The <i>ReactorAFM</i>: Non-contact atomic force microscope operating under high-pressure and high-temperature catalytic conditions

Roobol, S. B.; Cañas‐Ventura, Marta E.; Bergman, M.; Spronsen, Matthijs A. van; Onderwaater, Willem G.; Tuijn, P. C. van der; Koehler, Raymond; Ofitserov, A.; Baarle, G. J. C. van; Frenken, J.W.M.

doi:10.1063/1.4916194

Cited by 32 publications

(22 citation statements)

References 28 publications

(29 reference statements)

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“…These methods include the integration of a flow reactor with a scanning probe microscopy (SPM) system, [6][7][8] the application of differential pumping stages and electrostatic lenses in near-ambient-pressure (NAP) X-ray photoelectron spectroscopy (XPS), 9,10 the use of high-pressure vibrational spectroscopy, [11][12][13] and X-ray diffraction setups. 14,15 Simultaneously, theoretical modeling has matured by taking the energies derived from density functional theory (DFT) as input for thermodynamic calculations.…”

Section: Joost W M Frenkenmentioning

confidence: 99%

Surface science under reaction conditions: CO oxidation on Pt and Pd model catalysts

2017

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Platinum and palladium are frequently used as catalytic materials, for example for the oxidation of CO. This is one of the most widely studied reactions in the field of surface science. Although seemingly uncomplicated, it remains an active and interesting topic, which is partially explained by the push to conduct experiments on model systems under relevant reaction conditions. Recent developments in the surface-science methodology have allowed obtaining chemical and structural information on the active phase of model catalysts. Tools of the trade include near-ambient-pressure X-ray photoelectron spectroscopy, high-pressure scanning tunneling microscopy, high-pressure surface X-ray diffraction, and high-pressure vibrational spectroscopy. Interpretation is often aided by density functional theory in combination with thermodynamic and kinetic modeling. In this review, results for the catalytic oxidation of CO obtained by these techniques are compared. On several of the Pt and Pd surfaces, new structures develop in excess O 2 . For Pt, this requires a much larger excess of O 2 than for Pd. Most of these structures also develop in pure O 2 and are identified as (surface) oxides. A large body of evidence supports the conjecture that these oxides are more reactive than the corresponding O-covered metallic surfaces under similar conditions, although still debated in the literature. An outlook on this developing field, including directions that move away from CO oxidation towards more complex chemistry, concludes this review.

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Section: Joost W M Frenkenmentioning

confidence: 99%

Surface science under reaction conditions: CO oxidation on Pt and Pd model catalysts

2017

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“…For the AFM mode, we use the same electrical read-out circuit as the ReactorAFM. 9 A Zurich Instruments HF2LI lock-in amplifier is placed in the experimental hutch, close to the microscope. It is connected to the LPM control system via four 20 m long BNC cables carrying the relevant signals from the force sensor.…”

Section: Control Electronicsmentioning

confidence: 99%

“…Examples are Xray photoelectron spectroscopy (XPS), 1 X-ray scattering techniques, 2,3 transmission electron microscopy (TEM), 4,5 scanning tunneling microscopy (STM), [6][7][8] and atomic force microscopy (AFM), 9 which have been developed to investigate a wide array of relevant catalytic systems, ranging from single-crystal model catalysts to supported nanoparticles. Each of these techniques contributes only a specific component to our understanding of heterogeneous catalysis.…”

Section: Introductionmentioning

confidence: 99%

“…A complete view of the setup is presented in Figure 1. Our design is based on the ReactorSXRD setup 26 that has been developed previously at the ID03 beamline of the European Synchrotron Radiation Facility (ESRF) for in situ study of catalyst surfaces by surface X-ray diffraction 27 and on the ReactorSTM 7 and ReactorAFM 9 setups that have been developed earlier at Leiden University. It combines a UHV system for sample preparation procedures with a flow reactor in which gas pressures up to 1 bar and sample temperatures up to 1000…”

Section: Introductionmentioning

confidence: 99%

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Combined scanning probe microscopy and x-ray scattering instrument for in situ catalysis investigations

Onderwaater

Tuijn

Mom

et al. 2016

Review of Scientific Instruments

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We have developed a new instrument combining a scanning probe microscope (SPM) and an X-ray scattering platform for ambient-pressure catalysis studies. The two instruments are integrated with a flow reactor and an ultra-high vacuum system that can be mounted easily on the diffractometer at a synchrotron end station. This makes it possible to perform SPM and X-ray scattering experiments in the same instrument under identical conditions that are relevant for catalysis.

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“…Examples are transmission electron microscopy (TEM), 8 surface X-ray diffraction (SXRD), 9 scanning tunneling microscopy (STM), [10][11][12][13][14] and atomic force microscopy (AFM). 15 Scanning tunneling microscopy is one of the few atomically sensitive surface-science techniques that do not introduce fundamental problems or limitations when bridging the pressure gap. It can operate in the full range from UHV to high pressures of, e.g., 1 bar and beyond, and from cryogenic temperatures to temperatures well above 1000 K. 16,17 With its capability to image surfaces with atomic resolution, the STM holds the promise to determine the detailed dependence of the structure of model catalyst surfaces on various gas environments, to identify the active sites for catalytic reactions and to elucidate the role of possible promoters, all under the relevant, high-pressure, high-temperature conditions of the catalytic processes of interest.…”

Section: Introductionmentioning

confidence: 99%

The ReactorSTM: Atomically resolved scanning tunneling microscopy under high-pressure, high-temperature catalytic reaction conditions

Herbschleb

Tuijn

Roobol

et al. 2014

Review of Scientific Instruments

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A new scanning tunneling microscope reactor used for high-pressure and high-temperature catalysis studies Review of Scientific Instruments 79, 084101 (2008) To enable atomic-scale observations of model catalysts under conditions approaching those used by the chemical industry, we have developed a second generation, high-pressure, high-temperature scanning tunneling microscope (STM): the ReactorSTM. It consists of a compact STM scanner, of which the tip extends into a 0.5 ml reactor flow-cell, that is housed in a ultra-high vacuum (UHV) system. The STM can be operated from UHV to 6 bars and from room temperature up to 600 K. A gas mixing and analysis system optimized for fast response times allows us to directly correlate the surface structure observed by STM with reactivity measurements from a mass spectrometer. The in situ STM experiments can be combined with ex situ UHV sample preparation and analysis techniques, including ion bombardment, thin film deposition, low-energy electron diffraction and x-ray photoelectron spectroscopy.

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The ReactorAFM: Non-contact atomic force microscope operating under high-pressure and high-temperature catalytic conditions

Cited by 32 publications

References 28 publications

Surface science under reaction conditions: CO oxidation on Pt and Pd model catalysts

Surface science under reaction conditions: CO oxidation on Pt and Pd model catalysts

Combined scanning probe microscopy and x-ray scattering instrument for in situ catalysis investigations

The ReactorSTM: Atomically resolved scanning tunneling microscopy under high-pressure, high-temperature catalytic reaction conditions

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