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Three independent analysis methods were developed to investigate the distribution of solid mass in foams analyzed by X-ray tomography with effective pixel sizes larger than the thickness of the solid network (sub-pixel conditions). Validation of the methods was achieved by a comparison with the results obtained employing high-resolution tomography for the same set of foams. The foams showed different solid mass distribution, which varied from being preferentially located on the edges, with a fraction of mass in the struts nearing 0.6, to materials in which the fraction of mass in the struts was low, under 0.15. In all cases, the accuracy of the proposed approaches was greater for materials with a higher fraction of mass in the struts. The method based on deconvolution of the attenuation probability density function yielded the closest results to the high-resolution characterizations. In contrast, analysis of the solid matrix thickness distribution after watershed segmentation, and binarization of high thickness regions (struts segmentation) required normalization through macroscopic measurements and revealed higher deviations with respect to the high-resolution results. However, segmentation-based methods allowed investigation of the heterogeneity of the fraction of mass in the struts along the sample.
Non-invasive 3D methods for imaging cementum increments using synchrotron radiation sources are one of the most promising new avenues for cementum research. This technique offers the opportunity to overcome the major caveats to traditional thin section imaging, and provides volumetric datasets of sub-micrometer resolution that can be investigated in new ways. Such studies can unlock the 3D structure of cementum increments, and 3D measures may allow for new inferences on the relationship between cementum growth and life history. However, as a new field of research, synchrotron X-ray imaging of cementum must ensure reproducibility by employing quantitative approaches to develop optimal experimental procedures and settings for imaging cementum in different samples. The quantitative parameter optimisation procedure we introduce in this chapter should form a crucial part of the imaging protocol that we present here, in which we outline the major steps in preparing for, performing and concluding a synchrotron imaging experiment, based on our own experience.
Precious ornaments from the Museum Royal Tombs of Sipán were analyzed by X-ray computed microtomography (microCT). The ornaments analyzed were golden earrings produced by the Moche culture that flourished along the north coast of present-day Peru between approximately 100 and 600 AD. Sipán, also known as Huava Rajada, is a mochica archaeological complex in the north of Peru. In particular, the spectacular jewelry, mainly composed of gold, silver, and copper alloys, gilded copper, and tumbaga, from the Museum “Royal Tombs of Sipán,” in Lambayeque, north of Peru, are some of the most sophisticated metalworking ever produced of pre-Columbian America. A portable microCT system consisting of a high-resolution flat panel detector and a mini X-ray tube were used for the structural analysis of these ornaments. The microCT images show parts of the internal structure, highlighting the manufacturing technique and gold sheets joining techniques of the Moche artisans. Furthermore, the advantage of using the portable microCT system for nondestructive testing is clear when the sample cannot be taken to the laboratory.
The mineral component (at least 95 wt. %) of dental enamel is hydroxyapatite (hydroxylapatite) with multiple substitutions. The biogenic origin of enamel is reflected in the unusual ribbon-like morphology of the crystals, which are extremely elongated in the c-axis direction, and their organized arrangement within the tissue. The study of enamel dissolution has been driven by the very high prevalence of dental caries. In enamel caries, the initial demineralization results in subsurface dissolution of mineral. While the surface remains intact, reversal of the lesion by remineralization is possible. Problems of understanding the physico-chemical processes in enamel demineralization include the general problems concerning the structure and chemistry of apatites formed in aqueous media. Added to these are the general problem of dissolution in an inhomogeneous porous medium and the complication that enamel apatite has a naturally variable composition which changes during demineralization. The use of model systems in caries research is illustrated by reference to X-ray absorption studies of enamel and synthetic analogues.
Ti6Al4V alloy samples with large pores suitable for bone implants are fabricated by pressing and sintering. Ti6Al4V powder is mixed with different volume fractions of salt particles. The sintering behavior up to 1260 °C is studied by dilatometry and pore features are observed by scanning electron microscopy and X-ray microtomography. Sintered materials with a relative density between 0.26 and 0.97 are obtained. 3D image analysis proves that large pores form a connected network when the amount of salt is 20% and above. The Young’s modulus and the yield stress of sintered materials deduced from compression tests span over wide ranges of values, which are consistent with real bone data. A simple analytical model is proposed to estimate the relative density as a function of the fraction of salt. This model combined with classical Gibson and Ashby’s power equations for mechanical properties can predict the fraction of salt required to obtain prescribed properties.
