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Measurement and Manipulation of the Charge State of an Adsorbed Oxygen Adatom on the Rutile TiO2(110)-1×1 Surface by nc-AFM and KPFM

  • Quanzhen Zhang
    Quanzhen Zhang
    Department of Applied Physics, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan
    More by Quanzhen Zhang
  • , 
  • Yan Jun Li*
    Yan Jun Li
    Department of Applied Physics, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan
    *[email protected]
    More by Yan Jun Li
    Orcidhttp://orcid.org/0000-0001-7845-326X
  • , 
  • Huan Fei Wen
    Huan Fei Wen
    Department of Applied Physics, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan
    More by Huan Fei Wen
    Orcidhttp://orcid.org/0000-0002-2972-9669
  • , 
  • Yuuki Adachi
    Yuuki Adachi
    Department of Applied Physics, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan
    More by Yuuki Adachi
  • , 
  • Masato Miyazaki
    Masato Miyazaki
    Department of Applied Physics, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan
    More by Masato Miyazaki
  • , 
  • Yasuhiro Sugawara
    Yasuhiro Sugawara
    Department of Applied Physics, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan
    More by Yasuhiro Sugawara
  • , 
  • Rui Xu
    Rui Xu
    CAS Key Laboratory of Standardization and Measurement for Nanotechnology, CAS Center for Excellence in Nanoscience, National Center for Nanoscience and Technology, Beijing 100190, P. R. China
    More by Rui Xu
  • , 
  • Zhi Hai Cheng
    Zhi Hai Cheng
    CAS Key Laboratory of Standardization and Measurement for Nanotechnology, CAS Center for Excellence in Nanoscience, National Center for Nanoscience and Technology, Beijing 100190, P. R. China
    More by Zhi Hai Cheng
    Orcidhttp://orcid.org/0000-0003-4938-4490
  • , 
  • Ján Brndiar
    Ján Brndiar
    Center for Computational Materials Science, Institute of Physics, Slovak Academy of Sciences, 84511 Bratislava, Slovakia
    More by Ján Brndiar
  • , 
  • Lev Kantorovich
    Lev Kantorovich
    Department of Physics, King’s College London, The Strand, London, WC2R 2LS, United Kingdom
    More by Lev Kantorovich
    Orcidhttp://orcid.org/0000-0001-9379-6834
  • , and 
  • Ivan Štich
    Ivan Štich
    Center for Computational Materials Science, Institute of Physics, Slovak Academy of Sciences, 84511 Bratislava, Slovakia
    Institute of Informatics, Slovak Academy of Sciences, 84507 Bratislava, Slovakia
    More by Ivan Štich
    Orcidhttp://orcid.org/0000-0003-3338-8737
Cite this: J. Am. Chem. Soc. 2018, 140, 46, 15668–15674
Publication Date (Web):October 16, 2018
https://doi.org/10.1021/jacs.8b07745
Copyright © 2018 American Chemical Society
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    Abstract

    Abstract Image

    For the first time, the charge states of adsorbed oxygen adatoms on the rutile TiO2(110)-1×1 surface are successfully measured and deliberately manipulated by a combination of noncontact atomic force microscopy and Kelvin probe force microscopy at 78 K under ultrahigh vacuum and interpreted by extensive density functional theory modeling. Several kinds of single and double oxygen adatom species are clearly distinguished and assigned to three different charge states: Oad–/2Oad–, Oad2–/2Oad2–, and Oad––Oad2–, i.e., formal charges of either one or two electrons per atom. Because of the strong atomic-scale image contrast, these states are clearly resolved. The observations are supported by measurements of the short-range force and local contact potential difference as a function of the tip–sample distance as well as simulations. Comparison with the simulations suggests subatomic resolution by allowing us to resolve the rotated oxygen p orbitals. In addition, we manage to reversibly switch the charge states of the oxygen adatoms between the Oad– and Oad2– states, both individually and next to another oxygen, by modulating the frequency shift at constant positive voltage during both charging and discharging processes, i.e., by the tip-induced electric field of one orientation. This work provides a novel route for the investigation of the charge state of the adsorbates and opens up novel prospects for studying transition-metal-oxide-based catalytic reactions.

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/jacs.8b07745.

    • Experimental details and schematic circuits of FM-KPFM with bias voltage feedback; typical AFM image and corresponding ball model of the rutile TiO2(110)-1 × 1 surface in the hole mode; ball models of the two proposed adsorption and dissociation types of oxygen adatoms on the rutile TiO2(110) surface; stable 2Oad–, 2Oad2– species after spectral measurement; charging the adsorbed oxygen species by increasing the bias voltage; further simulation details, such as the geometry, including that of the polarons, the preparation of desired oxygen charge states in the simulations, subatomic resolution, Bader analysis of computed charges on the oxygen species, and the effect of the electric field on the key electronic states and charge distributions corresponding to different charging (PDF)

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    Cited By

    This article is cited by 48 publications.

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