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Combined Operando X‐ray Diffraction/Raman Spectroscopy of Catalytic Solids in the Laboratory: The Co/TiO 2 Fischer–Tropsch Synthesis Catalyst Showcase
Author(s) -
Cats Korneel H.,
Weckhuysen Bert M.
Publication year - 2016
Publication title -
chemcatchem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.497
H-Index - 106
eISSN - 1867-3899
pISSN - 1867-3880
DOI - 10.1002/cctc.201600074
Subject(s) - raman spectroscopy , fischer–tropsch process , catalysis , synchrotron radiation , analytical chemistry (journal) , materials science , carbide , spectroscopy , synchrotron , cobalt , diffraction , chemistry , chemical engineering , optics , organic chemistry , selectivity , metallurgy , physics , quantum mechanics , engineering
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 MoK α radiation instead of the more conventional CuK α radiation. We have applied the instrument to study the long‐term deactivation of Co/TiO 2 Fischer–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 (Co 2 C), 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.