No abstract

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.

X-ray graphite optics consists of thin layers of Pyrolytic Graphite (PG) attached to a substrate of focusing shape. Pyrolytic Graphite is a perfect artificial graphite obtained by annealing of carbon deposit at temperatures about 3000 °C under deformation. By varying the annealing conditions, one could get PG of different mosaic structure and mechanical properties. A wide variability of the reflecting layer characteristics and optics shape makes the graphite optics useful in an extended range of applications. The optics could be adjusted to applications that require moderate resolution as EDXRF (energy dispersive X-Ray fluorescence) and as well as for high-resolution applications as EXAFS (extended X-ray absorption fine structure), XANES (X-ray absorption near-edge structure) and XES (X-ray emission spectroscopy). To realize the optics with theoretically optimized parameters the relationship between the production procedure and the mosaicity and reflectivity of the optics was experimentally studied. The influence of thickness, the type of PG (Highly Oriented PG (HOPG) or Highly Annealed PG (HAPG)) and substrate characteristics on the optics performance is presented.

Highly annealed pyrolytic graphite (HAPG) is an advanced type of pyrolytic graphite that, as a mosaic crystal, combines high integral reflectivity with a very low mosaicity of typically less than 0.1°. When used as dispersive X‐ray optics, a high resolving power has been observed, rendering HAPG very suitable for applications in high‐resolution X‐ray spectroscopy, which conventionally relies on ideal crystals. For the design and modelling of HAPG crystals in applications requiring high spectral resolution, the diffraction properties must be known very accurately. To close this gap, a comprehensive characterization of HAPG crystals was performed that allows for modelling of the diffraction properties in different diffraction orders over a broad spectral range. The crystal properties under investigation are the mosaic spread, the peak reflectivity and the intrinsic reflection width. The investigations were carried out for different thickness crystal films, which were mounted adhesively on a substrate. It is shown that the diffraction properties are strongly correlated to the grade of adhesion, which depends crucially on the substrate material and its surface properties. The investigations were performed using monochromated tunable synchrotron radiation of high spectral purity with a high‐precision experimental setup and calibrated detection devices at the electron storage ring BESSY II.

A new method of producing strongly bent highly oriented pyrolytic graphite (HOPG) is presented. The method allows one to make a crystal of almost arbitrary shape, but has some thickness limits. A review of the results obtained on this type of crystal by different laboratories during the last 10 years is given. An x-ray intensity gain from a synchrotron radiation source and Mo Ka tube beams of one order of magnitude could be achieved when using a crystal of optimized shape. The application of the crystals for secondary monochromatization in EDXRF improves by one order of magnitude the detection limits for the elements of interest.