Combined Operando X-ray Diffraction/Raman Spectroscopy of Catalytic Solids in the Laboratory: The Co/TiO2Fischer-Tropsch Synthesis Catalyst Showcase.
A novel laboratory setup for combined operando X-ray diffraction and Raman spectroscopy of catalytic solids with online product analysis by gas chromatography is presented. The setup can be used with a laboratory-based X-ray source, which results in important advantages in terms of time-on-stream that can be measured, compared to synchrotron-based experiments. The data quality was much improved by the use of a relatively high-energy MoKαradiation instead of the more conventional CuKαradiation. We have applied the instrument to study the long-term deactivation of Co/TiO2Fischer-Tropsch synthesis (FTS) catalysts. No sign of Co sintering or bulk oxidation was found during the experiments. However, part of the metallic Co was converted into cobalt carbide (Co2C), at elevated pressure (10 bar). Furthermore, graphitic-like coke species are clearly formed during FTS at atmospheric pressure, whereas at elevated pressure fluorescence hampered the interpretation of the measured Raman spectra.
Inorganic Chemistry and Catalysis Debye Institute for Nanomaterials Science Utrecht University Universiteitslaan 99 3584 CG Utrecht The Netherlands.
Korneel H
KH
Cats
Inorganic Chemistry and Catalysis Debye Institute for Nanomaterials Science Utrecht University Universiteitslaan 99 3584 CG Utrecht The Netherlands.
Bert M
BM
Weckhuysen
Fischer-Tropsch synthesis; Raman spectroscopy; X-ray diffraction; carbon; cobalt