A 5 wt% Pd/SiO2 catalyst was synthesized by heating PdCl2-impregnated SiO2 in H2 at 300°C for 2 h. It was found that the metal particle dispersion is improved when the reduction step is preceded by calcination
at 300°C for 2h. Thermogravimetry of the impregnated support in air, N2 and H2 atmospheres was used to monitor the interactions occurring during the various preparative steps (i.e. drying, calcination
and reduction) of the catalyst. The solid prduct of each preparative step was characterized by X-ray diffractometry and UV/Vis
diffuse reflectance spectroscopy. The results indicate that following the drying step (at 110°C in air) the palladium occurs
in two detectable forms: PdCl2 particles and Si−O−Pdn+ surface species. The calcination appears to transform the PdCl2 particles into the latter surface species. The H2-reduction eventually converts the surface species into finely-dispersed Pd° metal particles (average size=8–14 nm). No other
reduction products, such as PdySix, were detected.