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Graphene oxide windows for in situ environmental cell photoelectron spectroscopy

Nature Nanotechnology volume 6, pages 651–657 (2011)Cite this article

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Abstract

The performance of new materials and devices often depends on processes taking place at the interface between an active solid element and the environment (such as air, water or other fluids). Understanding and controlling such interfacial processes require surface-specific spectroscopic information acquired under real-world operating conditions, which can be challenging because standard approaches such as X-ray photoelectron spectroscopy generally require high-vacuum conditions. The state-of-the-art approach to this problem relies on unique and expensive apparatus including electron analysers coupled with sophisticated differentially pumped lenses. Here, we develop a simple environmental cell with graphene oxide windows that are transparent to low-energy electrons (down to 400 eV), and demonstrate the feasibility of X-ray photoelectron spectroscopy measurements on model samples such as gold nanoparticles and aqueous salt solution placed on the back side of a window. These proof-of-principle results show the potential of using graphene oxide, graphene and other emerging ultrathin membrane windows for the fabrication of low-cost, single-use environmental cells compatible with commercial X-ray and Auger microprobes as well as scanning or transmission electron microscopes.

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Figure 1: Design of ambient-pressure XPS systems.
Figure 2: Fabrication of GO windows for E-cells.
Figure 3: Experimental setup and GO overlayer characterization.
Figure 4: Principle of effective attenuation length measurements of GO sheets.
Figure 5: Suspended GO membranes as windows for an E-cell.
Figure 6: XPS on wet samples.

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Acknowledgements

A.K. thanks E. Strelcov, C. Watts and J. Bozzola (SIUC) for their help in the preparation of the experiment. The work at ELETTRA was partly supported by AMBIOSEN Friuli Venezia-Giulia regional grant 47/78. M.K.A. thanks P. Parisse for AFM measurements. The TEM and FIB work was performed in the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by NSF-NSEC, NSF-MRSEC, the Keck Foundation, the State of Illinois and Northwestern University. The SIUC part of the research was supported by a NSF ECCS-0925837 grant. L.J.C and J.H. were supported by the NSF through a CAREER award (DMR 0955612).

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Authors and Affiliations

  1. Southern Illinois University, Carbondale, 62901, Illinois, USA

    Andrei Kolmakov

  2. Northwestern University, Evanston, 60208, Illinois, USA

    Dmitriy A. Dikin, Laura J. Cote & Jiaxing Huang

  3. Sincrotrone Trieste 34012 Trieste, Italy

    Majid Kazemian Abyaneh, Matteo Amati, Luca Gregoratti & Maya Kiskinova

  4. Chemie Department, TU München, Lichtenbergstr. 4, Garching, D-85748, Germany

    Sebastian Günther

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  1. Andrei Kolmakov
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Contributions

A.K. conceived the project, designed and tested the E-cell prototypes, and assembled the manuscript, with contributions from all co-authors. D.D., L.C. and J.H. developed the methods of GO synthesis, processing and Langmuir–Blodgett deposition onto SiO2/Si3N4 membrane samples. D.D. performed all micromachining and carried out SEM, TEM and HRTEM characterization of the GO overlayers and suspended membranes. M.K.A., M.A., L.G., S.G. and M.K conducted the SPEM experiments and the corresponding data analysis of the photoelectron images and spectra. A.K. and S.G. participated in spectromicroscopy tests as users of the ELETTRA ESCA microscopy beamline.

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Correspondence to Andrei Kolmakov.

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Kolmakov, A., Dikin, D., Cote, L. et al. Graphene oxide windows for in situ environmental cell photoelectron spectroscopy. Nature Nanotech 6, 651–657 (2011). https://doi.org/10.1038/nnano.2011.130

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