rocks: a 2D wave propagation model, and a differential effective medium model (3D). The results from both models have comparable pore-free fast and slow velocities of 6.5 and 5.5 km/s, respectively. Introducing 5% fractures with 5:2:1 aspect ratio, oriented with the longest axes parallel to foliation decreases these velocities to 6.3 and 5.0 km/s, respectively. Adding both randomly oriented and foliation-parallel fractures hinders the anisotropy increase with fracture volume. The anisotropy becomes independent of porosity when 80% of fractures are randomly oriented. Modeled anisotropy in 2D and 3D are different for similar fracture aspect ratios, being 30 and 15%, respectively. This discrepancy is the result of the underlying assumptions and limitations. Our numerical results explain the effects that fracture orientations and shapes have on previously published field- and laboratory-based studies. Through this numerical study, we show how mica-dominated, pore-free P-wave anisotropy compares to that of fracture volume, shape and orientation for protolith and shear zone rocks of the Alpine Fault.

In-situ synchrotron X-ray tomography investigation of the imperfect smooth-shell cylinder structure

Lattice materials at micro scale with extraordinary stiffness and strength have demonstrated promising industrial application potentials in aerospace, transport, automotive, biomedical and other sections. However, the complex fabrication process at micro scale will inevitably induce stochastic geometric defects within as-fabricated lattice materials, thus quantitatively evaluation of the mechanical integrity of 3D-printed micro lattice structures becomes a critical important issue. In this paper, mechanical behavior of the micro Schwarz Primitive triply periodic minimal surfaces (P-TPMS) cylinder shell structures fabricated with projection micro-stereolithography (PμSL) 3D printing technique were investigated. Meanwhile, synchrotron X-Ray micro-tomography (SR-μCT) 3D imaging and interrupted in-situ compression experiment were employed for quantifying the effect of defects on the compression mechanical performances. It is found that the thickness along vertical direction was larger than along horizontal direction. Afterwards, three different types of finite element models were developed for understanding the effects of fabrication defects on the mechanical behavior characteristic. Simulation results demonstrated that the statistical model was more accurate and efficient when compared with the ideal model and real geometry reconstructed model. Finally, parametric study was also presented to gain insight into the role of thickness imperfections on the mechanical performance of the shell.