The characterization of the Cu +/ZSM-5 catalysts prepared via reduction of ion-exchanged Cu 2+/ZSM-5 samples and highly dispersed Ti-oxide catalysts anchored on Vycor glass has been undertaken by in-situ photoluminescence, EPR, XAPS (XANES and FT-EX-AFS), and FT-IR spectroscopy. UV-irradiation of the Cu +/ZSM-S catalyst in the presence of NO leads to the direct photocatalytic decomposition of NO into N 2 and O 2 at normal temperatures. UV-irradiation of the highly dispersed anchored Ti-oxide catalyst in the presence of CO 2 and H 2O also leads to the evolution of CH 4, CO, and CH 3OH at normal temperatures. The clarification of the coordination structure of the active surface sites and the direct detection of the reaction precursors and intermediate species in these photocatalytic systems contributed significantly in characterizing the molecular scale reaction mechanisms. Based on these results, the design of highly concentrated and efficient photocatalysts has successfully been achieved by application of the sol-gel method.
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