A multiscale approach combining phase-contrast X-ray micro- and nanotomography is applied for imaging a Cretaceous fossil inflorescence in the resolution range from 0.75 μm to 50 nm. The wide range of scale views provides three-dimensional reconstructions from the external gross morphology of the inflorescence fragment to the finest exine sculptures of in situ pollen. This approach enables most of the characteristics usually observed under light microscopy, or with low magnification under scanning and transmission electron microscopy, to be obtained nondestructively. In contrast to previous tomography studies of fossil and extant flowers that used resolutions down to the micron range, we used voxels with a 50 nm side in local tomography scans. This high level of resolution enables systematic affinities of fossil flowers to be established without breaking or slicing specimens.
This article presents a detailed study of the microstructure of Iberian expanded clay lightweight aggregates (LWA). Other than more commonly used mercury porosimetry (MP) and water absorption methods, the experimental study involves optical microscopy, scanning electron microscopy (SEM), and microtomography (μ-CT). Pore connectivity and how it is deployed are shown to some degree, and the pore size spectrum is estimated. LWA are in general characterized by a dense outer shell up to 200 μm thick, encasing an inner cellular structure of 10–100 times bigger pore size. Aggregate pore sizes may span from some hundreds of nanometers up to over 1 mm, though the range of 1–25 μm is more typical. A noteworthy fraction of these pores is closed, and they are mainly up to 1 μm. It is also shown that macropore spatial arrangement is affected by the manufacturing process. A step forward is given to understanding how the outer shell and the inner pore network influence the mechanical and physical LWA properties, particularly the density and water absorption. The joint consideration of μ-CT and SEM seems to be the most appropriate methodology to study LWA microstructure. MP analysis is likely to distort LWA pore spectrum assessment.
Due to the extraordinary beam characteristics of the new PETRA III synchrotron, i.e., the high brilliance, the extremely low emittance of 1 nm rad, and the high fraction of coherent photons even in the hard X-ray range, the imaging beamline (IBL) at PETRA III will provide state of the art imaging and tomography capabilities with resolution well into the nanometer range. Novel applications of tomographic techniques allow for high speed in situ measurements as well as highest spatial and density resolutions. Additionally, the highly coherent beam enables the application of phase contrast methods in an exceptional way. Since the focus is on the energy range between 5 and 50 keV, the IBL will among others be ideally suited for microtomography and nanotomography on small engineering materials science samples as well as for studying soft matter, bones, medical implants, and biomatter.
Fossil embryos are paramount for our understanding of the development of extinct species. However, although thousands of fossil amniote eggs are known, very few embryos in ovo have been described. First reports of fossil embryos were based on broken eggs, where the embryonic remains were already exposed, because destructive methods on complete eggs were avoided. Investigations of complete eggs therefore required nondestructive approaches, such as X-ray microtomography (μCT). However, due to the general low density contrast between fossilized bones and infilling matrix, only a few specimens have been reported using these techniques. Using propagation phase contrast X-ray synchrotron microtomography (PPC-SR-μCT), we report here the discovery of three well-preserved embryos in Early Cretaceous eggs from Thailand. By scanning these eggs using different imaging techniques, we show that vastly different interpretations can be made regarding the preservation state and/or the developmental stage of these embryos. PPC-SR-μCT also revealed differential contrast between bone categories, presumably reflecting the ossification pattern of these embryos. Applying such an approach to large-scale studies of fossil eggs could lead to more discoveries and detailed studies of fossil embryos, providing important developmental and phylogenetic information on extinct and extant amniotes.
La méthodologie proposée pour l’étude du comportement de matériaux cellulaires soussollicitation dynamique est abordée par une approche multi-échelles. Le comportement desmousses polymères étudiées dépend du matériau constitutif, et de sa structure poreuse. Lesmatériaux cellulaires de l’étude sont constitués de grains millimétriques poreux; le cœurde ces grains est constitué de cellules microscopiques. La méthodologie proposée vise àreproduire la morphologie multi-échelles du matériau cellulaire, celles des grains et descellules, d’implémenter des modèles de comportement simples à ces différentes échellesafin de reproduire les phénomènes physiques complexes observés et la réponse macroscopiquedu matériau. L’observation et l’analyse des phénomènes locaux est un travail préparatoireà la modélisation multi-échelles. Cet article décrit les méthodes expérimentales etnumériques qui ont été développées pour l’observation fine de la structure des matériauxcellulaires, et quantifier des déformations et des dommages de ces structures à l’échelledes cellules et des grains. Deux approches de modélisation ont été ensuite envisagées; unmodèle éléments-finis pour décrire la structure des grains, et une autre approchenumérique plus originale qui s’appuie sur la méthode des éléments discrets pourreprésenter la structure microscopique des cellules.
