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Organisationseinheit der BAM
Eingeladener Vortrag
- nein (8)
Quantitative X-ray refraction topography is applied for improved nondestructive evaluation of advanced high performance ceramics. The method is based on X-ray small angle scattering by refraction of X-rays due to density differences of microstructures in heterogeneous materials. It determines the amount of inner surfaces and interfaces within the range of µm to nm dimensions. As the scattered refraction intensity is proportional to the inner surface density of a sample, a reference standard gives a quantitative measure for analytical requirements. X-ray refraction scanning topography visualizes integral interface properties at 10 µm spatial resolution by two-dimensional computer images. Characteristic microstructure parameters, i.e. density fluctuation, porosity and pore size distribution of several examples of SiO[2]-and SiC ceramics at different stages of sintering are presented.
X-Ray Refraction Techniques
(2005)
High performance composites and other light weight materials are generally a comple problem to the performance of nondestructive testing methods. X-ray refraction provide unconventional X-ray scattering techniques to meet the actual demand for improve nondestructive characterization of these advanced materials. Scanning the samples across collimated narrow incident X-ray beam permits to image integral micro-structures (a present) with a resolution of 10 µm. Investigations of samples after strain-induced micro cracks and fibre debonding in impact damaged epoxy are shown.
The physics of X-ray refraction are analogous to the well known refraction of light b optical lenses and prisms, governed by Snell's law. The special feature is the deflection a very small angles of few minutes of arc, as the refractive index of X-rays in matter i nearly one. Due to the density differences at inner surfaces most of the incident X-rays ar deflected. As the scattered intensity of refraction is proportional to the specific surface of sample, a reference standard gives a quantitative measure for analytical determinations.
Figure 1 represents a two-dimensional damage distribution of an impact in a 0/90° CFR laminate of 3 mm, thickness. Unlike in ultrasonic testing, there is no shadowing effect o the successive layers. By use of X-ray refraction the exact concentration of debonde fibres is calculated for each position. Additionally the refraction allows the selection of th fibre orientation.
X-ray dark field imaging
(2014)
A new kind of enhanced contrast X-ray imaging of weakly absorbing materials in dark field mode is presented.
Samples such as plastics and biological tissue are a perpetual challenge for radiographic imaging. Recent innovative approaches such as Diffraction Enhanced Imaging (DEI), “phase contrast”, grating interferometry (Talbot-Lau), or Refraction Enhanced Imaging (REI) have in common that they yield enhanced contrast based on deflected X-rays.
Here, we introduce a REI modification, which works with a slightly bent single crystal reflecting in Bragg geometry. The samples are placed upstream of the thin crystal within a parallel synchrotron beam. The crystal’s curvature creates a dark-field stripe in the transmission image, similar to the inverse of a Darwin-Prins rocking curve of plane crystals. The reflection condition is met better or worse as a steady function of incidence position.
Refracted beam portions of sample interfaces appear bright on black stripes. The entire image is finally synthesized by multiple dark-field stripes. The technique is an alternative to the mentioned techniques. We demonstrate the technique’s advantage by examples of biological and technical microstructures.
X-ray compton tomography
(2014)
The potentials of incoherent X-ray Scattering (Compton) tomography are investigated. Imaging materials of very different density or atomic number at once is a perpetual challenge for X-ray tomography or radiography, in general. In a basic laboratory set-up for simultaneous perpendicular Compton Scattering and direct beam attenuation tomographic scans are conducted by single channel photon counting. This results in asymmetric distortions of the projection profiles of the scattering CT-data set. ln a first approach corrections of Compton scattering data by taking advantage of rotational symmetry yield tomograms without major geometric artefacts.
A cylindrical sample composed of PE, PA, PVC, glass and wood demonstrates similar Compton contrast for all the substances, while the conventional absorption tomogram only reveals the two high order materials.
Compärison to neutron tomography reveals astonishing similarities except for the glass component (without hydrogen). Therefore, Compton CT bears the potential to replace neutron tomography, which requires much more efforts.
The potentials of incoherent X-ray scattering (Compton) computed tomography (CT) are investigated. The imaging of materials of very different atomic number or density at once is generally a perpetual challenge for X-ray tomography or radiography. In a basic laboratory set-up for simultaneous perpendicular Compton scattering and direct beam attenuation tomography are conducted by single channel photon counting line scans. This results in asymmetric distortions of the projection profiles of the scattering CT data set. In a first approach, corrections of Compton scattering data by taking advantage of rotational symmetry yield tomograms without major geometric artefacts. A cylindrical sample composed of PE, PA, PVC, glass and wood demonstrates similar Compton contrast for all the substances, while the conventional absorption tomogram only reveals the two high order materials. Comparison to neutron tomography
reveals astonishing similarities except for the glass component (without hydrogen). Therefore, Compton CT offers the potential to replace neutron tomography, which requires much more efforts.
