In situ Pair Distribution Function (PDF) analysis on a laboratory diffractometer at temperatures up to 1000 °C
The PDF Parts for the Anton Paar HTK 1200N High-Temperature Oven Chamber allow total X-ray scattering experiments to be performed under non-ambient conditions on a laboratory dif-fractometer. Results of measurements on a quartz sample show the possibilities for in situ PDF analysis.
The total X-ray scattering technique (including Bragg peaks and diffuse scattering) and pair distribution function (PDF) analysis (1) are a powerful combination to study the structural properties of both crystalline and non-crystalline materials. Unlike conventional X-ray diffraction methods which rely on the presence of long-range order within the sample, the total X-ray scattering technique probes the local atomic arrangement and can therefore be used for the study of amorphous, nanocrystalline or nanostructured materials and even liquids. From an experimental point of view, a typical PDF analysis requires the use of intense high energy X-ray radiation (E ≥ 15 keV) and a wide 2θ measurement range. After initial feasibility studies regarding the use of standard laboratory diffractometers for PDF analysis (2-4), this application has been further developed to improve data quality and to extend the range of materials, environmental conditions, and measurement geometries that can be used for PDF experiments. Studies performed on different crystalline, nanocrystalline, and amorphous materials of scientific and technological interest, including organic materials, oxides, metallic alloys, etc., have demonstrated that PDF analysis with a laboratory diffractometer can be a valuable tool for structural characterization of a wide range of materials (2-6).
1. T. Egami, S. J. L. Bilinge, Underneath the Bragg Peaks, Volume 16, Elsevier 2012, 2nd Edition.
2. H. te Nijenhuis et al., Z. Kristallogr. Suppl. 2009, 30. 163.
3. C. A. Reiss et al., Z. Kristallogr. 2012, 227, 257.
4. M. Sommariva, Solid State Phenomena 2013, 203- 204, 17.
5. E. Talaie et al., Energy Environ. Sci. 2015, 8, 2512.
6. D. Umeyama et al., Chem. Comm. 2015, 51, 12728.
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