Experimental
Homemade surface setup available at IRCELYON
An ultrahigh vacuum (UHV) chamber allows to prepare (Ar ion sputtering and annealing) and characterize (Auger electron spectroscopy, AES and low energy electron diffraction, LEED) single-crystal surfaces.
A static catalytic reactor (volume 120 cm3, pressure up to 1 atm) with IR laser heating is coupled to the UHV chamber (see picture). The reaction kinetics is followed by mass spectrometry and gas chromatography. This reactor can be used both with crystals and powder-supported catalysts.
The combination of the heating device (in the UHV chamber) and the mass spectrometer allows us to perform thermodesorption spectroscopy (TDS, TPD, TPRS...) with supported catalysts under UHV.
Pictures of the experimental setup. (a) General view of the UHV chambers. The reactor is at the rear, right-hand side. (b) Gas handling system. (c) Catalytic cell with IR laser and UV diode. The diode can be replaced with a pyrometer head. (d) Gas sampling systems for MS and GC analyses.
See Rev. Sci. Instrum. 2013, 84, 094101
Example of application: Sci. Technol. Adv. Mater. 2019, 20, 557
Infrared spectroscopy apparatus
The infrared spectrometer (Thermo Nicolet 6700) is equiped with two compartments for in situ transmission CO-FTIR under low P and T (glass cell, DTGS detector), and operando DRIFTS under gas flow (Harrick cell, MCT detector).
Picture showing the two IR benches and the gas handling system.
Example of application: ACS Catal. 2019, 9, 5752
High-pressure flow fixed bed reactor for CO2 hydrogenation
Example of application: Green Chemistry 2021, 23, 7259
Other techniques of interest
Electron microscopies (HR-TEM/STEM/ETEM...)
In situ/operando X-ray techniques (XAS, XRD...)
Surface techniques (STM, XPS, LEIS...)
Product analysis techniques (GCxGC-MS...)
Theoretical methods (DFT...)