AVS 64th International Symposium & Exhibition
    Novel Trends in Synchrotron and FEL-Based Analysis Focus Topic Wednesday Sessions
       Session SA+AS+HC+SS-WeA

Paper SA+AS+HC+SS-WeA3
Graphene Capped Static and Fluidic Systems for In-Liquid Atmospheric Pressure XPS/AES/SEM and PEEM Studies of Electrochemical Interfaces

Wednesday, November 1, 2017, 3:00 pm, Room 9

Session: In Situ and Operando Characterization of Interfacial Reactions in Energy & Electronic Devices
Presenter: Hongxuan Guo, NIST, Center for Nanoscale Science and Technology
Authors: H.X. Guo, NIST, Center for Nanoscale Science and Technology
E. Strelcov, NIST, Center for Nanoscale Science and Technology
A. Yulaev, NIST, Center for Nanoscale Science and Technology
S. Nemšák, Peter Grünberg Institute and Institute for Advanced Simulation, Germany
D.N. Mueller, Peter Grünberg Institute and Institute for Advanced Simulation, Germany
C.M. Schneider, Peter Grünberg Institute and Institute for Advanced Simulation, Germany
A. Kolmakov, NIST, Center for Nanoscale Science and Technology
Correspondent: Click to Email
The liquid-solid electrochemical interfaces are a central topic of modern energy-related electrochemistry and catalysis research. For the last two decades, this research line benefited greatly from the development of differentially pumped electron optics and refreshable sample delivery systems which became an experimental core of the modern ambient pressure electron spectroscopy. An alternative experimental approach to atmospheric pressure electron microscopy (SEM1, SPEM2, PEEM3) and spectroscopy (XPS4-5, XAS3,6) has been recently tested. In this approach, high electron transparency and molecular impermeability of the graphene membrane was employed to separate the liquid or gaseous sample from ultra-high vacuum environment of electron spectrometer.

In this presentation, we will show our recent work on design and performance of the static and fluidic microfabricated arrays (MCA) capped with bilayer graphene. With such a liquid cell, we characterized water and aqueous solution employing synchrotron-based and standard laboratory XPS, SEM, EDX, and Auger spectroscopy setups7. In particular, Cu electroplating and copper sulfate electrolyte polarization at the graphene working electrode have been studied spectroscopically in real time and nanoscopic spatial resolution.

Acknowledgement

ES, HG, and AY acknowledge support under the Cooperative Research Agreement between the University of Maryland and the National Institute of Standards and Technology Center for Nanoscale Science and Technology, Award 70NANB14H209, through the University of Maryland.

Reference

1. J. D. Stoll and A. Kolmakov, Nanotechnology 23 (50), 505704 (2012).

2. A. Kolmakov, D. A. Dikin, L. J. Cote, J. Huang, M. K. Abyaneh, M. Amati, L. Gregoratti, S. Günther and M. Kiskinova, Nature nanotechnology 6 (10), 651-657 (2011).

3. H. Guo, E. Strelcov, A. Yulaev, J. Wang, N. Appathurai, S. Urquhart, J. Vinson, S. Sahu, M. Zwolak and A. Kolmakov, Nano letters (2017).

4. J. Kraus, R. Reichelt, S. Günther, L. Gregoratti, M. Amati, M. Kiskinova, A. Yulaev, I. Vlassiouk and A. Kolmakov, Nanoscale 6 (23), 14394-14403 (2014).

5. R. S. Weatherup, B. Eren, Y. Hao, H. Bluhm and M. B. Salmeron, The journal of physical chemistry letters 7 (9), 1622-1627 (2016).

6. J.-J. Velasco-Velez, C. H. Wu, T. A. Pascal, L. F. Wan, J. Guo, D. Prendergast and M. Salmeron, Science 346 (6211), 831-834 (2014).

7. A. Yulaev, H. Guo, E. Strelcov, L. Chen, I. Vlassiokiv and A. Kolmakov, ACS Applied Materials & Interfaces (accepted) (2017).