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Scanning Tunneling Microscopy at Elevated Pressure

Operando Observations of Model Catalysts

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In-situ Materials Characterization

Part of the book series: Springer Series in Materials Science ((SSMATERIALS,volume 193))

Abstract

Advanced experiments and theory make it increasingly clear that there can be essential differences between the behavior of catalysts under actual operation conditions and under the (near)-vacuum conditions of traditional laboratory experiments and total-energy calculations. These differences involve the structure, morphology, composition, reaction mechanisms and, importantly, the activity and selectivity of the catalyst. This forces us to cross the ‘pressure gap ’ with new instruments and adapted versions of existing experimental techniques. This chapter focuses on the development of dedicated scanning probe microscopy for operando observations of active model catalysts. The combination is advocated of an uncompromised, ultrahigh vacuum environment for the preparation and traditional characterization of model catalyst samples with a high-pressure flow reactor cell, integrated with the essential components of a Scanning Tunneling Microscope (STM) or Atomic Force Microscope (AFM). With such a configuration it becomes possible to perform atomic-scale observations on well-defined model catalysts under fully controlled working conditions. These structural observations acquire further significance by being combined with time-resolved mass spectrometry measurements on the gas mixture that flows out of the reactor, allowing one not only to measure the influence of the gas mixture on the surface structure but also to correlate that structure with the catalytic performance. This chapter highlights some of the important design considerations for high-pressure scanning probe instruments and illustrates their performance with results obtained for catalytic oxidation and reduction reactions.

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Acknowledgments

This chapter would not have been possible without the work by many people. In particular, I would like to mention Kees Herbschleb, Dunja Stoltz, Marta Cañas-Ventura, Violeta Navarro-Paredes, Sander Roobol, Bas Hendriksen, Stefania Bobaru and Peter Rasmussen. A special thanks goes out to the technical support staff of Leiden University, in particular to Peter van der Tuijn who has been responsible for the design of the latest version of the ReactorSTM. I am indebted to Gertjan van Baarle and Alexei Ofitserov of Leiden Probe Microscopy B.V., who have combined the development of a commercial version of the ReactorSTM [58] with a significant role in the development of the prototype instruments in the author’s laboratory. This project is financially supported by a Netherlands SmartMix grant and the NIMIC partner organizations (http://NIMIC.Physics.LeidenUniv.nl) through NIMIC, a public–private program.

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  1. Kamerlingh Onnes Laboratory, Leiden University, Niels Bohrweg 2, 2333 CA, Leiden, The Netherlands

    Joost W. M. Frenken

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  1. Joost W. M. Frenken
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Editors and Affiliations

  1. Microscopy & Microanalysis Unit, The University of the Witwatersrand, Johannesburg, Germany

    Alexander Ziegler

  2. Photon-Science Detector Group, Deutsches Elektronen Synchrotron, Hamburg, Germany

    Heinz Graafsma

  3. Nanotechnology Systems Division, Hitachi High Technologies America, Inc., Pleasanton, California, USA

    Xiao Feng Zhang

  4. Leiden University Kamerlingh Onnes Laboratory, Leiden, The Netherlands

    Joost W.M. Frenken

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Frenken, J.W.M. (2014). Scanning Tunneling Microscopy at Elevated Pressure. In: Ziegler, A., Graafsma, H., Zhang, X., Frenken, J. (eds) In-situ Materials Characterization. Springer Series in Materials Science, vol 193. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-642-45152-2_6

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