Scanning Electrochemical Cell Microscopy: A Versatile Technique for Nanoscale Electrochemistry and Functional Imaging

Ebejer, Neil; Güell, Aleix G.; Lai, Stanley C. S.; McKelvey, Kim; Snowden, Michael E.; Unwin, Patrick R.

doi:10.1146/annurev-anchem-062012-092650

Cited by 277 publications

(390 citation statements)

References 100 publications

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“…Ag wire (0.255 mm 3N, MaTeck), was inserted in each 'barrel' to act as a quasi-reference counter electrode (QRCE), and a bias potential (V 2 ) was applied between the two QRCEs to induce a conductance current (i dc ) through the meniscus which was continuously monitored, providing the basis for the tip-substrate separation feedback mechanism ( Figure 1). [18][19][20] The potential of the substrate was controlled via V 1 (Figure 1), where the potential of the surface (V Surf ) is expressed as: 20 The current through the substrate (i Surf ) was continuously recorded with a home-built four decade autoranging current follower, optimized for ultra-low current low noise measurement. A specialized electrometer and an eighth-order brick wall filter allowed the measurement of currents in the range of only tens of fA (SI, section S1).…”

Section: Photo-seccm Setupmentioning

confidence: 99%

Scanning Electrochemical Cell Microscopy Platform for Ultrasensitive Photoelectrochemical Imaging

et al. 2015

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Developing nanoscale structure-activity correlations is of major importance for the fundamental understanding and rational development of (photo)electrocatalysts. However, the low conversion efficiency of characteristic materials generates tiny photoelectrochemical currents at the submicron to nanoscale, in the fA range, which are challenging to detect and measure accurately. Here we report the coupling of scanning electrochemical cell microscopy (SECCM) with photo-illumination, to create a sub-micron spatial resolution cell that opens up high resolution structure-(photo)activity measurements. We demonstrate the capabilities of the technique as a tool for: (i) high spatial resolution (photo)activity mapping using an ionic liquid electrolyte at a thin film of TiO 2 aggregates, commonly used as a photo-anode in dye sensitized solar cells (DSSCs); and (ii) in-situ (photo)activity measurements of an electropolymerized conjugated polymer on a transparent Au substrate in a controlled atmospheric environment. Quantitative data, including localized (photo)electrochemical transients and external quantum efficiency (EQE) are extracted, and prospects for further technique development and enhancement are outlined.2

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Section: Photo-seccm Setupmentioning

confidence: 99%

Scanning Electrochemical Cell Microscopy Platform for Ultrasensitive Photoelectrochemical Imaging

et al. 2015

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“…2,3 While the simplest nanopipettes contain just a single channel, multichannel devices are also possible, which increases the versatility of nanopipettes for nanoscience applications. 4,5 The channels can be open 5,6 (filled with electrolyte and a control electrode) or functionalized with deposited carbon, for example, to produce ultramicroelectrodes (UMEs) 7,8 that can also be further functionalized [9][10][11] to tune the sensory properties. Nanoelectrodes can also be fabricated by electrochemically plating nanopipettes with a variety of different metals.…”

Section: Introductionmentioning

confidence: 99%

“…27 Beyond electroanalysis, nanopipettes are finding novel applications as devices for electrospray massspectrometry. 28,29 Nanopipette probes, employed in different types of scanning probe microscopy (SPM) techniques, 5,11,30 are used increasingly for the study of interfacial properties across a range of materials including electrodes and living cells. 3,31,32 Examples of SPM techniques that can employ nanopipettes include scanning electrochemical microscopy (SECM), 30,33 scanning ion conductance microscopy (SICM), 31,[34][35][36][37][38] SICM-SECM 9,39 and scanning electrochemical cell microscopy (SECCM).…”

Section: Introductionmentioning

confidence: 99%

“…3,31,32 Examples of SPM techniques that can employ nanopipettes include scanning electrochemical microscopy (SECM), 30,33 scanning ion conductance microscopy (SICM), 31,[34][35][36][37][38] SICM-SECM 9,39 and scanning electrochemical cell microscopy (SECCM). 5,40 Beyond the surface or interface being investigated, the size, shape and surface properties of the nanopipette may also strongly influence the SPM response, such that robust theoretical models, underpinned by a complete knowledge of the nanopipette characteristics, are needed for quantitative analysis.…”

Section: Introductionmentioning

confidence: 99%

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Characterization of Nanopipettes

et al. 2016

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Nanopipettes are widely used in electrochemical and analytical techniques as tools for sizing, sequencing, sensing, delivery and imaging. For all of these applications, the response of a nanopipette is strongly affected by its geometry and surface chemistry. As the size of nanopipettes becomes smaller, precise geometric characterization is increasingly important, especially if nanopipette probes are to be used for quantitative studies and analysis. This contribution highlights the combination of data from voltage-scanning ion conductivity experiments, transmission electron microscopy (TEM) and finite element method (FEM) simulations to fully characterize nanopipette geometry and surface charge characteristics, with an accuracy not achievable using existing approaches. Indeed, it is shown that presently used methods for nanopipette characterization can lead to highly erroneous information on nanopipettes. The new approach to characterization further facilitates high-level quantification of the behavior of nanopipettes in electrochemical systems, as demonstrated herein for a scanning ion conductance microscope (SICM) setup.

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“…Electrochemical measurements with, and control of, nanopipettes filled with electrolyte solution provide a platform for nanoscience, with myriad applications spanning analytical science, 1-5 materials characterization [6][7][8][9] and live cell studies. 10 Nanopipettes used as the probe in scanning ion conductance microscopy (SICM) are particularly powerful as a means of imaging the local topography of substrates.…”

Section: Introductionmentioning

confidence: 99%

Surface Charge Mapping with a Nanopipette

et al. 2014

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Nanopipettes are emerging as simple but powerful tools for probing chemistry at the nanoscale.In this contribution the use of nanopipettes for simultaneous surface charge mapping and topographical imaging is demonstrated, using a scanning ion conductance microscopy (SICM) format. When a nanopipette is positioned close to a surface in electrolyte solution the direct ion current (DC), driven by an applied bias between a quasi-reference counter electrode (QRCE) in the nanopipette and a second QRCE in the bulk solution is sensitive to surface charge. The charge sensitivity arises because the diffuse double layers at the nanopipette and the surface interact, creating a perm-selective region which becomes increasingly significant at low ionic strengths (10 mM 1:1 aqueous electrolyte herein). This leads to a polarity-dependent ion current and surface-induced rectification as the bias is varied. Using distance-modulated SICM, which induces an alternating ion current component (AC) by periodically modulating the distance between the nanopipette and the surface, the effect of surface charge on the DC and AC is explored and rationalized. The impact of surface charge on the AC phase (with respect to the driving sinusoidal signal) is highlighted in particular; this quantity shows a shift that is highly sensitive to interfacial charge and provides the basis for visualizing charge simultaneously with topography. The studies herein highlight the use of nanopipettes for functional imaging with applications from cell biology to materials characterization where understanding surface charge is of key importance.3

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Scanning Electrochemical Cell Microscopy: A Versatile Technique for Nanoscale Electrochemistry and Functional Imaging

Cited by 277 publications

References 100 publications

Scanning Electrochemical Cell Microscopy Platform for Ultrasensitive Photoelectrochemical Imaging

Scanning Electrochemical Cell Microscopy Platform for Ultrasensitive Photoelectrochemical Imaging

Characterization of Nanopipettes

Surface Charge Mapping with a Nanopipette

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