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Eingeladener Vortrag
- nein (21)
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.
Kurzfassung
Röntgen-Computertomographie (CT) ist eine industriell eingeführte Technik zur zerstörungsfreien Fehlererkennung. Seit einiger Zeit werden industrielle CT-Anlagen auch zur Geometriebestimmung, d.h. für dimensionelle Messungen eingesetzt. Bei diesen Messungen treten Messabweichungen auf, die wegen komplexer Einflussgrößen derzeit nur schlecht quantifiziert werden können. Die Größe der beobachteten Messabweichungen erschwert zum Teil noch die weitere Anwendung der CT als Messtechnik. Das momentan mit CT messbare Teilespektrum wird bei dickwandigen Bauteilen durch die fehlende Verfügbarkeit von Röntgendetektoren für hohe Energien (speziell Flächendetektoren) beschränkt. Im folgenden wird ein Forschungsprojekt zwischen 10 deutschen Industrieunternehmen und Instituten und zwei deutschen Bundesanstalten (Physikalisch-Technische Bundesanstalt (PTB) und Bundesanstalt für Materialforschung und -prüfung) vorgestellt, dass die Weiterentwicklung der CT als dimensionelle Messtechnik zur Aufgabe hat. Das Projekt hat eine Laufzeit von drei Jahren (Start 01.Okt. 2003). Es werden hier die Projektziele und erste Ergebnisse vorgestellt.
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.
Die sehr gute Reproduzierbarkeit von tomographischen Messungen zusammen mit den digital vorliegenden Ergebnissen ermöglicht die zerstörungsfreie dreidimensionale quantitative Analyse der untersuchten Bauteile und Proben mit Methoden der Bildverarbeitung. Vorwiegend für den Nachweis von Poren eingesetzt, lassen sich mit CT auch unterschiedliche Materialbestandteile analysieren, wobei die einzige Voraussetzung ein hinreichender Unterschied (es genügen wenige Prozent) in den Röntgenabsorptionseigenschaften der zu unterscheidenden Bestandteile ist.
Mit den in der Bundesanstalt für Materialforschung und -prüfung entwickelten Computertomographieanlagen kann der Anteil von Hohlräumen und Materialbestandteilen einer Probe bestimmt werden, wobei die Größe der nachzuweisenden Bestandteile sich über mehrere Größenordnungen erstreckt.
An ausgewählten Beispielen aus den Bereichen Keramik, Bodenproben und Fahr-bahnübergangssystemen aus Asphalt werden die quantitativen Ergebnisse dargestellt und die in der Bestandteilanalyse erreichbare Genauigkeit diskutiert.
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.
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.
Die Produktion von elektronischen, optischen und elektro-mechanischen Mikro- und Nanosystemen stellt hohe Anforderungen an die Messtechnik, um die Fertigungsprozesse zu optimieren und die Qualität zu prüfen. Existierende Messverfahren unterliegen Beschränkungen hinsichtlich des Auflösungsvermögens, der Messfeldgröße und des Ergebnisses der Messung. Der kombinierte Einsatz von Sensoren mit unterschiedlichen Fähigkeiten in den Auflösungsstufen mittels einer intelligenten Messstrategie ermöglicht eine effiziente Prüfung.
Neben den geeigneten Prüfstrategien werden auch Methoden zur Fusion und Auswertung der Daten von Sensoren mit unterschiedlichen Auflösungsfähigkeiten benötigt. Datenfusion bezeichnet dabei das Zusammenfügen verschiedener Messungen, um entweder unterschiedliche Eigenschaften eines Messobjekts in einem gemeinsamen Koordinatensystem angeben zu können oder um aus verschiedenen Messungen derselben Eigenschaft des Messobjekts einen Datensatz von höherer Qualität gegenüber den einzelnen Datensätzen zu erhalten. Voraussetzung für die Datenfusion ist Registrierung, die eine Überführung von Messdaten unterschiedlicher Messfelder oder Messmittel in ein gemeinsames Koordinatensystem darstellt und Thema dieses Beitrages ist.
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.
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.
