Gaps at the interface between dentine and self-adhesive resin cement in post-endodontic restorations quantified in 3D by phase contrast-enhanced micro-CT.

AIM: To assess the extent of gaps between root dentine and titanium or fibreglass post restorations following cementation with a self-adhesive resin cement. METHODOLOGY: Fourteen root filled maxillary central incisors restored with prefabricated posts made of Fibreglass (n = 7) or Titanium (n = 7) and cemented with RelyX Unicem 2 were imaged by rapid, high-resolution phase contrast-enhanced micro-CT (PCE-CT) in a synchrotron X-ray imaging facility (ID19, ESRF, 34 KeV, 0.65 µm pixel resolution). Reconstructions were used to measure canal, cement and post perimeters and cross-sectional areas and interfacial gaps at 0.1 mm increments in the root canal space, along the cervical region of the tooth. Remnants of endodontic sealer (AH Plus), when present, were also quantified. Mann-Whitney and 2-way ANOVA tests were used to compare findings within slices and between the two post groups. Pearson correlation coefficients (r) were determined between the interfacial gaps and the other measured parameters. RESULTS: Clearly detectable gaps were found in 45% (±14%) of the interfaces between dentine and cement, along the canal in the cervical area of the tooth beneath the core. The length of interfacial gaps was moderately correlated to the canal cross-sectional area, to the canal perimeter and to the canal area filled by cement (R = 0.52 ~ 0.55, P < 0.001). There was no significant difference between samples with fibreglass or titanium (P > 0.01). Both post types had defect-free interfaces with cement. Endodontic sealer remnants were found on ~10% of the canal walls and were moderately correlated to the presence of gaps. Approximately 30% of the sealer-affected interfaces exhibited no detachment between dentine, sealer and cement. CONCLUSIONS: Self-adhesive cements had interfacial gaps along substantial regions of the root canal surface, which was not correlated with the amount of cement in the canal. PCE-CT proved to be an excellent non-destructive method to study root canal restorations of hydrated samples in 3D.

Estimation of filler macro-dispersion in rubber matrix by radiometric stereo microscopy.

A new microscopic principle based on radiometric stereo microscopy is presented, which is designed for investigating macro-dispersion of filler in rubber. The image acquisition is combined with a stereological method of estimating the volume-weighted size distribution of the filler particles. Experimental results for carbon black filler in rubber obtained by radiometric stereo microscopy are compared with those from microtomography using synchrotron radiation, and, furthermore, a simulation study is used for evaluation. It turns out that using the new three-dimensional microscopic method, the size distribution of the filler particles can be estimated from fresh cuts of rubber with high accuracy, and thus it is an interesting alternative to well-established dark field microscopy. LAY DESCRIPTION: Macro-dispersion of globular filler particles in a rubber matrix is an important quantity that depends on manufacturing parameters and influences various rubber properties. Therefore, it must be carefully adjusted during the incorporation process and investigated by industrial quality control (ASTM D7723-18). Quality control is usually based on freshly made planar sections so-called fresh cuts through rubber specimen. After stress retention of the rubber one obtains a rough cutting surface in which the filler particles appear as imprints or bumps, called nodges. These nodges can be made visible by classical light microscopy under dark field (DFM) illumination. The systems disperGRADER+ or the disperGRADER Alpha View were specifically designed for rubber inspection. However, it has proved to be very difficult estimating the size distribution of the filler particles from the observed white spots in the DFM image. In any case it is still necessary to compute the size distribution of the filler particles from an estimated size distribution of the section profiles. The latter is numerically unstable, i.e. small errors of the estimated size distribution of the section profiles lead to large errors of the computed filler size distribution. Applying DFM combined with filler dispersion estimation as described in ASTM D7723-18 appears to be a fingerprint method only. For this reason, the new microscope nSPEC 3D was applied for rubber inspection. The principle used for surface imaging is based on radiometric stereo allowing for perfect three-dimensional reconstruction of curved surfaces of fresh cuts. From this reconstruction it is possible to measure the height of particle nodges as well as their volumes. Furthermore, we present a new stereological method for estimating the filler size distribution from samples of the height and the volume of the nodges. Finally, microtomography with synchrotron radiation and computer simulation are applied to evaluate accuracy of the presented method.

