X‐ray optics with high energy resolution and collection efficiency are required in X‐ray spectroscopy for investigations of chemistry and coordination. This is particularly the case if the X‐ray source emits a rather weak signal into a large solid angle. In the present work the performance of a spectrometer based on thin mosaic crystals was investigated for different spectroscopic methods using various X‐ray sources. It was found that, even with low‐power X‐ray sources, advanced high‐resolution X‐ray spectroscopy can be performed.
Three-dimensional micro-XRF is a recently developed microprobe which facilitates three-dimensional resolved chemical analyses with a resolution of around 20 mum. Arbitrary sites or sections of samples can be investigated without the need to section specimens physically. In this paper we demonstrate the use of the microprobe in combination with a cold nitrogen gas stream for the cryogenic fixation of specimens. A 3D micro-XRF setup at the new microfocus beamline at BESSY II was equipped with a nitrogen cryogenic stream. The distribution of Ca, Fe, Zn and Cu across virtual cross sections of a water-rich sample, the root of common duckweed, could be investigated without further sample preparation. This paper demonstrates the capabilities of 3D micro-XRF under cryogenic conditions for investigations of biological specimens.
The combination of polycrystalline silicon (poly-Si) thin films with aluminum doped zinc oxide layers (ZnO:Al) as transparent conductive oxide enables the design of appealing optoelectronic devices at low costs, namely in the field of photovoltaics. The fabrication of both thin-film materials requires high-temperature treatments, which are highly desired for obtaining a high electrical material quality. Annealing procedures are typically applied during crystallization and defect-healing processes for silicon and can boost the carrier mobility and conductivity of ZnO:Al layers. In a combined poly-Si/ZnO:Al layer system, an in-depth knowledge of the interaction of both layers and the control of interface reactions upon thermal treatments is crucial. Therefore, we analyze the influence of rapid thermal treatments up to 1050 °C on solid phase crystallized poly-Si thin-film solar cells on ZnO:Al-coated glass, focusing on chemical interface reactions and modifications of the poly-Si absorber material quality. The presence of a ZnO:Al layer in the solar cell stack was found to limit the poly-Si solar cell performance with open circuit voltages only below 390 mV (compared to 435 mV without ZnO film), even if a silicon nitride (SiN) diffusion barrier was included. A considerable amount of diffused zinc inside the silicon was observed. By grazing-incidence X-ray fluorescence spectrometry, a depth-resolving analysis of the elemental composition close to the poly-Si/(SiN)/ZnO:Al interface was carried out. Temperatures above 1000 °C were found to promote the formation of new chemical compounds within about 10 nm of interface, such as zinc silicates (Zn2SiO4) and aluminium oxide (AlxOy). These results give valuable insights about the temperature-limitations of Si/ZnO thin-film solar cell fabrication and the formation of high-mobility ZnO-layers by thermal anneal.
A combination of 3D micro X-ray fluorescence spectroscopy (3D micro-XRF) and micro-XRF was utilized for the investigation of a small collection of highly heterogeneous, partly degraded Dead Sea Scroll parchment samples from known excavation sites. The quantitative combination of the two techniques proves to be suitable for the identification of reliable marker elements which may be used for classification and provenance studies. With 3D micro-XRF, the three-dimensional nature, i.e. the depth-resolved elemental composition as well as density variations, of the samples was investigated and bromine could be identified as a suitable marker element. It is shown through a comparison of quantitative and semiquantitative values for the bromine content derived using both techniques that, for elements which are homogeneously distributed in the sample matrix, quantification with micro-XRF using a one-layer model is feasible. Thus, the possibility for routine provenance studies using portable micro-XRF instrumentation on a vast amount of samples, even on site, is obtained through this work.
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