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The fabric of mineral liner materials that had been exposed to organic compounds over a 12-year period was investigated as part of a wider research project. Macromorphological and micromorphological changes in the fabric were identified using computed tomography and polarisation microscopy.
Special care was taken to ensure artefact free sampling and sample preparation, in particular, the drying method used, has a substantial influence on the quality of the thin sections.
Fabric changes due to contaminant permeation over several years are, by and large, relatively small and their intensity is material specific. Silty clay CML1, in particular, contains a somewhat greater number of fissures and voids in comparison with the original material. The superposition of various processes in both test procedures and sample preparation may lead to fabric changes which can impede interpretation of the results.
In this paper the characterisation of functionally graded materials is elucidated by several different methods. These methods described here are used for the quantitative analysis of materials with a local dependence of microstructure parameters. Using X-ray microscopy (computed tomography) for 3D-measurements and optical microscopy on polished sections for 1D and 2D measurements on the same sample, a ceramic filter consisting of sintered spherical particles, various mathematical evaluation methods are described and compared.
Micro-computed tomography (µCT) provides quantitative three-dimensional information of bone around titanium implants similar to classical histology. The study, based on an animal model, using cuboid-shaped biofunctionalised Ti6Al4V implants with surrounding bone after 4 weeks, is performed using 3 µCT-systems with X-ray tubes, one synchrotron-radiation-based µCT-system (SRµCT), and classical histology. Although the spatial resolution of the µCTsystems is comparable, only the results of SRµCT agree with results of classical histology. The X-ray tube sources give rise to huge artefacts in the tomograms (interface scattering, beam hardening), which impaired the quantitative analysis of bone up to about 200 µm from the implant surface. Due to the non-destructive character of µCT the specimens can be subsequently examined by classical histology
without restriction. The quantitative comparison of bone formation uncovers the strong dependence of the detected amount of newly formed bone from the selected slice. This
implies the necessity of 3D analysis. SRµCT and classical histology prove that surface modifications of the titanium implant significantly influence the bone formation. Using SRµCT, the preparation artefacts due to cutting and polishing are excluded.
Rock porosity determination by combination of X-ray computerized tomography with mercury porosimetry
(1997)
Abstract First results are described of coupling of mercury porosimetry with X-ray computerized tomography (CT) as a new combination technique for rock porosity studies. This technique is suitable for rock samples with a pronounced mercury intrusion-extrusion hysteresis and includes CT measurements before and after mercury intrusion. The entrapped portion of mercury, when the pressure after the intrusion into the rock sample is reduced to 0.1 MPa, serves as a contrast agent in the porous network to localize spatial distribution of rock porosity by CT. The results obtained show that the mercury intrusion and therefore the porosity were quite different for the separate mineral phases. Therefore the combination of mercury porosimetry and computer tomography can give 3-D data on mineral-specific porosity distributions with additional pore size information. In contrast to mercury porosimetry as a single method, results of the combination technique with CT represent a direct visualization of porosity variation and do not depend on any special pore network model.
The application of two sets of methods for the characterization of rock pore systems is reported. Both are discussed in the context of other techniques described in the literature. (i) Impregnation with labelled polymethylmethacrylate (PMMA) and autoradiography or direct measurement of the tracer activity allows the investigation of the pattern of the spatial porosity distribution and quantitative measurement of mineral-specific, local porosities, porosity gradients as well as an assessment of hydraulic and diffusive transport properties. (ii) Quantitative information on surface areas within certain pore size ranges can be achieved by combination of mercury intrusion porosimetry with X-ray absorption computertomography. As examples of applications of these techniques, the effects of weathering, alteration, mechanical stress and large diameter coring on the pore network of rocks have been studied.