Growth of second stage mineral in Lytechinus variegatus.

Purpose and Aims: Sea urchin teeth consist of calcite and form in two stages with different magnesium contents. The first stage structures of independently formed plates and needle-prisms define the shape of the tooth, and the columns of the second stage mineral cements the first stage structures together and control the fracture behavior of the mature tooth. This study investigates the nucleation and growth of the second stage mineral. MATERIALS AND METHODS: Scanning electron microscopy (SEM) and synchrotron microComputed Tomography characterized the structures of the second phase material found in developing of Lytechinus variegatus teeth. RESULTS: Although the column development is a continuous process, defining four phases of column formation captures the changes that occur in teeth of L. variegatus. The earliest phase consists of small 1-2 µm diameter hemispheres, and the second of 5-10 µm diameter, mound-like structures with a nodular surface, develops from the hemispheres. The mounds eventually bridge the syncytium between adjacent plates and form hyperboloid structures (phase three) that appear like mesas when plates separate during the fracture. The mesa diameter increases with time until the column diameter is significantly larger than its height, defining the fourth phase of column development. Energy dispersive x-ray spectroscopy confirms that the columns contain more magnesium than the underlying plates; the ratios of magnesium to calcium are consistent with compositions derived from x-ray diffraction. CONCLUSION: Columns grow from both bounding plates. The presence of first phase columns interspersed among third stage mesas indicates very localized control of mineralization.

Torsion estimation of particle paths through porous media observed by in-situ time-resolved microtomography.

The torsion distribution of cell paths in two-phase flow of a cell suspension through a porous medium is an important quantity for chromatographic processes. It can be estimated from cell tracking in sequences of three-dimensional images of a suspension pumped through the medium, where the images are acquired by in-situ time-resolved microtomography using synchrotron radiation and inline phase contrast modus. This contribution presents a new method for estimating path torsion from discrete positions, where the estimation is based on an appropriate discretization of the differential-geometric formula of the torsion of a space curve. Investigations performed for an alcoholic suspension of silica gel particles pumped through a partially open polyurethane foam show that the shape of the inner surface of the foam has a considerable impact on the particle paths. It turns out that the variance of the torsion for slow particle moving close to the surface is a half order of magnitude smaller than that of fast particles, which underlines the importance of torsion for filter efficiency.

Inflammatory pseudotumor (IPT)-surgical cure of an inflammatory syndrome.

UNLABELLED: We report on four female adolescents, who presented with inflammatory symptoms. Extensive diagnostic workup revealed tumors on different locations. After surgical removal, clinical and laboratory signs of inflammation disappeared rapidly. On histology, the tumors showed a mixture of inflammatory cells characteristic of inflammatory pseudotumors in three of the patients. CONCLUSION: In patients with unclear inflammatory symptoms, inflammatory pseudotumor should be added to the differential diagnosis. WHAT IS KNOWN: • The inflammatory pseudotumor (IPT) is a mostly benign myofibroblastic tumor of the soft tissue and causes inflammatory symptoms. What is new: • IPTs have may wider than hitherto defined histologic features. Removal of IPT is curative.

Trimodal low-dose X-ray tomography.

X-ray grating interferometry is a coherent imaging technique that bears tremendous potential for three-dimensional tomographic imaging of soft biological tissue and other specimens whose details exhibit very weak absorption contrast. It is intrinsically trimodal, delivering phase contrast, absorption contrast, and scattering ("dark-field") contrast. Recently reported acquisition strategies for grating-interferometric phase tomography constitute a major improvement of dose efficiency and speed. In particular, some of these techniques eliminate the need for scanning of one of the gratings ("phase stepping"). This advantage, however, comes at the cost of other limitations. These can be a loss in spatial resolution, or the inability to fully separate the three imaging modalities. In the present paper we report a data acquisition and processing method that optimizes dose efficiency but does not share the main limitations of other recently reported methods. Although our method still relies on phase stepping, it effectively uses only down to a single detector frame per projection angle and yields images corresponding to all three contrast modalities. In particular, this means that dark-field imaging remains accessible. The method is also compliant with data acquisition over an angular range of only 180° and with a continuous rotation of the specimen.

