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Surface Analysis with FT-IR Emission Spectroscopy

Volume 46, Number 5 (May 1992) Page 811-818

Sullivan, David H.; Conner, W. Curtis; Harold, Michael P.

The technique of infrared emission spectroscopy (IRES) is reviewed and further examined in this study as a surface analysis tool. A system has been designed which allows simultaneous kinetic and in situ infrared emission analysis of catalyst surfaces. IRES spectra of several gas mixture/solid systems are obtained in order to examine sample preparation and spectra processing issues; these systems include Pt/Al2O3 exposed to CO and CO-NO mixtures, an oxidized copper plate, and a zeolite exposed to inert atmospheres. For the temperature range of importance to catalysis (300-600 K), IRES is limited to frequencies less than 2500 cm−1. However, IRES is especially well suited for studying solid-state vibrational modes (<1000 cm−1). Moreover, IRES allows catalyst samples to be studied without dilution or extensive sample preparation. The thin samples required for IRES make it possible to study both surface adsorbate and the solid-state lattice vibrations simultaneously. This information can provide useful insight into the interpretation of kinetic data of reactions on metal oxide catalysts. However, samples which are too thick or are supported on a high-emissivity surface will not yield satisfactory spectra. Two correction techniques are examined which reduce background and sample-reflectance effects in the emission spectra. Some of the IRES data are compared to the corresponding spectra obtained by transmission and diffuse-reflectance spectroscopy. IRES is shown to be competitive with these more popular techniques for IR surface analysis.