Archaeological bone, ivory and antler, as well as objects manufactured from them, are largely studied to extract as much information as possible from these materials. Among others, one key question in archaeology is the exact identification of the material. Even if the identification of different kinds of osseous material seems to be trivial in many cases, it can be a difficult issue when small, heavily carved and more or less altered ancient objects are concerned. This study was focused on the determination of parameters allowing the distinction of archaeological ivory, bone and antler in order to identify the raw material used for the manufacture of prehistoric objects. The high performance of synchrotron radiation (SR) and laboratory-based micro X-ray computed tomography (microCT), providing highly resolved three-dimensional information on the micromorphology, permitted the establishment of such distinctive features of modern references of ivory, antler, land mammal and whale bones: ivory shows characteristic tubular pores with a diameter of about 1 to 2 µm, bone and antler show typical osteon structures. In our measured references, antler shows on average larger and more elongated shaped pores of the osteons compared to terrestrial mammal bone. This feature however depends very much on the original localization of the studied sample within the antler. Whale bones can be distinguished from the other osseous materials by a cancellous, osteoporotic-like structure with irregularly distributed rounded porosities with diameters reaching up to 500 µm. These characteristics have also been tested on determined Palaeolithic fragments, as diagenetic changes during burial have to be considered and may lead to the modification of the parameters established on the basis of modern bone references. In general, the chemical composition of bone objects can change drastically over time while micromorphological features, as evidenced by microCT, seem to be less susceptible to such alterations. In addition, microCT enables the comparison of inner and possibly less altered parts of the objects, and can be considered as completely non-destructive for small mineralised prehistoric objects. In this study, specific morphological features allowing the distinction of ivory and of whale bone from other bone and antler material were determined, even for altered materials dating back to Palaeolithic periods. Thus, we provide, in addition to archaeozoological, chemical and isotopic markers, a new non-destructive tool to identify some raw materials used for the fabrication of osseous objects ranging from recent to prehistoric periods.
Die Struktur eines Materials bestimmt wesentlich dessen Gebrauchsverhalten. Diese einfache Weisheit ist Motivation für die ständige Weiterentwicklung des Untersuchungsinstrumentariums zur Gefügekennzeichnung von Baustoffen. Nachdem die Gefügeaufklärung insbesondere bei mineralischen Baustoffen bereits integrierter Bestandteil der Baustoffcharakterisierung ist, erhöht insbesondere die zunehmende Spezialisierung und Weiterentwicklung der Asphaltbaustoffe zusammen mit der Forderung nach gebrauchsgerechtem Leistungsnachweis den Bedarf an methodischer Entwicklung bei der Strukturkennzeichnung. Besondere Möglichkeiten zur tiefenaufgelösten und zerstörungsfreien räumlichen Visualisierung des Gefüges, der Ableitung strukturbeschreibender Kennwerte aber auch für eine anschließende Diskretisierung der inneren Struktur mittels finiter Elemente bietet das Verfahren der Computertomographie mit Röntgenstrahlen. Mit Hilfe verschiedener Anwendungen soll auf die Möglichkeiten dieser Methodik aufmerksam gemacht werden.
The use of high brilliance and partial coherent synchrotron light for radiography and computed tomography (CT) allows to image micro-structured, multi-component specimens with different contrast modes and resolutions up to submicrometer range. This is of high interest for materials research, life science and non-destructive evaluation applications. An imaging setup for microtomography and radiography installed at BESSY II (a third generation synchrotron light source located in Berlin, Germany) as part of its first hard X-ray beamline (BAMline) can now be used for absorption, refraction as well as phase contrast dedicated to inhouse research and applications by external users. Monochromatic synchrotron light between 6 keV and 80 keV is attained via a fully automated double multilayer monochromator. For imaging applications the synchrotron beam transmitted by the sample is converted with a scintillator into visible light. By use of microscope optics this luminescence image is then projected onto, e.g., a CCD chip. Several scintillating materials are used in order to optimise the performance of the detector system. Different optical systems are available for imaging ranging from a larger field of view and moderate resolutions (macroscope up to 14 mm x 14 mm field of view) to high resolution (microscope down to 0.35 μm pixel size), offering magnifications from 1.8× to 40×. Additionally asymmetric cut Bragg crystals in front of the scintillator can be used for a further magnification in one dimension by a factor of about 20. Slow and fast cameras are available, with up to 16 bit dynamic range. We show the suitability of the setup for numerous applications from materials research and life science.
X-ray refraction topography techniques are based on ultra-small angle scattering by micro-structural elements causing phase-related effects such as refraction and total reflection at a few minutes of arc as the refractive index of X-rays is nearly unity. The refraction contrast is several times higher than true absorption and results in images of cracks, pores and fibre debonding separations below the spatial resolution of the detector. In most cases the investigated inner surface and interface structures correlate to mechanical properties. For the exploration of micro structured materials the refraction technique has been improved by a 3D Synchrotron Refraction Computed Tomography test station. The specimen is placed in an X-ray beam between two single crystals, which suppresses all sample scattering. In addition, an asymmetric cut second crystal can magnify the image up to 50 times revealing nano meter resolution. The technique is an alternative to other attempts on raising the spatial resolution of CT machines.