We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets.
Microstructural aspects of composites such as reinforcement particle size, shape, and distribution play important roles in deformation behavior. In addition, Fe-rich inclusions and porosity also influence the behavior of these composites, particularly under fatigue loading. Three-dimensional (3-D) visualization of porosity and Fe-rich inclusions in three dimensions is critical to a thorough understanding of fatigue resistance of metal matrix composites (MMCs), because cracks often initiate at these defects. In this article, we have used X-ray synchrotron tomography to visualize and quantify the morphology and size distribution of pores and Fe-rich inclusions in a SiC particle-reinforced 2080 Al alloy composite. The 3-D data sets were also used to predict and understand the influence of defects on the deformation behavior by 3-D finite element modeling.
This paper gives a brief overview on3D imaging of magnetic domains with shearing grating neutron tomography. We investigated the three-dimensional distribution of magnetic domain walls in the bulk of a wedge-shaped FeSi single crystal. The width of the magnetic domains wasanalyzed at different locations within the crystal. Magnetic domains close to the tip of the wedge are much smaller than in the bulk. Furthermore, the three-dimensional shape of individual domains wasinvestigated. We discuss prospects and limitations of the applied measurement technique.
Magnetic domains have been the subject of much scientific investigation since their theoretical existence was first postulated by P.-E. Weiss over a century ago. Up to now, the three-dimensional (3D) domain structure of bulk magnets has never been observed owing to the lack of appropriate experimental methods. Domain analysis in bulk matter thus remains one of the most challenging tasks in research on magnetic materials. All current domain observation methods are limited to studying surface domains or thin magnetic films. As the properties of magnetic materials are strongly affected by their domain structure, the development of a technique capable of investigating the shape, size and distribution of individual domains in three dimensions is of great importance. Here, we show that the novel technique of Talbot-Lau neutron tomography with inverted geometry enables direct imaging of the 3D network of magnetic domains within the bulk of FeSi crystals.
The emerging technology of generation and detection of Terahertz waves (1 THz = 1012
Hz) offers diverse potentials in non-destructive testing (NDT) regarding security as well
as safety aspects. Herein, we focus on the latter with emphasis on imaging techniques.
The THz range (0.1
10 THz, 3mm
30 µm) closes the technological gap between
ultra high frequency electronics and FIR optics in the electro-magnetic (EM) spectrum.
Electro-optical sampling provides straight access to the EM wave including its phase
(rather than intensity). THz waves are well suited to characterize non-metallic materials
since they penetrate paper, plastics, ceramics and certain composites (e.g. GFC).
We employ a commercial fibre-coupled THz time domain spectrometer (TDS) for
scanning the samples laterally through a focal spot. At each position the entire temporal
pulse train is recorded, which offers the opportunity to use various parameters derivable
for imaging.
Topographic measurements are performed as reflection set-up. The achievable spatial
resolution is diffraction limited at about 100 µm -300 µm (which allows for perception
of single defects on a sub-mm scale). In contrast to typical pulse echoed ultrasound
testing THz topography is a non-contact inspection tool without coupling agents.
Several reflections of subsequent concealed layers are detected instead of just the first
encountered one. Comparing to X-ray (radiology) the non-ionizing THz-waves generate
images of similar contrast regarding metal and plastic (organic) components, while
conventional radiography emphasizes one type of material depending on the energy preselected.
Moreover, the full temporal information is exploited to derive spectra in
certain selected time windows, i.e. separated spectral properties of each layer in
multilayered structures.
Tomographic measurements are performed in transmission mode. The sample is
mounted on a rotation stage in order to allow for lateral scanning under the different
projection angles. The reconstruction is typically performed by filtered backprojection,
which is widely used for X-ray CT. The adaption of this technique to the THz range
comes along with several experimental drawbacks such as considerable refraction and
scattering. According to these difficulties we investigate the occurring artefacts. The
THz-TDS provides the opportunity to calculate a separate backprojection of each
frequency interval as obtained by the Fourier transformation of the recorded time
resolved amplitude. This results in a spectrally resolved reconstruction of each voxel,
which is unique in computed tomography technology.
