A New DRIFTS Cell for theIn-Situ Investigation of Heterogeneously Catalyzed Reactions

Drochner, Alfons; Fehlings, Michael G.; Krauß, Kai; Vogel, Herbert

doi:10.1002/(sici)1521-4125(200004)23:4<319::aid-ceat319>3.0.co;2-4

Cited by 33 publications

(15 citation statements)

References 6 publications

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“…In recent years, extensive applications of IR spectroscopy were witnessed in exploring various interfacial phenomena in electrochemical CO 2 RR, which features the low cost, facile optical design and operation, simple surface selection rule, and broad applicability to electrodes [34]. Four major configurations are accessible to in situ IR spectroscopy measurement: transmission [35], diffuse reflectance (DRIFTS) [36], reflection-absorption (RAS-IR), and attenuated total reflection (ATR-IR). Osawa and co-workers combined ATR-IR geometry with surface-enhancement of the IR absorption (SEIRA) [37][38][39][40].…”

Section: Infrared Spectroscopy (Ir)mentioning

confidence: 99%

In Situ Spectroscopic Methods for Electrocatalytic CO2 Reduction

Liu

Seifitokaldani

2020

Catalysts

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Electrochemical reduction of CO2 to value-added chemicals and fuels is a promising approach to store renewable energy while closing the anthropogenic carbon cycle. Despite significant advances in developing new electrocatalysts, this system still lacks enough energy conversion efficiency to become a viable technology for industrial applications. To develop an active and selective electrocatalyst and engineer the reaction environment to achieve high energy conversion efficiency, we need to improve our knowledge of the reaction mechanism and material structure under reaction conditions. In situ spectroscopies are among the most powerful tools which enable measurements of the system under real conditions. These methods provide information about reaction intermediates and possible reaction pathways, electrocatalyst structure and active sites, as well as the effect of the reaction environment on products distribution. This review aims to highlight the utilization of in situ spectroscopic methods that enhance our understanding of the CO2 reduction reaction. Infrared, Raman, X-ray absorption, X-ray photoelectron, and mass spectroscopies are discussed here. The critical challenges associated with current state-of-the-art systems are identified and insights on emerging prospects are discussed.

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Section: Infrared Spectroscopy (Ir)mentioning

confidence: 99%

In Situ Spectroscopic Methods for Electrocatalytic CO2 Reduction

Liu

Seifitokaldani

2020

Catalysts

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“…In this report, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) [26,27] is employed to elucidate the active phase of IrO 2 @TiO 2 by utilizing CO as a probe molecule. In doing so, we first prepare fully oxidized and fully reduced catalysts whose DRIFT spectra serve as reference spectra for the subsequent interpretation of operando CO spectra acquired during CO oxidation -a well-documented model reaction for oxidation catalysis [28] -under various reaction conditions.…”

Section: Introductionmentioning

confidence: 99%

Operando CO Infrared Spectroscopy and On-Line Mass Spectrometry for Studying the Active Phase of IrO2 in the Catalytic CO Oxidation Reaction

et al. 2023

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We combine operando diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) with on-line mass spectrometry (MS) to study the correlation between the oxidation state of titania-supported IrO2 catalysts (IrO2@TiO2) and their catalytic activity in the prototypical CO oxidation reaction. Here, the stretching vibration of adsorbed COad serves as the probe. DRIFTS provides information on both surface and gas phase species. Partially reduced IrO2 is shown to be significantly more active than its fully oxidized counterpart, with onset and full conversion temperatures being about 50 °C lower for reduced IrO2. By operando DRIFTS, this increase in activity is traced to a partially reduced state of the catalysts, as evidenced by a broad IR band of adsorbed CO reaching from 2080 to 1800 cm−1.

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“…Although we know from the corresponding UHV studies that under these conditions CO species adsorbed at the surface of ceria nanoparticles must be present, in the raw data these adsorbate vibrations are almost completely obscured by the intense gas-phase signals. The situation is improved by recording reference spectra for KBr powders 37 (Figure 1b), a material where under these conditions (295 K, 1 bar CO) the amount of CO adsorbed on the surface is negligibly small. 38 We find that in the difference spectra obtained by first normalizing the spectra in the frequency regime between 2080 and 2040 cm −1 and then subtracting the KBr reference data from the ceria data, vibrational bands arising from CO adsorbed on ceria surfaces can be clearly identified (Figure 2).…”

Section: Resultsmentioning

confidence: 99%

Bridging the Pressure and Materials Gap in Heterogeneous Catalysis: A Combined UHV, In Situ, and Operando Study Using Infrared Spectroscopy

Caulfield,

Sauter,

Idriss

et al. 2023

J. Phys. Chem. C

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The interactions of gas molecules with metal oxides used as catalysts or support materials in heterogeneous catalysis are highly intriguing. It is of great importance to gain detailed insight into the complex and often dynamic behavior of oxide particles under operando conditions. In this study, the understanding of CO interactions with cerium oxide surfaces is advanced by bridging the so-called materials and pressure gaps. This is accomplished by studying the influence of different types of materials, pressures, and temperatures by using different infrared spectroscopies as the primary investigation tool. Whereas low-temperature CO adsorption (<80 K) on various well-defined CeO2 single crystal surfaces yields distinct vibrational bands that can be assigned to different adsorption sites on fully stoichiometric and also on reduced surfaces using validated ab initio calculations, strong gas-phase contributions turn the interpretation of results obtained for powders under operando conditions into a major challenge. By using a combination of UHV-IRRAS, in situ transmission infrared spectroscopy, and operando DRIFTS measurements, the reference data obtained for single-crystal surfaces under UHV conditions could be used to assign the features observed in spectra obtained for powder materials. In the next step, the different CO vibrational bands were used to monitor surface structural changes occurring at elevated pressures and temperatures. An increase in the concentration of Ce3+ species as a result of CO-induced reduction could be directly demonstrated even at low (300 K) temperatures. Our results demonstrate important progress toward the noninvasive, nondestructive characterization of real catalysts under operando conditions.

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A New DRIFTS Cell for theIn-Situ Investigation of Heterogeneously Catalyzed Reactions

Cited by 33 publications

References 6 publications

In Situ Spectroscopic Methods for Electrocatalytic CO2 Reduction

In Situ Spectroscopic Methods for Electrocatalytic CO2 Reduction

Operando CO Infrared Spectroscopy and On-Line Mass Spectrometry for Studying the Active Phase of IrO2 in the Catalytic CO Oxidation Reaction

Bridging the Pressure and Materials Gap in Heterogeneous Catalysis: A Combined UHV, In Situ, and Operando Study Using Infrared Spectroscopy

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