The in vivo effects of coating titanium implants with organic extracellular matrix molecules were examined in the sheep tibia. Titanium screws (5.0 mm) were coated with type I collagen (Ti/Coll) or type I collagen and chondroitin sulfate (Ti/Coll/CS) by biomimetic fibrillogenesis. Uncoated screws (Ti) and screws coated with hydroxyapatite (Ti/HA) served as control. Six adult female sheep received one screw of each type to stabilize a midshaft tibial fracture with external fixation. Four cylindrical implants of 4-mm outer diameter and 3.3-mm inner diameter with the same coatings were inserted into the tibial head. No pin track infections were seen at the time of implant retrieval 6 weeks after implantation. Extraction torque was greater for Ti/HA (1181 Nmm) and Ti/Coll/CS (1088 Nmm) compared to Ti/Coll (900 Nmm) and Ti (904 Nmm) [N.S.]. Newly formed bone was noted around all coated screws within the medullary cavity. Macrophage and osteoclast activity was significantly reduced around Ti/Coll/CS in both types of implants compared to uncoated controls (p < 0.05). Osteoblast activity was significantly increased around loaded Ti/Coll and Ti/Coll/CS screws compared to uncoated Ti screws (p < 0.05). Microtomographic evaluation (SRµCT) revealed no significant differences in new bone formation around the unloaded tibial head implants.Coating of external fixation devices with of type I collagen and chondroitin sulfate appears to have similar effects with respect to stability and bone healing as HA but with less osteoclast activity. These findings were more pronounced under loaded than unloaded conditions in the sheeptibia.
Erstmals wurden MMCs mit Hilfe der Interface-Kontrast verstärkenden Röntgen-Refraktions-Technik in Kombination mit der 3D-CT-Technik untersucht. Die Methode der Röntgen-Refraktions-Topography sowie der Röntgen-Refraktions-Tomography wurden in den letzten Jahren speziell für die zerstörungsfreie Charakterisierung von Leichtbau-Hochleistungs-Werkstoffen wie Verbund-Werkstoffen und Keramiken entwickelt. Die Technik basiert auf der Refraktion von Röntgenlicht an Grenzflächen zwischen Bereichen unterschiedlicher Elektronendichte wie z.B. Faser- und Matrix-Werkstoff. Auf Grund der kurzen Röntgen-Wellenlänge hat der Brechungsindex einen Wert dicht bei eins, sodass der Streuwinkel nur wenige Bogenminuten beträgt. Der Vorteil der kurzen Wellenlänge besteht jedoch darin, dass Poren und Risse detektiert werden können, deren Größe im Nanometerbereich liegen. Damit kann die Refraktions-Technik zum besseren Verständnis von Mikro- und Submikro-Strukturen in der Materialwissenschaft eingesetzt werden. Mit der hier vorgestellten Refraktions-CT wurden Ermüdungsmechanismen an MMCs, bestehend aus SiC-Faser verstärktem Titan (Ti6242) untersucht. Die Messungen wurden am Röntgen-Messplatz der BAM (BAMline) am Synchrotron-Speicherring-BESSY in Berlin Adlershof durchgeführt.
Ein effektives Wassermanagement ist ein wichtiger Aspekt in der Entwicklung von Brennstoffzellen hinsichtlich Langzeitstabilität und Optimierung der Leistungsfähigkeit. Eine zentrale Rolle spielt dabei die Gasdiffusionslage, die für die gleichmäßige Verteilung der Reaktionsgase auf die elektrochemisch aktive Schicht (Katalysator) sorgen soll. In diesem Beitrag werden gemeinsame Forschungsaktivitäten des Helmholtz-Zentrums Berlin für Materialien und Energie (Entwicklung bildgebender Verfahren) sowie des Zentrums für Sonnenenergie- und Wasserstoff-Forschung (ZSW, Entwicklung von Brennstoffzellen) vorgestellt. Im Rahmen dieser Kooperation werden die Entstehung, die Verteilung und der Transport von flüssigem Wasser, kurz das Wassermanagement, unter Betriebsbedingungen untersucht. Mittels Synchrotronradiografie und -tomografie werden kleinste Wassercluster in der Gasdiffusionslage detektiert. Die gewonnenen Erkenntnisse dienen der Modifikation und einer gezielten Auswahl der eingesetzten Materialien.
