Simultaneous scanning tunneling microscopy and synchrotron X-ray measurements in a gas environment

Mom, Rik V.; Onderwaater, Willem G.; Rost, Marcel J.; Jankowski, Maciej; Wenzel, Sabine; Jacobse, Leon; Alkemade, P.F.A.; Vandalon, Vincent; Spronsen, Matthijs A. van; Weeren, Matthijs van; Crama, Bert; Tuijn, P. C. van der; Felici, Roberto; Kessels, W.M.M.; Carlà, Francesco; Frenken, J.W.M.; Groot, Irene M. N.

doi:10.1016/j.ultramic.2017.07.011

Cited by 8 publications

(13 citation statements)

References 37 publications

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“…In addition, in situ cleaving of samples is possible. Another SX-STM microscope has been developed and installed at the European Synchrotron Radiation Facility (ESRF) by Mom et al [18] and is used for high pressure (operando) measurements. The system comprises of a UHV chamber with a high-pressure cell/reactor on top and placed in a controlled gas atmosphere at pressures up to 1.1 bar.…”

Section: Results and Discussion Of Applications-sx-stm Spectroscopy mentioning

confidence: 99%

“…Typically, a complete endstation needs to be developed and installed at a given beamline. Since detection of SX-STM currents is associated with distinguishing between the actual tunneling current and a much larger photoelectron current, lock-in techniques are widely used to improve the signal-to-noise ratio [6,18,23]. Dedicated UHV compatible choppers along with topographic filters have been developed to modulate the incoming X-ray beam and provide a reference signal for the lock-in amplifiers (LIA) [26].…”

Section: Sx-stm Instrumentation and Methodsmentioning

confidence: 99%

“…Different approaches have been used to coat PtIr tips, which include boron nitride deposition (BN) or SiO 2 by e-beam deposition [7,12,13]. In the section below we review various approaches that have been developed and applied to fabrication of smart tips in the past five years [4,[14][15][16][17][18]].…”

Section: Smart Tipsmentioning

confidence: 99%

“…MIM tips have been used in a number of applications listed in Table 2, which provides an overview of various smart tips and their respective applications that have been used since 2014. Metal-Polymer coated Metal (MPM, PtIr-PV-Ti/Au) tips: Based on a method used to fabricate tips for electrochemical STM [25], polymer coated SX-STM tips have been developed [18]. An electrochemically etched 0.25 mm PtIr wire was pushed through a droplet of polyethylene-vinylacetate-based glue gun wax (PV) at 80 • C. The shield coating was applied by radiofrequency sputter deposition of a Ti seed layer followed by 100 nm Au for the polymer tips.…”

Section: Coaxially Shielded Stm Tipsmentioning

confidence: 99%

“…The coating thickness was not uniform, i.e., thicker in the middle of a tip (1 mm) and thinner at the apex (a few hundred nanometers). Atomic steps has been observed during STM imaging of Au(111) when using an MPM coaxial tip at 12.1 keV photon energy [18].…”

Section: Coaxially Shielded Stm Tipsmentioning

confidence: 99%

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X-ray Assisted Scanning Tunneling Microscopy and Its Applications for Materials Science: The First Results on Cu Doped ZrTe3

et al. 2019

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Synchrotron X-ray Scanning Tunneling Microscopy (SX-STM) is a novel imaging technique capable of providing real space chemically specific mapping with a potential of reaching atomic resolution. Determination of chemical composition along with ultra-high resolution imaging by SX-STM can be realized through excitation of core electrons by incident X-rays when their energy is tuned to an absorption edge of a particular atom during raster scanning, as is done in the conventional STM experiments. In this work, we provide a brief summary and the current status of SX-STM and discuss its applications for material science. In particular, we discuss instrumentation challenges associated with the SX-STM technique and present early experiments on Cu doped ZrTe3 single crystals.

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Section: Results and Discussion Of Applications-sx-stm Spectroscopy mentioning

confidence: 99%

Section: Sx-stm Instrumentation and Methodsmentioning

confidence: 99%

Section: Smart Tipsmentioning

confidence: 99%

Section: Coaxially Shielded Stm Tipsmentioning

confidence: 99%

Section: Coaxially Shielded Stm Tipsmentioning

confidence: 99%

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X-ray Assisted Scanning Tunneling Microscopy and Its Applications for Materials Science: The First Results on Cu Doped ZrTe3

et al. 2019

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Toward Precise Understanding of Catalytic Events and Materials Under Working Conditions

Urakawa

2021

Heterogeneous Catalysts

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Investigation of Active Catalysts at Work

Groot

2021

Acc. Chem. Res.

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Conspectus Even after being in business for at least the last 100 years, research into the field of (heterogeneous) catalysis is still vibrant, both in academia and in industry. One of the reasons for this is that around 90% of all chemicals and materials used in everyday life are produced employing catalysis. In 2020, the global catalyst market size reached $35 billion, and it is still steadily increasing every year. Additionally, catalysts will be the driving force behind the transition toward sustainable energy. However, even after having been investigated for 100 years, we still have not reached the holy grail of developing catalysts from rational design instead of from trial-and-error. There are two main reasons for this, indicated by the two so-called “gaps” between (academic) research and actual catalysis. The first one is the “pressure gap”, indicating the 13 orders of magnitude difference in pressure between the ultrahigh vacuum lab conditions and the atmospheric pressures (and higher) of industrial catalysis. The second one is the “materials gap”, indicating the difference in complexity between single-crystal model catalysts of academic research and the real catalysts, consisting of metallic nanoparticles on supports, promoters, fillers, and binders. Although over the past decades significant efforts have been made in closing these gaps, many steps still have to be taken. In this Account, I will discuss the steps we have taken at Leiden University to further our fundamental understanding of heterogeneous catalysis at the (near-)atomic scale. I will focus on bridging the pressure gap, though we are also working on closing the materials gap. Over the past years, we developed state-of-the-art equipment that is able to investigate the (near-)atomic-scale structure of the catalyst surface during the chemical reaction using several surface-science-based techniques such as scanning tunneling microscopy, atomic force microscopy, optical microscopy, and X-ray-based techniques (surface X-ray diffraction, grazing-incidence small-angle X-ray scattering, and X-ray reflectivity, in collaboration with ESRF). Simultaneously with imaging the surface, we can investigate the catalyst’s performance via mass spectrometry, enabling us to link changes in the catalyst structure to its activity, selectivity, or stability. Although we are currently investigating many industrially relevant catalytic systems, I will here focus the discussion on the oxidation of platinum during, for example, CO and NO oxidation, the NO reduction reaction on platinum, and the growth of graphene on liquid (molten) copper. I will show that to be able to obtain the full picture of heterogeneous catalysis, the ability to investigate the catalyst at the (near-)atomic scale during the chemical reaction is a must.

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Simultaneous scanning tunneling microscopy and synchrotron X-ray measurements in a gas environment

Cited by 8 publications

References 37 publications

X-ray Assisted Scanning Tunneling Microscopy and Its Applications for Materials Science: The First Results on Cu Doped ZrTe3

X-ray Assisted Scanning Tunneling Microscopy and Its Applications for Materials Science: The First Results on Cu Doped ZrTe3

Toward Precise Understanding of Catalytic Events and Materials Under Working Conditions

Investigation of Active Catalysts at Work

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