Carrying out dimensional measurements by CT means assessing coordinates in space. CT must therefore be treated as a coordinate measuring technique similar to optical or tactile Coordinate Measuring Machines (CMMs). The well-established standards and guidelines for the acceptance- and verificationtesting of CMMs require the use of calibrated reference standards to achieve measurement machine characteristics.
Hence, transferring these concepts from coordinate metrology to CT, a dedicated CT-specific reference standard was designed, manufactured and calibrated using a tactile CMM. For comparison purposes, a CAD model was created by reverse engineering using the calibration data. The calibrated model was fed into a virtual CT and the measurement process was simulated. The reference standard was measured by micro-CT.
By comparing the characteristics of the measurement output of CT and the output gained from simulation, the influences of measurement artefacts can be judged, for the first time, in analogy to existing Guidelines of coordinate metrology.
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.
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 high-resolution synchrotron-based imaging stations at the BAMline (BESSY) and TopoTomo (ANKA)
(2008)
The BAMline at the BESSY light source in Berlin and the TopoTomo beamline at the ANKA synchrotron facility in Karlsruhe (both Germany) operate in the hard X-ray regime (above 6 keV) with similiar photon flux density. For typical imaging applications, a double multilayer monochromator or a filtered white beam is used. In order to optimise the field of view and the resolution of the available indirect pixel detectors, different optical systems have been installed, adapted, respectively, to a large field of view (macroscope) and to high spatial resolution (microscope). They can be combined with different camera systems, ranging from 16-bit dynamic range slow-scan CCDs to fast CMOS cameras. The spatial resolution can be brought substantially beyond the micrometer limit by using a Bragg magnifier. The moderate flux of both beamlines compared to other 3rd generation light sources is compensated by a dedicated scintillator concept. For selected applications, X-ray beam collimation has proven to be a reliable approach to increase the available photon flux density. Absorption contrast, phase contrast, holotomography and refraction-enhanced imaging are used depending on the application. Additionally, at the TopoTomo beamline digital white beam synchrotron topography is performed, using the digital X-ray pixel detectors installed.
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.
Use of 3D Micro Tomography for the Investigation of the Mechanical Properties of Cellular Metals
(2003)
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.
Zwei Bildhauermodelle aus dem Georg-Kolbe-Museum Berlin standen
zur Restaurierung an. Das kleinere, "Lucino" (1920), 41cm, wurde hochauflösend
mit CT gemessen, da mittels CT sowohl der Herstellungsprozeß einer Gipsstatue
als auch der innere Zustand, wie Ergänzungen, Klebungen und Armierungen,
festgestellt werden können. Aus den CT Bildern ergab sich eine für die vorher vermutete
Gipszusammensetzung ungewöhnliche innere Struktur. Mit einer Freihand
bedienten Röntgenpistole zur Messung der Röntgenfluoreszenz wurde daraufhin die
Zusammensetzung des Materials der Statuette als Terracotta bestimmt. Durch den
Einsatz von Helium als Spülmittel konnten auch leichte Materialien nachgewiesen
und so eine Unterscheidung zwischen Gips und gebranntem Ton durchgeführt werden.
Aus den CT Daten wurde eine virtuelle Darstellung der äußeren Geometrie gewonnen.
Ein damit versuchsweise erstelltes Replik (Rapid Prototyping, 3D-Drucker,
TU-Berlin) entsprach nicht den Anforderungen des Museums zur Erstellung einer
Gußform für eine Bronzekleinserie der Statuette.
Die zweite Statue, die "Große Nacht" (1930) ist mit ihrer Größe von 2,12m und aufgrund
des durch korrodierende Metallarmierung verursachten Schadensbildes nicht
mehr transportfähig. Eine in-situ Untersuchung mit dem mobilen Tomographen, der
in den 1980ern zur Untersuchung von Bäumen gebaut und jetzt mit einem modernen
Flachdetektor und einer Röntgenröhre ausgestattet ist, wird vorgestellt. Die Möglichkeiten
der in-situ CT für große Skulpturen werden anhand der Ergebnisse diskutiert.