Combined scanning probe microscopy and x-ray scattering instrument for <i>in situ</i> catalysis investigations

Onderwaater, Willem G.; Tuijn, P. C. van der; Mom, Rik V.; Spronsen, Matthijs A. van; Roobol, S. B.; Saedi, Amirmehdi; Drnec, Jakub; Isérn, H.; Carlà, Francesco; Dufrane, T.; Koehler, Raymond; Crama, Bert; Groot, Irene M. N.; Felici, Roberto; Frenken, J.W.M.

doi:10.1063/1.4968804

Cited by 12 publications

(16 citation statements)

References 32 publications

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“…Examples are the use of highenergy X-rays and larger detectors in SXRD, the development of the ReactorAFM to be able to study the structure and reactivity of bulk oxides too insulating to study with STM, 8 or the integration of X-ray scattering with SPM. 15 However, there is definitively a need for further instrument development, some of which will be very challenging, such as the full closure of the pressure gap in XPS. Some development should be more straightforward and is directed at combining several techniques to obtain different types of information on the same sample under identical conditions.…”

Section: Discussionmentioning

confidence: 99%

“…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. 16 In this way, theoretical predictions can be made regarding the most stable phase as a function of the reaction conditions.…”

Section: Joost W M Frenkenmentioning

confidence: 99%

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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: Discussionmentioning

confidence: 99%

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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“…In situ techniques, where active catalysts can be studied under working reaction conditions, including the detection of conversion, have been developed successfully for a range of different spatially resolved (Ackermann et al, 2005; Hendriksen et al, 2010; Chenna & Crozier, 2012; Vendelbo et al, 2014; Kudernatsch et al, 2015; Onderwaater et al, 2016), spectroscopic (Knop-Gericke et al, 2000; Topsøe, 2003; Bañares, 2005; Bukhtiyarov et al, 2006; Tinnemans et al, 2006; Bluhm et al, 2007; Salmeron & Schlögl, 2008; Bentrup, 2010; Horn et al, 2010; Gänzler et al, 2015; Velasco-Vélez et al, 2016) and diffractive techniques (Beale et al, 2010). Using these in situ techniques, changes in the bulk and surface structures under working conditions can be detected.…”

Section: Introductionmentioning

confidence: 99%

Versatile Homebuilt Gas Feed and Analysis System for Operando TEM of Catalysts at Work

et al. 2020

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Understanding how catalysts work during chemical reactions is crucial when developing efficient catalytic materials. The dynamic processes involved are extremely sensitive to changes in pressure, gas environment and temperature. Hence, there is a need for spatially resolved operando techniques to investigate catalysts under working conditions and over time. The use of dedicated operando techniques with added detection of catalytic conversion presents a unique opportunity to study the mechanisms underlying the catalytic reactions systematically. Herein, we report on the detailed setup and technical capabilities of a modular, homebuilt gas feed system directly coupled to a quadrupole mass spectrometer, which allows for operando transmission electron microscopy (TEM) studies of heterogeneous catalysts. The setup is compatible with conventional, commercially available gas cell TEM holders, making it widely accessible and reproducible by the community. In addition, the operando functionality of the setup was tested using CO oxidation over Pt nanoparticles.

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“…The emerging synchrotron X-ray scanning tunneling microscopy (SX-STM) technique combines the high spatial resolution of STM with the information obtained through X-ray/matter interaction. The technique takes advantage of the fact that X-ray excited electrons can modulate the tunneling current in STM leading to structural, elemental, electronic, and magnetic contrast with high spatial resolution (Saito et al, 2006;Chiu et al, 2008;Okuda et al, 2009;Cummings et al, 2012;Onderwaater et al, 2016). A specialized smart tip in close proximity to the sample surface serves as a detector for the X-ray enhanced tunneling current (Rose et al, 2011;Cummings et al, 2017).…”

Section: Introductionmentioning

confidence: 99%

XTIP – the world's first beamline dedicated to the synchrotron X-ray scanning tunneling microscopy technique

et al. 2020

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In recent years, there have been numerous efforts worldwide to develop the synchrotron X-ray scanning tunneling microscopy (SX-STM) technique. Here, the inauguration of XTIP, the world's first beamline fully dedicated to SX-STM, is reported. The XTIP beamline is located at Sector 4 of the Advanced Photon Source at Argonne National Laboratory. It features an insertion device that can provide left- or right-circular as well as horizontal- and vertical-linear polarization. XTIP delivers monochromatic soft X-rays of between 400 and 1900 eV focused into an environmental enclosure that houses the endstation instrument. This article discusses the beamline system design and its performance.

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

Cited by 12 publications

References 32 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

Versatile Homebuilt Gas Feed and Analysis System for Operando TEM of Catalysts at Work

XTIP – the world's first beamline dedicated to the synchrotron X-ray scanning tunneling microscopy technique

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