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- Computed tomography (11)
- X-ray refraction (11)
- Pore size (4)
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- Porosity (3)
- Porous ceramics (3)
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Organisationseinheit der BAM
The first hard X-ray beamline at BESSY II will be installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a Double-Multilayer-Monochromator and a Double-Crystal-Monochromator. The two devices can be used separately or in-line. Main applications of monochromatic radiation with photon energies up to 50 keV are X-ray fluorescence analysis, micro-computed tomography, X-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV will be available for radiometric applications.
Different very dilute suspensions of magnetic nanoparticles (magnetite surrounded by an organic shell) in water (ferrofluids) were investigated using small-angle X-ray scattering. It is shown that the scattering originates not only from noncorrelated coreshell nanoparticles, but also from larger structures. By modelling, these structures can be identified as close-packed clusters consisting of coreshell particles (core diameter ~10 nm). The analysis of the radial distance distribution function, obtained by Fourier transformation of the scattered intensity, reveals a lower bound of the mean cluster size of about 40 nm. The formation of clusters is persistent, even in very dilute suspensions.
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.
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.
Microstructural characterization of porous materials by two-dimensional X-ray refraction topography
(2004)
X-ray refraction topography determines the internal surfaces and interfaces of non-metallic porous materials within the range of namometer to micrometer dimensions. The method is based on refraction of X-rays caused by interfaces of microstructures in heterogeneous materials.
Generally, it permits a non-destructive full volume characterization of the pore topology. The X-ray refraction scanning technique make possible to visualize integral interface properties up to 10 μm spatial resolution by two-dimensional topographic images. It detects the spatially resolved internal surfaces of both, open and closed pores. Comparison to a certified powder reference of uniform grain size and known packing density reveals a quantitative measure for calibration requirements. An investigation on SiC- and Al2O3-ceramics illustrate the quantitative characterization of the internal surface density, pore sizes and their spatial distribution as well as local porosity fluctuations.
Neutron tomography was applied to study the 3D water distribution in full polymer electrolyte membrane fuel cell (PEMFC) stacks. The water distribution after switch-off of the fuel cell was analyzed over a period of 36 h. We found a slowly increasing water amount in the fuel cell, but only few changes within a time period of 5 h, which is about the time necessary for neutron tomography. In this way, the requirement for successful tomography was obtained. It is demonstrated how the quasi in-situ tomography technique enables us to study the water content in individual flow field channels of three-fold stacks. Flow field as well as stack design issues are addressed by this visualization method showing weak points due to a non-uniform water distribution that can be identified by means of neutron imaging.
A novel approach is suggested to strongly suppress artifacts in radiography and computed tomography caused by the effect of diffuse background signals 'backlighting' of 2D X-ray detectors. Depending on the detector geometry the mechanism may be different. Either based on the optical scattering of the fluorescent screen materials into the 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 Beer's law in single projections (radiographs) as a 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.
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.
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 by 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–Beer's law in single projections (radiographs). When used as input data for computed tomography these violations are directly observed via modulation of the projected mass as a function of the rotation phase and the samples aspect ratio (dynamics). The magnitude of the diffuse background signal depends on the detector area covered by the projected sample. They are more pronounced the smaller the shadowed area and the stronger the total attenuation. This implies that the reconstruction suffers from additional anisotropic artifacts caused by elongated sample structures. This issue is studied simply by absorption of flat plates in a conventional laboratory radiography set-up and at a synchrotron radiation facility. In the latter case beam hardening artifacts can be excluded due to the monochromatic radiation. The proposed correction procedure requires simple integral intensity offsets as a constant (non-local) light scattering mechanism is assumed.
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.