Grating interferometric set-ups have been established in the last decade. They are promising candidates to obtain enhanced image contrast from weakly absorbing micro and nano structures. They are based on X-ray refraction and near-field diffraction using the Talbot effect.
At the expense of taking multiple images, Talbot-Lau grating interferometry allows separating the absorption, refraction, and scattering contributions by analysing the disturbances of a phase grating interference pattern. Contrary to other refraction enhanced methods, this technique can be applied using conventional X-ray tubes (divergent, polychromatic source). This makes it attractive to solve typical non-destructive testing problems.
We investigated the efficiency of phase gratings, i.e. the visibility (the amplitude of oscillations) upon variation of propagation distance and phase grating rotation around an axis parallel to the grid lines. This grating rotation changes the grating shape (i.e. the distributions of phase shifts). This can yield higher visibilities than derived from rectangular shapes.
Our study includes experimental results obtained from synchrotron radiation, as well as simulations for monochromatic radiation. The advantages of Talbot-Lau interferometry are demonstrated at the example of glass capillaries.
X-ray computed tomography is an important tool for non-destructively evaluating the 3-D microstructure of modern materials. To resolve material structures in the micrometer range and below, high brilliance synchrotron radiation has to be used. The Federal Institute for Materials Research and Testing (BAM) has built up an imaging setup for micro-tomography and -radiography (BAMline) at the Berliner storage ring for synchrotron radiation (BESSY). In computed tomography, the contrast at interfaces within heterogeneous materials can be strongly amplified by effects related to X-ray refraction. Such effects are especially useful for materials of low absorption or mixed phases showing similar X-ray absorption properties that produce low contrast. The technique is based on ultra-small-angle scattering by microstructural elements causing phase-related effects, such as refraction and total reflection. The extraordinary contrast of inner surfaces is far beyond absorption effects. Crack orientation and fibre/matrix debonding in plastics, polymers, ceramics and metal-matrix-composites after cyclic loading and hydro-thermal aging can be visualized. In most cases, the investigated inner surface and interface structures correlate to mechanical properties. The technique is an alternative to other attempts on raising the spatial resolution of CT machines.
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 employment of synchrotron radiation for refraction topography of materials has considerable advantages over standard x-ray sources. The much higher beam intensity and the parallel and monochromatic radiation provide faster measurements and better angular and spatial resolution. X-ray refraction techniques image the inner surface and interface concentration of micro-structured materials. This effect of x-ray optics is additional to small-angle scattering by diffraction, when the scattering objects reach micrometre dimensions. We have developed x-ray refraction techniques within the last decade in order to meet the growing demands for improved non-destructive characterization of high-performance composites, ceramics and other low-density materials. Sub-micron particle dimensions, the pore size of ceramics, the crack density distribution and single fibre debonding within damaged composites can be measured and visualized by computer-generated interface topographs. For this purpose investigations are now being performed at the new hard x-ray beamline of the Federal Institute for Materials Research and Testing (BAM) at BESSY, Berlin. This BAMline provides monochromatic radiation of photon energies from 5 to 60 keV from a double multilayer and/or a double-crystal monochromator. A separate instrument is dedicated to the further development and application of synchrotron radiation refraction (SRR) topography. Different from conventional small-angle scattering cameras with collimating slits and pinholes, scattering angles down to a few seconds of arc are selected by a single-crystal analyser, similar to a Bonse-Hart diffractometer. A 20 µm spatial resolution of the scattering micro-structures is achieved by a CCD camera with a fluorescent converter. First SRR topographs of aircraft composites [carbon fibre-reinforced plastics (CFRP), carbon fibre-reinforced ceramics (C/C), metal matrix ceramics (MMC)] will be reported.
In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics.
A novel approach to strongly suppress artifacts in radiography and computed tomography caused by the effect of
diffuse background signals ('backlighting') of 2D X-ray detectors is suggested. Depending on the detector
geometry the mechanism may be different, either based on the optical scattering of the fluorescent screen
materials into optical detection devices or Compton or X-ray fluorescence scattering by the detector components.
Consequently, these erroneous intensity portions result in locally different violations of Lambert Beers law in
single projections (radiographs) as function of the detector area coverage and the magnitude of the attenuation.
The absorption of multiple metal sheets is investigated by monochromatic synchrotron radiation, thus excluding
beam hardening. The proposed correction procedure simply requires the individual subtraction of one and the
same fraction of the primary and transmitted mean intensity, as a constant (non-local) scattering mechanism is
assumed.
