Versatile, Low-Volume, Thin-Layer Cell for in Situ Spectroelectrochemistry

Abstract

The design of a versatile, thin-layer cell to perform in situ spectroelectrochemistry is discussed. The cell is lowvolume, leak-tight, and easily disassembled. It is constructed of chemically resistant materials and can be used to probe the electrochemical reactions of corrosives as well as moisture-and air-sensitive materials. The use of this cell to monitor the electrochemical reactions of oxyhalide electrolytes by in situ infrared spectroelectrochemistry and pyridine by surface-enhanced Raman scattering spectroscopy is demonstrated.

Surface Raman Spectroscopy

“…Information on the behavior of the surface metal oxide species during catalytic reactions has been provided by in situ characterization studies [14] . Investigations of synergistic effects were performed on 18 O -exchange and the reoxidation of SbO x -O 3 physical mixtures. In this case, peroxide species were detected on working methanecoupling catalysts at temperatures up to 1070 K, and identifi ed as centers for the activation of methane [15] .…”

“…Special cells for SERS spectroelectrochemistry have been manufactured from chemically resistant materials, and with a working electrode accessible to the laser radiation. The versatility of such a cell has been demonstrated in electrochemical reactions of corrosive, moisture -sensitive materials such as oxyhalide electrolytes [18] . Langmuir -Blodgett ( LB ) fi lms and self -assembled monolayer s ( SAM s) deposited on metal surfaces have been studied using SERS spectroscopy in several investigations.…”

A low temperature in situ infrared reflected absorbance spectroelectrochemical (LT IRRAS) cell

“…Meanwhile, a variety of IR spectroelectrochemical cells, which extended the use of this technique, have been developed for the demands of in situ FTIR spectroelectrochemical studies [3][4][5][6][7].…”

“…The external reflection method which usually depends on specular reflectance on smooth electrode surfaces is used most widely for in situ infrared spectroelectrochemistry, since it is convenient to determine both adsorbate and solution species involved in electrochemical reactions, and a wide varieties of electrodes can be employed to study, such as massive materials and metal single crystal electrodes [12,21,24]. Some external IR reflection absorbance spectroelectrochemical cells have also been reported in the literature [4][5][6]21,[24][25][26][27][28].…”

“…A variety of IR RAS cells have been developed for in situ FTIR spectroelectrochemical experiments, but most of them were only fit for room temperature [4,5,28,30]. However, there are many electrode products which unstable at room temperature.…”