<i>In Situ</i> IR Characterization of CO Interacting with Rh Nanoparticles Obtained by Calcination and Reduction of Hydrotalcite‐Type Precursors

Abstract

Supported Rh nanoparticles obtained by reduction in hydrogen of severely calcined Rh/Mg/Al hydrotalcite‐type (HT) phases have been characterized by FT‐IR spectroscopy of adsorbed CO [both at room temperature (r.t.) and nominal liquid nitrogen temperature] and Transmission Electron Microscopy (TEM). The effect of reducing temperature has been investigated, showing that Rh crystal size increases from 1.4 nm to 1.8 nm when the reduction temperature increases from 750°C to 950°C. The crystal growth favours the formation of bridged CO species and linear monocarbonyl species with respect to gem ‐dicarbonyl species; when CO adsorbs at r.t., CO disproportionation occurs on Rh and it accompanies the formation of Rh I (CO) 2 . The role of interlayer anions in the HT precursors to affect the properties of the final materials has been also investigated considering samples prepared from silicate‐instead of carbonate‐containing precursors. In this case, formation of Rh I (CO) 2 and CO disproportionation do not occur, and this evidence is discussed in terms of support effect.