Hydrogen analysis is of particular importance in thin film technology and it is often necessary to obtain a depth profile. The method with the best depth resolution is NRA using the 6385 keV resonance of the 1H(15N,αγ)12C nuclear reaction. The correct quantification of the depth and concentration scales in the measured hydrogen profiles relies on accurate stopping power values. We present a method to deduce these values from a combination of two techniques: NRA and X-ray reflectometry (XRR). This method is applied to the determination of the stopping power of ~6.4 MeV 15N ions in H-containing amorphous Si-layers (a-Si:H). Density-independent stopping powers at different H concentrations are determined by combining the results from NRA and XRR with an overall uncertainty of 3.3%, showing good agreement with SRIM values. This work shows exemplary the methodology for future evaluation of stopping powers for quality assurance in NRA.
Well-defined and facetted bimetallic gold–palladium nanoalloys have been synthesized and anchored in spherical polyelectrolyte brushes (SPB) as composite particles (AuPd@SPB). These particles are better catalysts in aqueous phase than the pure metals. The atomistic arrangement of these nanoalloys has been analysed by extended X-ray absorption fine structure (EXAFS) spectroscopy at the Au–L3 and the Pd–K absorption edge. The samples with high amounts of gold appear as almost statistically mixed random alloys. Alloy compositions with less gold show slight enrichment of Pd at the surface of the particle. In addition, signals of non-metallic palladium appear at the Pd–K edge which indicate the presence of the Pd2+ species in addition to metallic palladium. The relation of these structural features to the catalytic activity is discussed.
Larger spectral bandwidth and higher photon flux density are the major advantages of multilayer monochromators over crystal-based devices. Especially for synchrotron-based hard X-ray microimaging applications the increased photon flux density is important in order to achieve high contrast and resolution in space and/or time. However, the modifications on the beam profile induced by reflection on a multilayer are a drawback which can seriously harm the performance of such a monochromator. A recent study [A. Rack, T. Weitkamp, M. Riotte, D. Grigoriev, T. Rack, L. Helfen, T. Baumbach, R. Dietsch, T. Holz, M. Krämer, F. Siewert, M. Meduna, P. Cloetens, E. Ziegler, J. Synchrotron Radiat. 17 (2010) 496510] has shown that the modifications in terms of beam flatness and coherence preservation can be influenced via the material composition of the multilayer coating. The present article extends this knowledge by studying further material compositions used on a daily basis for hard X-ray monochromatization at the beamline ID19 of the European Synchrotron Radiation Facility.
Biocompatible materials such as titanium are regularly applied in oral surgery. Titanium-based implants for the replacement of missing teeth demand a high mechanical precision in order to minimize micro-bacterial leakage, especially when two-piece concepts are used. Synchrotron-based hard x-ray radiography, unlike conventional laboratory radiography, allows high spatial resolution in combination with high contrast even when micro-sized features in such highly attenuating objects are visualized. Therefore, micro-gap formation at interfaces in two-piece dental implants with the sample under different mechanical loads can be studied. We show the existence of micro-gaps in implants with conical connections and study the mechanical behavior of the mating zone of conical implants during loading. The micro-gap is a potential source of implant failure, i.e., bacterial leakage, which can be a stimulus for an inflammatory process.
A new instrument for simultaneous microbeam small- and wide-angle X-ray scattering and X-ray fluorescence (SAXS/WAXS/XRF) is presented. The instrument is installed at the microfocus beamline at BESSY II and provides a beam of 10 µm size with a flux of about 109 photons s-1. A SAXS resolution up to 500 Å d-spacing and a range of scattering vectors of almost three orders of magnitude are reached by using a large-area high-resolution CCD-based detector for simultaneous SAXS/WAXS. The instrument is particularly suited for scanning SAXS/WAXS/XRF experiments on hierarchically structured biological tissues. The necessary infrastructure, such as a cryo-stream facility and an on-site preparation laboratory for biological specimens, are available.
Synchrotron radiation (SR) has been used in recent years as an excellent excitation source for X-ray fluorescence spectrometry. SR offers, in contrast to conventional X-ray sources, highly brilliant polychromatic, polarized radiation with which micro-domain X-ray fluorescence spectrometry becomes possible. A feasibility study of utility, conducted at BESSY (Berlin) and at DELTA (Dortmund), both synchrotron facilities of the third generation, to evaluate the use of wavelength dispersive X-ray fluorescence spectrometry in combination with synchrotron radiation is presented. First results for material analysis, obtained by combining the synchrotron radiation and a commercially available spectrometer commonly attached to a scanning electron microscope, are presented. The spectrometer, of the linear type, uses curved focusing Bragg-crystals of the Johann type which leads to a high spectral resolution up to 3 eV. Examples of micro-domain analyses are presented and compared with those obtained by synchrotron radiation induced energy dispersive X-ray fluorescence.