Water transport in an operating PEM fuel cell was investigated with synchrotron X-ray radiography with a spatial resolution of 3 µm and a temporal resolution of 5 s. This method allows for the detection of water accumulations with less than 10 µm diameter. We demonstrate that synchrotron X-ray imaging can dramatically expand the possibilities of imaging with high spatial and time resolution, especially as a complement to neutron radiography. Water transport processes from the first appearance of small water accumulations in the gas diffusion layer to their transport into the channel system were analysed in situ. Correlations between local effects such as water formation and operating conditions of the whole system, e.g. power variations, were found. A recently described eruptive water transport mechanism is analysed in detail.
Corrosion of steel reinforcement in concrete exposed to chloride containing environments is a serious problem in civil engineering practice. Electrochemical methods, e.g., potential mapping, provide information whether the steel reinforcement is still passive or depassivation has been initiated. By applying such techniques no information on the type of corrosion, its extent and distribution of corrosion products is available. Particular the corrosion progress is a significant problem. Especially in the case of macrocell corrosion in reinforced concrete structures, the development at the anode cannot be separated into corrosion damage resulting from macrocell corrosion or self-corrosion. Until now also in laboratory tests it is impossible to collect such information without destroying specimens after electrochemical testing was performed. To overcome this problem it was tried to study the steel surface within the mortar specimens by X-ray tomography (CT). Within the scope of these investigations it could be shown, that X-ray tomography is suitable to make corrosion pits and their development visible which are embedded in a mortar with a cover thickness of about 35 mm. In this publication the time-dependent corrosion damage of reinforced steel is documented by X-ray tomography.
By means of synchrotron X-ray computed tomography, model composites consisting of silica and styrenebutadiene rubber were studied with a very high spatial resolution. By our analysis technique we were able to determine the nano- and micro dispersion from the experimental results by our numerical analysis. These results are discussed with respect to crucial advantages of the generically 3-dimensional tomography technique as compared to 2-dimensional methods. Our quantitative analysis of the 3d images demonstrates that in the case of our model composites the filler dispersion is good, independent on the filler concentration. Our new 3-dimensional results evidence that considering only 2-d pictures may lead to ambiguities that can lead to wrong conclusions.
Algorithms were developed to approximate the 3-dimensional internal packing density distributions of fibrous filter media at different levels of detail and complexity. Each algorithm uses certain input information derived from X-ray tomographic data of filter samples.
Algorithm 1 creates a binary media structure consisting of the true (i.e. tomographically determined) void distribution plus regions of uniform packing density. The average packing density of the media is maintained constant. Algorithm 2 creates a model fibrous structure of straight fibres of equal diameter and random length positioned randomly in space, while maintaining the true (i.e. tomographically determined) fibre orientation distribution. The number and length of the fibres on average adds up to the packing density of the filter. The model fibrous structure is recreated by a stationary Poisson process of convex bodies. Algorithm 3 distributes pores of random size and location within a homogeneous matrix, such that the average packing density again coincides with the true (i.e. tomographically determined) packing density. This algorithm is also based on a stationary Poisson process of convex bodies.
The capability of each algorithm to recreate the essential structural features of the media was tested against 'reality' by computing the respective overall pressure drop of the filter as well as the velocity distribution in the filter interior, and comparing with the results obtained for the 'true' packing density distribution of a sample measured by tomography. Compared to the assumption of a completely homogenous filter (which gives roughly 2 times the actual Δp), all algorithms are closer to reality. The binary algorithm deviates in Δp by a factor of 1.8; algorithm 3 comes within a factor of 1.6 of the true Δp. The best approximation is by algorithm 2 which narrows the difference in Δp to a factor of 1.4.
Branch junctions are mechanically particularly
interesting areas of trees, because they have to withstand a
combination of static and dynamic loads, from the stem as
well as from the branch. In the present work, the local
adaptation of material properties at branch junctions was
assessed by mapping microfibril angle and tissue density.
