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Non-destructive evaluation of advanced materials by synchrotron radiation refraction topography
(2002)
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.
Micro damage structures of fiber reinforced polymers (FRP) can be characterized nondestructively by X-ray refraction topography, which images inner surfaces. The damage accumulation after fatigue treatment of short glass fiber reinforced polybutylene terephthalate (PBT-GF) is correlated to the applied load and the number of cycles. Micro cracks and fiber/matrix debonding during fatigue can be detected separately due to their different direction of X-ray small angle scattering. The residual strength over the crack surface decreases by a linear decay as 30 %, 60 % and 90 % of the materials lifetime is passed.
HYJECT
(2002)
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.
Non-destructive Inspection of Ceramic/Composite Materials using Non-classical X-Ray Techniques
(1999)
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.
For the first time Metal Matrix Composites (MMC) have been investigated by 3D Computed Tomography combined with enhanced interface contrast due to X-ray refraction. X-ray refraction is a relatively new approach for the characterization of advanced materials. The related techniques of Refraction Topography and Refraction Computed Tomography have been developed and applied at our laboratory during the last decade to meet the actual demand for improved nondestructive characterization of high performance composites, ceramics and other low density materials and components. X-ray refraction occurs, when X-rays crosses interfaces of spherical or cylindrical shape (e.g. pores or fibres) in the same way as visible light is refracted by lenses. These X-ray optical effects can be observed at small scattering angles of few minutes of arc as the refractive index n of X-rays is nearly unity (n = 1 10-6). Due to the short X-ray wavelength of about 0.1 nm the technique determines the amount of inner surfaces and interfaces of nanometer dimensions. The technique is expected to solve many problems in understanding the meaning of micro and sub micro structures in materials science. With the results of the CT investigation, some questions could be clarified for a better understanding of fatigue failure mechanisms under cyclic loading conditions. The specimens for the test programme have been provided by MTU Aero Engines. They consist of a titanium matrix (Ti6242) reinforced by SiC fibres (SCS6). The investigations have been performed at the materials research station of BAM (BAMline) at the Synchrotron Facility BESSY in Berlin, Germany.
Precise Measurements of Fibre Direction, Type and Content in CFRP by X-Ray Rotation Topography
(2003)
C-fibre degradation debonding and lamella buckling measurement in CMC by new X-ray topography
(1993)
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.
Tomography data obtained from transmission electron microscopes are especially attractive due to their unrivaled spatial resolution in the nanometer range or even less, but they require enormous efforts in sample preparation and suffer from a diverse accumulation of experimental restrictions, which unavoidably result in fundamental reconstruction artifacts. These restrictions refer to: partial opacity, a limited view (limited angle or missing wedge), very few angles (with respect to the detector size), limited to a region of interest (ROI; due to the sample size), variable angular increments as well as sample degradation due the interactions with the electron beam. An advanced version of the DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm proves to cope with most of these severe deviations from ideal CT measuring conditions. However, careful data preprocessing is required in order to exploit the capabilities of the algorithm.
Nanometer sized Ruthenium catalyst particles for fuel cell applications are 3D imaged at a few Ångström resolution in order to estimate their partial free surface on carbon black supports, which rule the efficiency of the catalytic activity.
Comparisons of DIRECTT reconstructions to the conventional filtered back projection, prove the significant improvements.