X-ray topography is a well known imaging technique to characterise strain and extended defects in single crystals. Topographs are typically collected on X-ray films. On the one hand such photographic films show a limited dynamic range and the production of films will be discontinued step by step in the near future. On the other hand new imaging detectors improved for X-ray tomography become more and more attractive even for topography because of increasing resolution, dynamic range, speed and active area. In this paper we report about the upgrade of the TOPOTOMO beamline at the synchrotron light source ANKA, Research Centre Karlsruhe, with a high resolution digital camera for the topography use.
Biocompatible materials such as porous bioactive calcium phosphate ceramics or titanium are regularly applied in dental surgery: ceramics are used to support the local bone regeneration in a given defect, afterwards titanium implants replace lost teeth. The current gold standard for bone reconstruction in implant dentistry is the use of autogenous bone grafts. But the concept of guided bone regeneration (GBR) has become a predictable and well documented surgical approach using biomaterials (bioactive calcium phosphate ceramics) which qualify as bone substitutes for this kind of application as well. We applied high resolution synchrotron microtomography and subsequent 3d image analysis in order to investigate bone formation and degradation of the bone substitute material in a three-dimensional manner, extending the knowledge beyond the limits of classical histology. Following the bone regeneration, titanium-based implants to replace lost teeth call for high mechanical precision, especially when two-piece concepts are used in order to guaranty leak tightness. Here, synchrotron-based radiography in comparison with classical laboratory radiography yields high spatial resolution in combination with high contrast even when exploiting micro-sized features in these kind of highly attenuating objects. Therefore, we could study micro-gap formation at interfaces in two-piece dental implants with the specimen under different mechanical load. We could prove the existence of micro-gaps for implants with conical connections as well as to study the micromechanical behavior of the mating zone of conical implants during loading. The micro-gap is a potential issue of failure, i. e. bacterial leakage which can induce an inflammatory process.
For quantitative SRXRF measurements the angle of incidence of the incoming X-ray beam is an important factor. When the sample is focused by a long-range-microscope, the determination of the angle can be automatized using a simple algorithm. This was developed to improve the orientation of especially round or ornate samples. As a side effect the three dimensional surface can be reconstructed, too.
Fingerprinting ancient gold work requires the use of nondestructive techniques with high spatial resolution (down to 25 µm) and good detection limits (micrograms per gram level). In this work experimental setups and protocols for synchrotron radiation induced X-ray fluorescence (SRXRF) at the BAMline of the Berlin electron storage ring company for synchrotron radiation (BESSY) in Berlin for the measurement of characteristic trace elements of gold are compared considering the difficulties, shown in previous works, connected to the quantification of Pt. The best experimental conditions and calculation methods were achieved by using an excitation energy of 11.58 keV, a silicon drift chamber detector (SDD) detector, and pure element reference standards. A detection limit of 3 µg/g has been reached. This newly developed method was successfully applied to provenancing the Xiongnu gold from the Gol Mod necropolis, excavated under the aegis of the United Nations Educational, Scientific and Cultural Organization (UNESCO). The composition of the base alloys and the presence of Pt and Sn showed that, contrary to what is expected, the gold foils from the first powerful empire of the steppes along the Great Wall were produced with alluvial gold from local placer deposits located in Zaamar, Boroo, and in the Selenga River.
The propagation of synchrotron radiation through nanocapillary structures with channel sizes of 200 nm and periods in the micrometer size has been studied experimentally. It was shown that the propagation through individual capillary channels has a mode formation character. Furthermore it was shown that during the propagation through capillary channels the coherence of synchrotron radiation is partially conserved. Interference of beams propagating through different capillary channels is observed which leads to a periodically modulated distribution of the radiation intensity in a plane far from the exit of the structure. These investigations are of high relevance for the understanding of X-ray transmission through nanocapillaries and the appearance of wave properties at this size scale.
Compact pnCCD-based X-ray camera with high spatial and energy resolution: a color X-ray camera
(2011)
For many applications there is a requirement for nondestructive analytical investigation of the elemental distribution in a sample. With the improvement of X-ray optics and spectroscopic X-ray imagers, full field X-ray fluorescence (FF-XRF) methods are feasible. A new device for high-resolution X-ray imaging, an energy and spatial resolving X-ray camera, is presented. The basic idea behind this so-called 'color X-ray camera' (CXC) is to combine an energy dispersive array detector for X-rays, in this case a pnCCD, with polycapillary optics. Imaging is achieved using multiframe recording of the energy and the point of impact of single photons. The camera was tested using a laboratory 30 µm microfocus X-ray tube and synchrotron radiation from BESSY II at the BAMline facility. These experiments demonstrate the suitability of the camera for X-ray fluorescence analytics. The camera simultaneously records 69696 spectra with an energy resolution of 152 eV for manganese Kα with a spatial resolution of 50 µm over an imaging area of 12.7 × 12.7 mm². It is sensitive to photons in the energy region between 3 and 40 keV, limited by a 50 µm beryllium window, and the sensitive thickness of 450 µm of the chip. Online preview of the sample is possible as the software updates the sums of the counts for certain energy channel ranges during the measurement and displays 2-D false-color maps as well as spectra of selected regions. The complete data cube of 264 × 264 spectra is saved for further qualitative and quantitative processing.