Laboratory setup for rapid in situ powder X-ray diffraction elucidating Ni particle formation in supercritical methanol
| Autor: | Jakob Voldum Ahlburg, Frederik Holm Gjørup, Mogens Christensen |
|---|---|
| Rok vydání: | 2019 |
| Předmět: |
010302 applied physics
Materials science Rietveld refinement Analytical chemistry chemistry.chemical_element Atmospheric temperature range 01 natural sciences Supercritical fluid 010305 fluids & plasmas Nickel chemistry 0103 physical sciences X-ray crystallography Particle Instrumentation Powder diffraction Diffractometer |
| Zdroj: | H. Gjørup, F, Ahlburg, J V & Christensen, M 2019, ' Laboratory setup for rapid in situ powder X-ray diffraction elucidating Ni particle formation in supercritical methanol ', Review of Scientific Instruments, vol. 90, no. 7, 073902, pp. 073902 . https://doi.org/10.1063/1.5089592 |
| ISSN: | 1089-7623 0034-6748 |
| DOI: | 10.1063/1.5089592 |
| Popis: | The design and function of a custom-made Soller slit for a laboratory 2D area detector is presented through a series of demonstration imagesand an in situ experiment following the formation of nickel particles in supercritical methanol. The in situ experiment is performed in acapillary sample environment, modified for a laboratory scale Rigaku Smartlab diffractometer, and with a temperature range of 300–1050 K.The formation of nickel particles was followed successfully using laboratory in situ X-ray powder diffraction with a time resolution in the orderof 27 s. Observations from the area detector images showed the appearance of three distinct phases during the reaction: Ni3(NO3)2(OH)4,NiO, and Ni. The images were linearly integrated and analyzed using Rietveld refinement. A reaction mechanism is proposed based on anevaluation of the weight fractions and scattering factors as a function of reaction time. |
| Databáze: | OpenAIRE |
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