Applications of in-situ wide spectral range infrared absorption spectroscopy for CO oxidation over Pd/SiO2 and Cu/SiO2 catalysts

doi:10.1016/S1872-2067(21)64054-8

Abstract

Abstract:

Infrared (IR) absorption spectroscopy has been widely used for dynamic characterization of catalysts and mechanism of catalytic reactions. However, due to the strong infrared absorption of heterogeneous catalysts (mainly oxides, or supported metal and metal oxides, etc.) below 1200 cm^-1, and the intensity of regular infrared light source rapidly decays at low-wavenumber range, most in-situ infrared spectroscopy studies are limited to the detection of surface adsorbates in the range of 4000-900 cm^-1. The change of catalytically active component itself (M-O, M-M bond, etc., 1200-50 cm^-1) during the reaction is hard to be tracked under reaction conditions by in-situ IR. In this work, a home-made in-situ IR reactor was designed and a sample preparing method was developed. With such progresses, the changes of reactants, products, surface adsorbates, and catalysts themselves can be measured under the same reaction conditions with a spectral range of 4000-400 cm^-1, providing a new opportunity for in-situ characterization of heterogeneous catalysis. CO oxidation on Pd/SiO₂ and Cu/SiO₂ catalysts were taken as examples, since both the two catalytic systems were extensively used commercially, and moreover reduction and oxidation of palladium and copper occur during the examined reaction conditions. The characteristic bands of Pd²⁺-O (670, 608 cm^-1), Cu⁺-O (635 cm^-1) and Cu²⁺-O (595, 535 cm^-1) were observed by IR, and the changes during CO oxidation reaction were successfully monitored by IR. The oxidation/reduction of palladium and copper were also confirmed by ex-situ XPS. Moreover, Pd⁰ in Pd/SiO₂ and Cu⁺ in Cu/SiO₂ were found as the thermal dynamically stable phases under the examined conditions for CO oxidation.

Key words: In-situ infrared spectroscopy, X-ray photoelectron spectroscopy, Heterogeneous catalysis, CO oxidation, Palladium, Copper

Xuefei Weng, Shuangli Yang, Ding Ding, Mingshu Chen, Huilin Wan. Applications of in-situ wide spectral range infrared absorption spectroscopy for CO oxidation over Pd/SiO₂ and Cu/SiO₂ catalysts[J]. Chinese Journal of Catalysis, 2022, 43(8): 2001-2009.

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Figures/Tables 7

Fig. 1. In-situ IR spectra for the Pd/SiO2 catalyst. (a) After exposing to 3 Torr O2 at 600 K. (b) Reduction of PdO by CO (5 Torr) at the indicated temperatures.

Fig. 2. XPS Pd 3d spectra for the Pd/SiO2 catalyst. (a) Oxidation in air (21% O2/N2). (b) Reduction in H2 at various temperatures. It was held for 30 min at each temperature.

Fig. 3. In-situ IR spectra of CO adsorption on the pre-oxidized PdO/SiO2 catalyst as a function of the annealing temperature with p(CO) = 0.3 Torr. All spectra were acquired at 150 K, except the black one (in 0.01 Torr CO, 120 K).

Fig. 4. (a) In-situ IR spectra of CO oxidation over the pre-oxidized PdO/SiO2 catalyst. 5 Torr CO and 5 Torr O2 at RT (black), then flashed to 398 K for 2 min and cooled down to RT for the IR spectra acquiring. Six cycles were performed and the mixture gas was refilled for each cycle. (b) In-situ IR spectra of CO oxidation over the pre-reduced Pd/SiO2 catalyst, six cycles of reaction under 20 Torr mixture (CO/O2 = 4/3) at 423 K for 1 min were performed and the mixture gas was refilled for each cycle.

Fig. 5. (a) Oxidation of the pre-reduced Cu/SiO2 catalyst in 5 Torr O2 at the indicated temperatures for 10 min. (b) Reduction of the pre-oxidized CuO/SiO2 catalyst in 2 Torr H2 at the indicated temperatures for 10 min.

Fig. 6. The XPS spectra of Cu 2p (a) and Cu LMM (b) of the Cu/SiO2 catalyst during oxidation in 21%O2/N2 and reduction in 5%H2/Ar at the indicated temperatures. The sample was held at each temperature for 30 min.

Fig. 7. In-situ IR spectra of CO oxidation on the pre-reduced (a) and pre-oxidized (b) Cu/SiO2 catalyst at the indicated temperatures. 0.5 Torr CO and 0.5 Torr O2 at each temperature for 5 min.

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Applications of in-situ wide spectral range infrared absorption spectroscopy for CO oxidation over Pd/SiO₂ and Cu/SiO₂ catalysts

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