The presence of elongation, streak and blurring artifacts in tomograms recorded under a missing wedge of rotation angles presents a major challenge for the quantitative analysis of tomographic image data. We show that the missing wedge artifacts of standard reconstruction algorithms may be reduced by the innovative reconstruction technique DIRECTT. For the comparison of missing wedge artifacts we apply techniques from spatial statistics, which have been specifically designed to investigate the shape of phase boundaries in tomograms.
Statistical analysis of tomographic reconstruction algorithms by morphological image characteristics
(2010)
We suggest a procedure for quantitative quality control of tomographic reconstruction algorithms. Our task-oriented evaluation focuses on the correct reproduction of phase boundary length and has thus a clear implication for morphological image analysis of tomographic data. Indirectly the method monitors accurate reproduction of a variety of locally defined critical image features within tomograms such as interface positions and microstructures, debonding, cracks and pores. Tomographic errors of such local nature are neglected if only global integral characteristics such as mean squared deviation are considered for the evaluation of an algorithm. The significance of differences in reconstruction quality between algorithms is assessed using a sample of independent random scenes to be reconstructed. These are generated by a Boolean model and thus exhibit a substantial stochastic variability with respect to image morphology. It is demonstrated that phase boundaries in standard reconstructions by filtered backprojection exhibit substantial errors. In the setting of our simulations, these could be significantly reduced by the use of the innovative reconstruction algorithm DIRECTT.
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.
Incomplete tomographic data sets such as limited view (missing wedge) data represent a well-known challenge
for reconstruction algorithms, since they unavoidably lead to substantial image artefacts. Such data sets may
occur in industrial computed tomography of limited access (e.g. extended components, fixed objects), directional
opacity, limited sample life time or laminographic set-up. We present strategies to effectively suppress the
typical elongation artefacts (e.g. lemon-like deformed pores) by our iterative algorithm DIRECTT which offers
the opportunity to vary the versatile reconstruction parameters within each cycle. Those strategies are applied to
experimental data obtained from metallic foams as well as model simulations. Comparison is drawn to state-ofthe-
art techniques (filtered backprojection and algebraic techniques). Further reference is made to reconstructions
of complete data sets serving as gold standards. For quantitative assessment of the reconstruction
quality adapted techniques based on spatial statistics are introduced.
CT (computed tomography) reconstructions of fuel cell components of a yet unrivaled spatial resolution and quality are presented. This is achieved by application of the novel DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm. We focus on two different key issues which essentially rule the fuel cell's durability on different length scales and physical interactions. On the resolution scale of some 100 µm agglomerations of condensed water in flow-field channels are detected by means of quasi-in situ neutron CT (after operation). Five orders of magnitude below nanometer sized Ru catalyst particles on carbon black support are visualized by electron tomography. Both types of experiments are especially adapted to the type of material involved but they are accompanied by severe deviations from ideal CT measuring conditions, as well. In order to overcome the tremendous reconstruction artifacts of standard algorithms, we employ DIRECTT which is described in detail. Comparisons of DIRECTT reconstructions to the conventional filtered back projection, prove the significant improvements in both experimental methods.
We present transmission electron microscope (TEM) tomography investigations of ruthenium-based fuel cell catalyst materials as employed in direct methanol fuel cells (DMFC). The digital three-dimensional representation of the samples not only enables detailed studies on number, size, and shape but also on the local orientation of the ruthenium particles to their support and their freely accessible surface area. The shape analysis shows the ruthenium particles deviate significantly from spherical symmetry which increases their surface to volume ratio. The morphological studies help to understand the structure formation mechanisms during the fabrication as well as the high effectiveness of these catalysts in the oxygen reduction reaction at the cathode side of fuel cells.
Precise Measurements of Fibre Direction, Type and Content in CFRP by X-Ray Rotation Topography
(2003)
The morphology and thermal behaviour of polypropylenegraftmaleic anhydride (PPgMA) layered silicate (montmorillonite) nanocomposites were investigated using X-ray diffraction, transmission electron microscopy, differential scanning calorimetry and thermogravimetry. The study focuses on the influence of the presence of oxygen during the preparation of PPgMAnanocomposite using two different modified clays. The nanocomposites show tactoid, intercalated and exfoliated structures side by side with different dominant states depending on the clay used and on the processing conditions. The systems are described as multi-component blends rather than binary blends since the organic ions do not only change the mixing behaviour, but also influence material properties. Beside the physical barrier property of the clay layers also chemical processes were found to play an important role.