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The first hard x-ray beamline at BESSY II has been 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. Depending on the application, the two devices are used separately or in-line. The main applications of the monochromatic radiation with photon energies up to 60 keV are x-ray fluorescence analysis, micro computed tomography, x-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV is available for radiometric applications.
New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (16061669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of µg/cm². Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is together with external micro-proton-induced X-ray emission the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing FrenchGerman database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection.
A layer of Sb atoms, implanted with an energy of 400 keV and a nominal dose of 5×1016 atoms/cm2 into a high purity silicon wafer, was certified for its areal density (atoms/cm2) using Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA) and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) and for its isotope ratio using INAA and ICP-IDMS. Excellent agreement between the results of the different independent methods was found. In the present work, the measurements of the homogeneity of the areal density of Sb, previously determined with RBS in spots having 1 mm diameter, are improved with synchrotron X-ray fluorescence analysis: Higher precision in even smaller sample spots allows to estimate a reduced inhomogeneity of the whole batch of samples of the order of only 0.4%. Thus the uncertainty of the certified value can further be reduced. Down to fractions of a chip with 0.3×0.4 mm2 area, the areal density is now certified as (4.81±0.06)×1016 Sb atoms/cm2, where the expanded uncertainty 0.06 (coverage factor k=2) corresponds to only 1.2%. The relative merits of the different analytical methods are discussed.
Electron probe microanalysis (EPMA) measurement of thin-film thickness in the nanometre range
(2002)
The thickness of thin films of platinum and nickel on fused silica and silicon substrates has been determined by EPMA using the commercial software STRATAGEM for calculation of film thickness. Film thickness ranged in the order 10 nm. An attempt was made to estimate the confidence range of the method by comparison with results from other methods of analysis. The data show that in addition to the uncertainty of the spectral intensity measurement and the complicated fitting routine, systematic deviation caused by the underlying model should be added. The scattering in the results from other methods does not enable specification of a range of uncertainty, but deviations from the real thickness are estimated to be less than 20%.
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.
Four hundred sixteen silver coins stemming from the Ottoman Empire (16th and 17th centuries) were analyzed in order to confirm the fineness of the coinage as well as to study the provenance of the alloy used for the coins. As most of the coins showed the typical green patina on their surfaces due to corrosion processes which have led to the depletion of copper in the near-surface domains of the silver coins in comparison to their core composition, small samples by cutting splinters from the coins had to be taken, embedded in synthetic resin and cross-sectioned in order to investigate the true-heart metal composition. The type of the alloy was investigated as well as if coins minted in different locations demonstrated homogeneous traits concerning the predominant impurities which could suggest a common ore. Several X-ray based techniques (µ-XRF, µ-SRXRF and µ-PIXE) could be applied in order to determine the silver contents as well as the minor and trace elements. Finally, SEM/EDX was applied in order to study the homogeneity/heterogeneity of the coins and the presence of surface enrichments. In general, the silver content of the analyzed specimen varies between 90% and 95%. These outcomes have not supported the historical interpretations, which predict that during the period studied a debasement of approximately 44% of the silver content of the coins should have occurred.
Trace-elements are more significant for provenancing archaeological metallic artifacts than the main components. For gold, the most promising elements are platinum group elements (PGE), Sn, Te, Sb, Hg and Pb. Several small fragments of natural Transylvanian gold placer and primary were studied by using micro-PIXE technique at the Legnaro National Laboratory AN2000 microbeam facility, Italy and at the AGLAE accelerator, C2RMF, Paris, France and by using micro synchrotron radiation X-ray fluorescence (micro-SR-XRF) at BESSY synchrotron, Berlin, Germany. The goal of the study was to identify the trace-elements, especially Sn, Sb and Te. A spectacular application to five Dacian gold bracelets authentication is presented (Sn and Sb traces).