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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.
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.
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.
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.
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.
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.
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.
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.
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.
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.