Adding diffuse reflectance infrared Fourier transform spectroscopy capability to extended x-ray-absorption fine structure in a new cell to study solid catalysts in combination with a modulation approach

Journal Article · Tue Jul 15 00:00:00 EDT 2014 · Review of Scientific Instruments

DOI:https://doi.org/10.1063/1.4890668· OSTI ID:22308685

Chiarello, Gian Luca ^[1]; Nachtegaal, Maarten; Marchionni, Valentina; Quaroni, Luca; Ferri, Davide ^[2]

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1. Dipartimento di Chimica, Università degli Studi di Milano, Via C. Golgi 19, I-20133 Milano, Italy and Empa, Swiss Federal Laboratories for Materials Science and Technology, Lab. for Solid State Chemistry and Catalysis, Ueberlandstrasse 129, CH-8600 Dübendorf (Switzerland)
2. Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland)

We describe a novel cell used to combine in situ transmission X-ray absorption spectroscopy (XAS) with diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) in a single experiment. The novelty of the cell design compared to current examples is that both radiations are passed through an X-ray and IR transparent window in direct contact with the sample. This innovative geometry also offers a wide surface for IR collection. In order to avoid interference from the crystalline IR transparent materials (e.g., CaF{sub 2}, MgF{sub 2}, diamond) a 500 μm carbon filled hole is laser drilled in the center of a CaF{sub 2} window. The cell is designed to represent a plug flow reactor, has reduced dead volume in order to allow for fast exchange of gases and is therefore suitable for experiments under fast transients, e.g., according to the concentration modulation approach. High quality time-resolved XAS and DRIFTS data of a 2 wt.% Pt/Al{sub 2}O{sub 3} catalyst are obtained in concentration modulation experiments where CO (or H{sub 2}) pulses are alternated to O{sub 2} pulses at 150 °C. We show that additional information can be obtained on the Pt redox dynamic under working conditions thanks to the improved sensitivity given by the modulation approach followed by Phase Sensitive Detection (PSD) analysis. It is anticipated that the design of the novel cell is likely suitable for a number of other in situ spectroscopic and diffraction methods.

• OSTI ID: 22308685
• Journal Information: Review of Scientific Instruments, Vol. 85, Issue 7; Other Information: (c) 2014 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA); ISSN 0034-6748
• Country of Publication: United States
• Language: English

Related Subjects

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY
ABSORPTION SPECTROSCOPY
ABUNDANCE
ALUMINIUM OXIDES
CARBON MONOXIDE
CATALYSTS
CRYSTALS
DIAMONDS
DIFFRACTION METHODS
FINE STRUCTURE
FOURIER TRANSFORM SPECTROMETERS
GASES
HYDROGEN
INFRARED RADIATION
MAGNESIUM FLUORIDES
OXYGEN
PULSES
SENSITIVITY
TIME RESOLUTION
WORKING CONDITIONS
X-RAY SPECTROSCOPY