Abstract

Elucidating the atomic structure and chemistry of catalysts by correlative scanning photoemission electron microscopy and atom probe tomography.

Highlights

  • Prepared oxides of Ir–Ru are commonly used for catalysis applications, in particular to facilitate the anodic oxygen evolution reaction (OER) in proton exchange membrane water electrolysis (PEMWE) devices.[1]

  • The microscope collects spectra in a snapshot mode which substantially reduces the beam exposure time per pixel.[38]. This prevents radiation damage on the sample's surface that may occur in the standard m-spot X-ray photoelectron spectroscopy (XPS) mode, on beam-sensitive materials such as oxides

  • The atom probe tomography reconstruction of a specimen prepared from the as-deposited sample, the top surface of which had been investigated with scanning photoemission electron microscopy (SPEM) is shown in Fig. S2a.† A view on the cross section of a 5 nm thick slice through the 3D reconstruction (Fig. S2b†) reveals the presence of oxygen and carbon species on the top surface of the sample

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Summary

Introduction

Journal of Materials Chemistry A understand the electrochemical properties of Ir–Ru mixed oxide anodes prepared by this synthesis method. The oxidation of metallic bulk alloys used in heterogeneous catalysis was previously the center of some APT studies.[21,22,23,24,25] Soon a er, nanoparticles (NP) used in real catalysis applications were investigated.[26,27,28,29,30] the measurement of NPs can introduce further challenges as they typically need to be embedded in a solid matrix material before measurement, potentially introducing a number of measurement artifacts (e.g. ion trajectory aberrations) which complicate the APT data analysis and interpretation These attempts demonstrate the growing demand for shedding light on the atomic scale surface chemistry of catalytically active materials. These aspects are critical to understand when designing efficient, long-lived catalysts

Sample preparation
Scanning photoemission electron microcopy
Atom probe tomography
Spectromicroscopy
Validation of proposed experimental protocol
Relevance for OER catalysis
Outlook
Conclusions
Full Text
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