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Atomic force microscopy with nanoelectrode tips for high resolution electrochemical, nanoadhesion and nanoelectrical imaging

Nellist, Michael R. and Chen, Yikai and Mark, Andreas and Gödrich, Sebastian and Stelling, Christian and Jiang, Jingjing and Poddar, Rakesh and Li, Chunzeng and Kumar, Ravi and Papastavrou, Georg and Retsch, Markus and Brunschwig, Bruce S. and Huang, Zhuangqun and Xiang, Chengxiang and Boettcher, Shannon W. (2017) Atomic force microscopy with nanoelectrode tips for high resolution electrochemical, nanoadhesion and nanoelectrical imaging. Nanotechnology, 28 (9). Art. No. 095711. ISSN 0957-4484. doi:10.1088/1361-6528/aa5839.

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Multimodal nano-imaging in electrochemical environments is important across many areas of science and technology. Here, scanning electrochemical microscopy (SECM) using an atomic force microscope (AFM) platform with a nanoelectrode probe is reported. In combination with PeakForce tapping AFM mode, the simultaneous characterization of surface topography, quantitative nanomechanics, nanoelectronic properties, and electrochemical activity is demonstrated. The nanoelectrode probe is coated with dielectric materials and has an exposed conical Pt tip apex of ~200 nm in height and of ~25 nm in end-tip radius. These characteristic dimensions permit sub-100 nm spatial resolution for electrochemical imaging. With this nanoelectrode probe we have extended AFM-based nanoelectrical measurements to liquid environments. Experimental data and numerical simulations are used to understand the response of the nanoelectrode probe. With PeakForce SECM, we successfully characterized a surface defect on a highly-oriented pyrolytic graphite electrode showing correlated topographical, electrochemical and nanomechanical information at the highest AFM-SECM resolution. The SECM nanoelectrode also enabled the measurement of heterogeneous electrical conductivity of electrode surfaces in liquid. These studies extend the basic understanding of heterogeneity on graphite/graphene surfaces for electrochemical applications.

Item Type:Article
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URLURL TypeDescription
Brunschwig, Bruce S.0000-0002-6135-6727
Xiang, Chengxiang0000-0002-1698-6754
Boettcher, Shannon W.0000-0001-8971-9123
Additional Information:© 2017 IOP Publishing Ltd. Received 14 November 2016, revised 6 January 2017; Accepted for publication 10 January 2017; Published 31 January 2017. ZH, RP, and CL (employed by Bruker) developed the technique, manufactured the nanoelectrode probe, fabricated the Pt/nitride sample, and were involved in most of the measurements in collaboration with the other authors. Results collected on HOPG and the mesh electrodes were primarily performed by SWB and MRN. SWB, MRN, and ZH led manuscript preparation. SWB and MRN acknowledge support by the Department of Energy, Basic Energy Sciences, award number DE-SC0014279. The modeling and simulation work, and some of the SEM imaging were performed by YC, JJ and CX, and were supported by the Joint Center for Artificial Photosynthesis, a DOE Energy Innovation Hub, supported through the Office of Science of the US Department of Energy under Award Number DE-SC0004993. GP, MR, AM, SG and CS performed the preparation of and measurements on the Au nanomesh electrode, and acknowledge the support from the German Research Foundation (DFG) in the framework of the Collaborative Research Center (SFB 840). CS acknowledges support from the Elite Network of Bavaria (ENB). BSB acknowledges support from the National Science Foundation (NSF) Center for Chemical Innovation in Solar Fuels (CHE-1305124) for research (probe testing and device evaluation) carried out at the Molecular Materials Research Center of the Beckman Institute of the California Institute of Technology. RK assisted in the test of chemical compatibility and the PF-TUNA in liquid measurement.
Funding AgencyGrant Number
Department of Energy (DOE)DE-SC0014279
Department of Energy (DOE)DE-SC0004993
Deutsche Forschungsgemeinschaft (DFG)SFB 840
Elite Network of BavariaUNSPECIFIED
Issue or Number:9
Record Number:CaltechAUTHORS:20170131-095024118
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Official Citation:Michael R Nellist et al 2017 Nanotechnology 28 095711
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:73865
Deposited By: Tony Diaz
Deposited On:31 Jan 2017 18:05
Last Modified:12 Jul 2022 17:31

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