In situ observation of phase changes of a silica-supported cobalt catalyst for the Fischer–Tropsch process by the development of a synchrotron-compatible in situ/operando powder X-ray diffraction cell

Abstract

In situ characterization of catalysts gives direct insight into the working state of the material. Here, the design and performance characteristics of a universal in situ synchrotron-compatible X-ray diffraction cell capable of operation at high temperature and high pressure, 1373 K, and 35 bar, respectively, are reported. Its performance is demonstrated by characterizing a cobalt-based catalyst used in a prototypical high-pressure catalytic reaction, the Fischer-Tropsch synthesis, using X-ray diffraction. Cobalt nanoparticles supported on silica were studied in situ during Fischer-Tropsch catalysis using syngas, H 2 and CO, at 723 K and 20 bar. Post reaction, the Co nanoparticles were carburized at elevated pressure, demonstrating an increased rate of carburization compared with atmospheric studies.

Role of Co2C in ZnO‐promoted Co Catalysts for Alcohol Synthesis from Syngas

“…An XRD scan was acquired every 2 minutes during the reduction and every 10 minutes during measurements at reaction conditions. Samples were contained within a custom reactor as previously described . Samples were packed in glass capillaries between two plugs of quartz wool.…”

Reversing the Irreversible: Thermodynamic Stabilization of Lithium Aluminum Hydride Nanoconfined Within a Nitrogen-Doped Carbon Host

“…SAXS/WAXS measurements were conducted at SSRL beam line 1-5 with λ = 0.7999 Å incident energy and a 1 m sample-to-detector distance. Samples were prepared in ø 1.0 mm quartz capillaries with 10 µm thick walls in an Ar glovebox and connected to a heating cell 40 with Swagelok compression ttings. A type K thermocouple was inserted into the capillary to monitor sample temperature.…”

Impurity Control in Catalyst Design: The Role of Sodium in Promoting and Stabilizing Co and Co2C for Syngas Conversion

“…The catalyst bed was held in place by two plugs of quartz wool, and a K‐type thermocouple was inserted into the capillary and positioned against the powder bed to monitor the temperature. The capillary was loaded into a custom‐built high temperature and pressure reactor described previously [31] . Gas flow rates were controlled using mass flow controllers (Brooks) and metal carbonyls were removed from the CO feed with a Nanochem Metal‐X purifier (Matheson).…”