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Compounds with Iron and Rare Earth elements as reference materials for X-Ray spectroscopy

During the last two decades synchrotron-based methods have been established in energy and materials sciences as driving forces for the investigation of composition, structure and function of new materials. These methods benefit from the unique characteristics of the synchrotron radiation, e.g. polarization, coherence and brilliance. In XANES spectroscopy the electronic properties of chemical bonding could be measured to describe the structure of unknown compounds or to identify compounds by comparison with reference spectra. Since the access to synchrotron lab time is strictly limited the development of a laboratory XANES spectrometer with comparable resolution to Synchrotron-based technique, reasonable measuring time and relatively high sample throughput would be highly desirable for routine analysis in science and industry. For this drawbacks, like lower brilliance of X-ray tubes, sufficient area density of analyte masses or intensity losses during spectral separation, have to be overcome.

Scheme of laboratory XANES spectrometer at TU Berlin for measurement of samples in transmission

The group of Prof. U. Kanngießer at the TU Berlin is successful testing graphite mosaic crystals in von Hamos-geometry [1] for spectral resolution of E/DE around 2000 at a laboratory XANES spectrometer. Together with her group we systematically optimize sample preparation and test the influence of several parameters (particle size, mass density, matrix composition, …) on spectral quality and the afterwards calculated results. The focus is currently set on iron and Rare Earth containing compounds, which are under investigation in many different scientific fields and play an important role in industrial applications. For this purpose selected oxides, sulfides and complexes are synthesized with different particle sizes followed by comprehensive characterization of the material and their testing for several preparation procedures. First promissiong results have already been obtained for iron compound.

For this purpose selected oxides, sulfides and complexes are synthesized with different particle sizes followed by comprehensive characterization of the material and their testing for several preparation procedures. First promissiong results have already been obtained for iron compound.

Spectra of pure iron Fe(0) (left), a mixture of 50% Fe(0) and Fe2O3 (center) and pure Fe2O3 (right).

Literature

C. Schlesiger, L. Anklamm, H. Stiel, W. Malzer, B. Kanngießer, Journal of Analytical Atomic Spectrometry 30, 1080-1085 (2015) 

Cooperation partners

 Prof. B. Kanngießer, Dr. W. Malzer, TU Berlin