Exploiting coherence for real-time studies by single-bunch imaging.

First real-time studies of ultra-fast processes by single-bunch imaging at the European Synchrotron Radiation Facility are reported. By operating the storage ring of the ESRF in single-bunch mode with its correspondingly increased electron bunch charge density per singlet, the polychromatic photon flux density at insertion-device beamlines is sufficient to capture hard X-ray images exploiting the light from a single bunch (the corresponding bunch length is 140 ps FWHM). Hard X-ray imaging with absorption contrast as well as phase contrast in combination with large propagation distances is demonstrated using spatial samplings of 11 µm and 35 µm pixel size. The images acquired allow one to track crack propagation in a bursting piece of glass, breaking of an electrical fuse as well as cell wall rupture in an aqueous foam. Future developments and their potential in the frame of the proposed Phase II of the ESRF Upgrade Program are discussed.

The rupture of a single liquid aluminium alloy film.

The present study is based on the idea of understanding the rupture of films in metal foams by studying free standing metallic films as a model system. Liquid dynamics, the velocity of the rupturing material as well as the behaviour of ceramic particles inside the melt were analysed optically ex situ and by synchrotron X-ray radiography in situ. It was found that the resistance of films to rupture is mainly based on the interaction between solid particles and an immobile oxide skin, the formation of which depends on the oxygen content of the surrounding atmosphere and the presence of magnesium.

ANKAphase: software for single-distance phase retrieval from inline X-ray phase-contrast radiographs.

A computer program named ANKAphase is presented that processes X-ray inline phase-contrast radiographs by reconstructing the projected thickness of the object(s) imaged. The program uses a single-distance non-iterative phase-retrieval algorithm described by David Paganin et al. [(2002), J. Microsc. 206, 33-40]. Allowing for non-negligible absorption in the sample, this method is strictly valid only for monochromatic illumination and single-material objects but tolerates deviations from these conditions, especially polychromaticity. ANKAphase is designed to be applied to tomography data (although it does not perform tomographic reconstruction itself). It can process series of images and perform flat-field and dark-field correction. Written in Java, ANKAphase has an intuitive graphical user interface and can be run either as a stand-alone application or as a plugin to ImageJ, a widely used scientific image-processing program. A description of ANKAphase is given and example applications are shown.

Identification of root filling interfaces by microscopy and tomography methods.

AIM: To assess differences in observed cross-sectional areas of root canals and filling materials, as imaged by three microscopy and two tomography methods. METHODOLOGY: Six roots filled with laterally compacted Gutta-percha and AH26 were scanned with phase-contrast enhanced microtomography in a synchrotron facility. Reconstructed virtual slices were compared with sections of both wet and acrylic-embedded roots, evaluated also by light and electron microscopy (EM) and laboratory-based microtomography (µCT). The different contrasts of Gutta-percha, voids, sealer and root dentine were identified and correlated. Inner canal border, outer Gutta-percha rim and the external margin of a void were manually delineated, and the enclosed areas were repeatedly measured by three observers. Interobserver and interimaging method differences were tested by 2-way anova with Bonferroni adjustments (P < 0.05). Percentages of Gutta-percha-filled canal areas (PGP) were determined. RESULTS: Phase-contrast enhanced microtomography revealed internal interfaces and detailed 3D volumes of accentuated voids as well as micrometre-sized particles and gaps within the treated roots. Overestimates in the cross-sectional areas were obtained by light microscopy, whereas underestimates were obtained by µCT and EM. Differences exceeded 40%; however, PGP values by all methods were within 5% for the same slice. Differences between observers were sometimes significant, but they were not method related (<3%). CONCLUSIONS: Phase-contrast enhanced microtomography is a powerful non-destructive ex vivo investigation method for studying the interfaces within root canals and filling materials at a micrometre resolution. The method does not require damage-prone sectioning/polishing during sample preparation procedures. Caution should be used when quantifying the extent of Gutta-percha in root fillings by measurements using µCT, light and EM.

Machine learning applied to X-ray tomography as a new tool to analyze the voids in RRP Nb3Sn wires.

