[Solid/liquid interfacial in situ IR microscope and step-scan time-resolved FTIR spectroscopy and applications in...

Electrochemical in situ microscope IR reflection spectroscopy and step-scan time-resolved FTIR reflection spectroscopy were established by using an IR-plan advantage microscope and a Nexus 870 FTIR instrument, and a home-made signal synchronizer that harmonizes electrode polarization potential and step-scan spectral data collection sequence. These new techniques have been applied in studies of particular IR properties of 2-dimensional nanomaterials. By applying a treatment of fast potential cycling with different time (tau), a set of nanostructured Pt microelectrodes were prepared. CO adsorption was employed as a probe reaction together with in situ developed microscope FTIR spectroscopy. The results illustrated the variation of abnormal IR features with the nanostructure and the thickness (i.e., the size) of film formed on Pt microelectrode, i.e., following the increase of tau in fast potential cycling treatment, the direction of CO band was turned from absorption to antiabsorption direction, and the intensity and the width of CO band were increased. By taking the advantage of the abnormal infrared effects of nanostructured Pt microelectrode, the sensitivity of in situ IR reflection spectroscopy has been significantly improved, and spectra of time-resolution as fast as 50 micros have been recorded at solid/liquid interfaces. The current studies demonstrated not only the success of development of new techniques of in situ IR spectroscopy, but also the exploitation of the established techniques in studies of nanomaterials.