Fabrication of Scanning Electrochemical Microscopy-Atomic Force Microscopy Probes to Image Surface Topography and Reactivity at the Nanoscale

Velmurugan, Jeyavel; Agrawal, Amit; An, Sang M.; Choudhary, Eric; Szalai, Veronika A.

doi:10.1021/acs.analchem.7b00210

Cited by 23 publications

(20 citation statements)

References 35 publications

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“…An EC‐AFM probe can be modified in different ways, for example fabricated to be a SECM probe by using a Pt wire with insulation sheath as the tip . With these modifications, EC‐AFM can carry out the functions of a SECM setup on top of normal EC‐AFM imaging.…”

Section: Electrochemical Scanning Probe Microscopiesmentioning

confidence: 99%

Electrochemical Scanning Probe Microscopies in Electrocatalysis

et al. 2018

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surface coordination, strain effects, [6][7][8][9] ligand effects, [10,11] ensemble effects, [12] and the electrolyte composition. [13] A detailed understanding of these effects requires experimental and computational procedures to investigate the working mechanisms of the electrocatalysis. Ideally, atomically resolved topographic and chemical information of the catalyst surface under reaction conditions is required. Transmission electron microscopy (TEM) has been reported to be capable of in operando investigation of catalyst structures while catalytic reactions are taking place. [14] However, the instrumentation utilized for such purpose has very strong restrictions and realistic operating conditions cannot be easily applied so far. Alternatively, scanning probe microscopies (SPMs) and electrochemical scanning probe microscopies (EC-SPMs) are able to perform structural measurements of catalytic systems under reaction conditions with resolution down to atomic scales. Normally, EC-SPMs, for instance electrochemical scanning tunneling microscopy (EC-STM), electrochemical atomic force microscopy (EC-AFM), and scanning electrochemical potential microscopy (SECPM), can provide structural information on the solid side of the electrode/electrolyte interface at the atomic level for conductive samples (EC-STM is limited in the case of semi/nonconductive samples). However, these techniques usually lack the capability of chemical sensitivity, ultrahigh resolution reactivity monitoring, and probing the property of the electrolyte side of the interface. One well-developed exception is the scanning electrochemical microscopy (SECM), which will also be discussed in detail within this review. Additionally, SECM and related methods permit gleaning information about the electrolyte side of the electrochemical interface. However, the resolution of SECM and related methods is limited by the size of the SECM-probe and the working principle of SECM.In this review, first a very brief overview on electrocatalysis and on the importance of model substrates for understanding the fundamental underlying principles is given. Thereafter, the operational principle of different SPM techniques is summarized. The main focus of the work lies then on the application of the techniques to study phenomena important for electrocatalysis, including surface topography and adsorption processes. Within that context, also the application of room Improvements toward highly efficient electrochemical energy conversion require a detailed understanding of the underlying electrochemical processes at electrified solid-liquid interfaces. In situ and in operando studies by means of electrochemical scanning probe microscopy (EC-SPM) have become indispensable experimental tools due to their capability of resolving surface topography down to the atomic level even within the harsh environment of electrolytes. EC-SPM methodologies have thus contributed tremendously to the current understanding of electrocatalysis. In this review article, recent achievements in complement...

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Section: Electrochemical Scanning Probe Microscopiesmentioning

confidence: 99%

Electrochemical Scanning Probe Microscopies in Electrocatalysis

et al. 2018

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“…SECM-SICM for example uses the SICM component of the probe as a means of achieving distance control for topography, with simultaneous measurement of an electrochemical signal using the SECM component of the probe, and is discussed in greater detail in Section 3 (vide infra). Although SECM-SICM and SECM-AFM require specialized probes (Figure 1), these are becoming more widely adopted [39]. For example, SECM-AFM probes are now commercially available, and SECM-SICM probes can be fabricated in minutes at low cost (excluding the large initial cost of a laser-based pipette puller).…”

Section: Constant-distance Imaging Modesmentioning

confidence: 99%

Advances and Perspectives in Chemical Imaging in Cellular Environments Using Electrochemical Methods

Lazenby

White

2018

Chemosensors

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This review discusses a broad range of recent advances (2013)(2014)(2015)(2016)(2017) in chemical imaging using electrochemical methods, with a particular focus on techniques that have been applied to study cellular processes, or techniques that show promise for use in this field in the future. Non-scanning techniques such as microelectrode arrays (MEAs) offer high time-resolution (<10 ms) imaging; however, at reduced spatial resolution. In contrast, scanning electrochemical probe microscopies (SEPMs) offer higher spatial resolution (as low as a few nm per pixel) imaging, with images collected typically over many minutes. Recent significant research efforts to improve the spatial resolution of SEPMs using nanoscale probes and to improve the temporal resolution using fast scanning have resulted in movie (multiple frame) imaging with frame rates as low as a few seconds per image. Many SEPM techniques lack chemical specificity or have poor selectivity (defined by the choice of applied potential for redox-active species). This can be improved using multifunctional probes, ion-selective electrodes and tip-integrated biosensors, although additional effort may be required to preserve sensor performance after miniaturization of these probes. We discuss advances to the field of electrochemical imaging, and technological developments which are anticipated to extend the range of processes that can be studied. This includes imaging cellular processes with increased sensor selectivity and at much improved spatiotemporal resolution than has been previously customary.

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“…There are also combined techniques such as SECM-SICM [30][31] and SECM-atomic force microscopy (AFM) [32]. However, ion conductance (vide infra) and AFM, when coupled to SECM, require specialized probes that allow for the deconvolution of topography and electroactivity [33]. SECM-AFM probes are commercially available, although due to the nature of feedback of AFM, imaging soft cellular samples can be problematic [34].…”

Section: Constant-distance Imaging Modesmentioning

confidence: 99%