The electro-mechanical and electro-thermal properties of high-performance Restacked-Rod-Process (RRP) Nb3Sn wires are key factors in the realization of compact magnets above 15 T for the future particle physics experiments. Combining X-ray micro-tomography with unsupervised machine learning algorithm, we provide a new tool capable to study the internal features of RRP wires and unlock different approaches to enhance their performances. Such tool is ideal to characterize the distribution and morphology of the voids that are generated during the heat treatment necessary to form the Nb3Sn superconducting phase. Two different types of voids can be detected in this type of wires: one inside the copper matrix and the other inside the Nb3Sn sub-elements. The former type can be related to Sn leaking from sub-elements to the copper matrix which leads to poor electro-thermal stability of the whole wire. The second type is detrimental for the electro-mechanical performance of the wires as superconducting wires experience large electromagnetic stresses in high field and high current conditions. We analyze these aspects thoroughly and discuss the potential of the X-ray tomography analysis tool to help modeling and predicting electro-mechanical and electro-thermal behavior of RRP wires and optimize their design.

In vitro synchrotron-based radiography of micro-gap formation at the implant-abutment interface of two-piece dental implants.

Micro-gap formation at the implant-abutment interface of two-piece dental implants was investigated in vitro using high-resolution radiography in combination with hard X-ray synchrotron radiation. Images were taken with the specimen under different mechanical loads of up to 100 N. The aim of this investigation was to prove the existence of micro-gaps for implants with conical connections as well as to study the mechanical behavior of the mating zone of conical implants during loading. Synchrotron-based radiography in comparison with classical laboratory radiography yields high spatial resolution in combination with high contrast even when exploiting micro-sized features in highly attenuating objects. The first illustration of a micro-gap which was previously indistinguishable by laboratory methods underlines that the complex micro-mechanical behavior of implants requires further in vitro investigations where synchrotron-based micro-imaging is one of the prerequisites.

Comparative study of multilayers used in monochromators for synchrotron-based coherent hard X-ray imaging.

A systematic study is presented in which multilayers of different composition (W/Si, Mo/Si, Pd/B(4)C), periodicity (from 2.5 to 5.5 nm) and number of layers have been characterized. In particular, the intrinsic quality (roughness and reflectivity) as well as the performance (homogeneity and coherence of the outgoing beam) as a monochromator for synchrotron radiation hard X-ray micro-imaging are investigated. The results indicate that the material composition is the dominating factor for the performance. By helping scientists and engineers specify the design parameters of multilayer monochromators, these results can contribute to a better exploitation of the advantages of multilayer monochromators over crystal-based devices; i.e. larger spectral bandwidth and high photon flux density, which are particularly useful for synchrotron-based micro-radiography and -tomography.

X-ray diffraction microtomography (XRD-CT), a novel tool for non-invasive mapping of phase development in cement materials.

A recently developed synchrotron-based imaging technique, X-ray diffraction microtomography (XRD-CT), has been applied here for the first time to a complex system, the hydrating Portland cement paste, in order to monitor the evolution of microstructure and phase formation with a 3D non-invasive imaging approach. The ettringite-XRD-peak-based image reconstructions, combined with transmission microtomography (X-microCT) images, allowed to assess the ubiquitous distribution of this phase, which appears early in the hydration process and showed its preferential concentration in the relatively less compact regions of the paste. The comparison of greyscale histograms for cement pastes after 9 and 58 h from hydration showed an increase of ettringite content with age, in agreement with the quantitative Rietveld analysis of the sum patterns. By renormalizing the greyscale histograms to the relative weight fraction, as obtained from Rietveld refinements, a new technique which allows estimation of phase contents with spatial resolution has been developed. The results achievable by combining XRD-CT, X-microCT and Rietveld appear very promising to provide experimental snapshots of the cement hydration process to be compared with results obtained from computer simulations.

On the possibilities of hard X-ray imaging with high spatio-temporal resolution using polychromatic synchrotron radiation.

Time-resolved imaging with penetrating radiation has an outstanding scientific value but its realisation requires a high density of photons as well as corresponding fast X-ray image detection schemes. Bending magnets and insertion devices of third generation synchrotron light sources offer a polychromatic photon flux density which is high enough to perform hard X-ray imaging with a spatio-temporal resolution up to the µm-µs range. Existing indirect X-ray image detectors commonly used at synchrotron light sources can be adapted for fast image acquisition by employing CMOS-based digital high speed cameras already available on the market. Selected applications from life sciences and materials research underline the high potential of this high-speed hard X-ray microimaging approach.