Images of the density distribution were obtained by computer
tomography (CT). Wide angle X-ray scattering
(WAXS) was used to determine the microfibril angle distribution
with high-resolution around the junctions. The
stem tissue around the junctions showed increased density
and microfibril angle, which points towards an optimisation
for fracture toughness. The tissue at the branch bases
showed low density combined with high MFA, which
provides deformability and flexibility and might act as
protection of the stem against load transmission from the
branch.
Synchrotron radiation-based microcomputed tomography (SR-µCT) has become a valuable tool in the
structural characterization of different types of materials, achieving volumetric details with micrometre
resolution. Biomedical research dealing with porous polymeric biomaterials is one of the research fields
which can benefit greatly from the use of SR-µCT. This study demonstrates that current experimental setups
at synchrotron beamlines achieve a sufficiently high resolution in order to visualize the positions of
individual cartilage cells cultivated on porous gelatine scaffolds made by a freeze-structuring technique.
Depending on the processing parameters, the pore morphology of the scaffolds investigated was changed
from large-pore sized but non-ordered structures to highly directional and fine pored. The cell-seeded
scaffolds were stained with a combined Au/Ag stain to enhance the absorption contrast in SR-µCT. While
only some cells showed enhanced absorption contrast, most cells did not show any difference in contrast
to the surrounding scaffold and were consequently not detectable using conventional greyscale threshold
methods. Therefore, using an image-based three-dimensional segmentation tool on the tomographic data
revealed a multitude of non-stained cells. In addition, the SR-µCT data were compared with data obtained
from scanning electron microscopy, energy dispersive X-ray spectroscopy and histology, while further
linking the initial cell density measured via a MTT assay to the pore size as determined by SR-µCT.
We present a modified aluminium casting which is especially suited as test piece for measuring casting defects and the geometry by means of cone-beam micro-focus X-ray systems, and which may become a reference standard for dimensional measurements and defect detection.
To obtain a test piece with inner geometries measured by tactile means, we divided a small aluminium cylinder head into four pieces in such a way that most inner surfaces can be reached with a tactile probe. Reference geometries (spheres and cylinders) were applied to define a coordinate system for aligning the measurements in the disassembled and re-assembled state. The four pieces were re-assembled after the tactile measurement.
The test piece also contains casting defects. In order to be able to use the assembled cylinder head as reference sample for defect detection, measurements with higher spatial resolution and better signal-to-noise ratio were performed on the single parts. For improving the reliability of the reference measurements, CT measurements of each part were carried out in three different orientations, and the individual defect detections were combined to obtain a reference data set with a high probability of defect detection and a low rate of erroneous detections.
A new method for comparing the defect detection in a CT measurement to a reference data set is demonstrated, which provides individual information on every detected flaw.
We discuss the results of measurements in the assembled state with respect to the reference data for flaw detection.
Pyrolysis and fire behaviour of a phosphorus polyester (PET-P-DOPO) have been investigated. The glycol ether of the hydroquinone derivative of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was used as a reactive halogen-free flame retardant in PET-P-DOPO. PET-P-DOPO is proposed as an alternative to poly(butylene terephthalate) (PBT) with established halogen-free additives. It exhibits a high LOI (39.3%) and achieves V-0 classification in the UL 94 test. Three different mechanisms (flame inhibition, charring and a protection effect by the intumescent char) contribute to the flame retardancy in PET-P-DOPO and were quantified with respect to different fire risks. The fire load was reduced by 66% of the PBT characteristic. The reduction is the superposition of the relative reduction due to flame inhibition (factor 0.625) and charring (factor 0.545). The peak of heat release rate (pHRR) was reduced by 83% due to flame inhibition, charring and the protection properties of the char (factor 0.486). The strength of all three mechanisms is in the same order of magnitude. The intumescent multicellular structure enables the char to act as an efficient protection layer. PBT flame-retarded with aluminium diethylphosphinate was used as a benchmark to assess the performance of PET-P-DOPO absolutely, as well as versus the phosphorus content. PET-P-DOPO exhibits superior fire retardancy, in particular due to the additional prolongation of the time to ignition and increase in char yield. PET-P-DOPO is a promising alternative material for creating halogen-free flame-retarded polyesters.