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Oxidation of CO over Co₃O₄ at ambient temperature was studied with flow reactor experiments, and in-situ spectroscopic and structural methods. The catalyst deactivates during the reaction. The rate of deactivation increased with increasing CO or CO₂ gas-phase concentration but decreased with increased O₂ concentration or increased temperature. Regeneration of the catalyst in 10% O₂/Ar was more efficient than regeneration in Ar alone. The presence of carbonates and surface carbon on the deactivated catalyst was concluded from TPO experiments. None of these species could, however, be correlated with the deactivation of the catalyst. In-situ FTIR showed the presence of surface carbonates, carbonyl, and oxygen species. The change in structure and oxidation state of the catalyst was studied by in-situ XRD, in-situ XANES, XPS, and flow reactor experiments. One possible explanation for the deactivation of …