Browsing by Subject "X-ray diffraction"

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  • Suuronen, Jussi-Petteri; Kallonen, Aki Petteri; Hänninen, Ville; Blomberg, Merja; Hämäläinen, Keijo; Serimaa, Ritva (2014)
    This article describes a novel experimental setup that combines X-ray microtomography (XMT) scans with in situ X-ray scattering experiments in a laboratory setting. Combining these two methods allows the characterization of both the micrometre-scale morphology and the crystallographic properties of the sample without removing it from the setup. Precise control of the position of the sample allows an accurate choice of the scattering beam path through the sample and facilitates the performance of X-ray scattering experiments on submillimetre-sized samples. With the present setup, a voxel size of less than 0.5 mm is achievable in the XMT images, and scattering experiments can be carried out with a beam size of approximately 200 200 mm. The potential of this setup is illustrated with the analysis of micrometeorite crystal structure and diffraction tomographic imaging of a silver behenate phantom as example applications.
  • Ahvenainen, Patrik; Kontro, Inkeri; Svedström, Kirsi (2016)
    Cellulose crystallinity assessment is important for optimizing the yield of cellulose products, such as bioethanol. X-ray diffraction is often used for this purpose for its perceived robustness and availability. In this work, the five most common analysis methods (the Segal peak height method and those based on peak fitting and/or amorphous standards) are critically reviewed and compared to two-dimensional Rietveld refinement. A larger () and more varied collection of samples than previous studies have presented is used. In particular, samples () with low crystallinity and small crystallite sizes are included. A good linear correlation () between the five most common methods suggests that they agree on large-scale crystallinity differences between samples. For small crystallinity differences, however, correlation was not seen for samples that were from distinct sample sets. The least-squares fitting using an amorphous standard shows the smallest crystallite size dependence and this method combined with perpendicular transmission geometry also yielded values closest to independently obtained cellulose crystallinity values. On the other hand, these values are too low according to the Rietveld refinement. All analysis methods have weaknesses that should be considered when assessing differences in sample crystallinity.
  • Boden, Pit; Di Martino-Fumo, Patrick; Busch, Jasmin M.; Rehak, Florian R.; Steiger, Sophie; Fuhr, Oliver; Nieger, Martin; Volz, Daniel; Klopper, Willem; Bräse, Stefan; Gerhards, Markus (2021)
    To develop new and flexible Cu-I containing luminescent substances, we extend our previous investigations on two metal-centered species to four metal-centered complexes. These complexes could be a basis for designing new organic light-emitting diode (OLED) relevant species. Both the synthesis and in-depth spectroscopic analysis, combined with high-level theoretical calculations are presented on a series of tetranuclear Cu-I complexes with a halide containing Cu4X4 core (X=iodide, bromide or chloride) and two 2-(diphenylphosphino)pyridine bridging ligands with a methyl group in para (4-Me) or ortho (6-Me) position of the pyridine ring. The structure of the electronic ground state is characterized by X-ray diffraction, NMR, and IR spectroscopy with the support of theoretical calculations. In contrast to the para system, the complexes with ortho-substituted bridging ligands show a remarkable and reversible temperature-dependent dual phosphorescence. Here, we combine for the first time the luminescence thermochromism with time-resolved FTIR spectroscopy. Thus, we receive experimental data on the structures of the two triplet states involved in the luminescence thermochromism. The transient IR spectra of the underlying triplet metal/halide-to-ligand charge transfer (M-3/XLCT) and cluster-centered ((CC)-C-3) states were obtained and interpreted by comparison with calculated vibrational spectra. The systematic and significant dependence of the bridging halides was analyzed.