Impact failure in two silicates revealed by ultrafast, in situ, synchrotron X-ray microscopy.

To travel safely behind screens that can protect us from stones and hail, we must understand the response of glass to impact. However, without a means to observe the mechanisms that fail different silicate architectures, engineering has relied on external sensors, post-impact examination and best-guess to glaze our vehicles. We have used single and multi-bunch, X-ray imaging to differentiate distinct phases of failure in two silicates. We identified distinct micromechanisms, operating in tandem and leading to failure in borosilicate glass and Z-cut quartz. A surface zone in the amorphous glass densifies before bulk fracture occurs and then fails the block, whilst in quartz, fast cracks, driven down cleavage planes, fails the bulk. Varying the rate at which ejecta escapes by using different indenter tip geometries controls the failed target's bulk strength. This opens the way to more physically based constitutive descriptions for the glasses allowing design of safer, composite panels by controlling the impulses felt by protective screens.

Collapse dynamics of spherical cavities in a solid under shock loading.

Extraordinary states of highly localised pressure and temperature can be generated upon the collapse of impulsively driven cavities. Direct observation of this phenomenon in solids has proved challenging, but recent advances in high-speed synchrotron radiography now permit the study of highly transient, subsurface events in real time. We present a study on the shock-induced collapse of spherical cavities in a solid polymethyl methacrylate medium, driven to shock states between 0.49 and 16.60 GPa. Utilising multi-MHz phase contrast radiography, extended sequences of the collapse process have been captured, revealing new details of interface motion, material failure and jet instability formation. Results reveal a rich array of collapse characteristics dominated by strength effects at low shock pressures and leading to a hydrodynamic response at the highest loading conditions.

Synchrotron-based radioscopy employing spatio-temporal micro-resolution for studying fast phenomena in liquid metal foams.

Investigations of pore coalescence and individual cell wall collapse in an expanding liquid metal foam by means of X-ray radioscopy with spatio-temporal micro-resolution are reported. By using white synchrotron radiation for imaging, the rupture of a film and the subsequent merger of two neighbouring bubbles could be recorded with a time sampling rate of 40000 frames s(-1) (25 micros exposure time) and a spatial sampling rate of 20 microm. The rupture time of a cell wall was found to be in the range of 300 micros. This value is in agreement with theoretical considerations which assume an inertia-dominated rupture time of cell walls in liquid metal foams.

Use of synchrotron-based radiography to diagnose pulsed power driven wire explosion experiments.

We describe the first use of synchrotron radiation to probe pulsed power driven high energy density physics experiments. Multi-frame x-ray radiography with interframe spacing of 704 ns and temporal resolution of <100 ps was used to diagnose the electrical explosion of different wire configurations in water including single copper and tungsten wires, parallel copper wire pairs, and copper x-pinches. Such experiments are of great interest to a variety of areas including equation of state studies and high pressure materials research, but the optical diagnostics that are usually employed in these experiments are unable to probe the areas behind the shock wave generated in the water, as well as the internal structure of the exploding material. The x-ray radiography presented here, performed at beamline ID19 at European Synchrotron Radiation Facility (ESRF), was able to image both sides of the shock to a resolution of up to 8 µm, and phase contrast imaging allowed fine details of the wire structure during the current driven explosion and the shock waves to be clearly observed. These results demonstrate the feasibility of pulsed power operated in conjunction with synchrotron facilities, as well as an effective technique in the study of shock waves and wire explosion dynamics.

Analysis of spatial cross-correlations in multi-constituent volume data.

We investigate spatial cross-correlations between two constituents, both belonging to the same microstructure. These investigations are based on two approaches: one via the measurement of the cross-correlation function and the other uses the spatial distances between the constituents. The cross-correlation function can be measured using the fast Fourier transform, whereas the distances are determined via the Euclidean distance transform. The characteristics are derived from volume images obtained by synchrotron microtomography. As an example we consider pore formation in metallic foams, knowledge of which is important to control the foam production process. For this example, we discuss the spatial cross-correlation between the pore space and the blowing agent particles in detail.