Tannin-based rigid foams of different bulk densities and their carbonized counterparts were investigated for the first time by X-ray microtomography. This method allowed acquisition of three-dimensional pictures of such highly porous materials. Through mathematical treatment of the images, extremely useful physical characteristics such as porosity, fraction of open cells, connectivity, tortuosity, and pore-size distribution were determined as a function of the foam's density. The obtained information was compared with independent data derived from pycnometry measurements and scanning electron microscope image analysis. The agreement was shown to be acceptable in the limit of the accuracy of the laboratory microtomograph (4 μm). Moreover, recalculating properties like permeability were shown to be quite possible based on the results of standard microtomography data.
Cold gas dynamic spray (cold spray) is a rapid deposition technology in which particles deposit at velocities above the speed of sound (∼340 ms−1). Generally, porosity forms in cold spray deposits due to insufficient deformation of particles. In this study, the unique capability of the X-ray microscopy and microtomography is utilized to visualize the internal structure of deposited material. The results show that this characterization technique successfully reveals porosities in the cold spray commercial purity (CP) titanium structure. Furthermore, microtomography images confirmed the experimental results for porosity measurements in which helium (compared with nitrogen) as carrier gas significantly decreases porosity in cold spray CP titanium.
A significant portion of Mesozoic amber is fully opaque. Biological inclusions in such amber are invisible even after polishing, leading to potential bias in paleoecological and phylogenetic studies. Until now, studies using conventional X-ray microtomography focused on translucent or semi-opaque amber. In these cases, organisms of interest were visualized prior to X-ray analyses. It was recently demonstrated that propagation phase contrast X-ray synchrotron imaging techniques are powerful tools to access invisible inclusions in fully opaque amber. Here we describe an optimized synchrotron microradiographic protocol that allowed us to investigate efficiently and rapidly large amounts of opaque amber pieces from Charentes (southwestern France). Amber pieces were imaged with microradiography after immersion in water, which optimizes the visibility of inclusions. Determination is not accurate enough to allow precise phylogenetic studies, but provides preliminary data on biodiversity and ecotypes distribution; phase contrast microtomography remains necessary for precise determination. Because the organisms are generally much smaller than the amber pieces, we optimized local microtomography by using a continuous acquisition mode (sample moving during projection integration). As tomographic investigation of all inclusions is not practical, we suggest the use of a synchrotron for a microradiographic survey of opaque amber, coupled with microtomographic investigations of the most valuable organisms.
Cone-beam X-ray microtomography attracts increasing attention due to its applications in biomedical sciences, material engineering, and industrial nondestructive evaluation. Rapid volumetric image reconstruction is highly desirable in all these areas for prompt visualization and analysis of complex structures of interest. In this article, we reformulate a generalized Feldkamp cone-beam image reconstruction algorithm, utilize curved voxels and mapping tables, improve the reconstruction efficiency by an order of magnitude relative to a direct implementation of the standard algorithm, and demonstrate the feasibility with numerical simulation and experiments using a prototype cone-beam X-ray microtomographic system. Our fast algorithm reconstructs a 256-voxel cube from 100 projections within 2 min on an Intel Pentium II® 233 MHz personal computer, produces satisfactory image quality, and can be further accelerated using special hardware and/or parallel processing techniques.
A laboratory test of X-ray tomography employing a diverging beam of
X-rays rather than the usual parallel X-ray beam is described. We chose to
test and demonstrate the advantages of divergent beam tomography by
imaging an extracted juvenile human premolar using an ordinary dental
X-ray source and a cooled CCD camera. Experiments with a three-piece
cover-glass sample and with the human tooth demonstrated that
three-dimensional reconstruction can be achieved at 34 μm per pixel
resolution employing an X-ray tube spot 800 μm in its smallest
direction without requiring close contact with the fluorescent screen.
Reconstruction of a 256 x 256 pixel single-plane image from 100 projection
images took only 45 sec on a personal computer with a Pentium 166 MHz
processor. We have also demonstrated a volume reconstruction of 256 x 256
x 256 voxels from the data. Successful extension of this work to
submicrometer projection X-ray microscopy is predicted. Improved
resolution of medical tomography is another possible application.
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