Exploring Electro-Chemo-Mechanical Phenomena on the Nanoscale Using Scanning Probe Microscopy
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Scanning Probe Microscopy
Scanning Electrochemical Microscopy
Scanning electrochemical probe microscopy (SEPM) techniques can disclose the local electrochemical reactivity of interfaces in single-entity and sub-entity studies. Operando SEPM measurements consist of using a SEPM tip to investigate the performance of electrocatalysts, while the reactivity of the interface is simultaneously modulated. This powerful combination can correlate electrochemical activity with changes in surface properties, e.g., topography and structure, as well as provide insight into reaction mechanisms. The focus of this review is to reveal the recent progress in local SEPM measurements of the catalytic activity of a surface toward the reduction and evolution of O2 and H2 and electrochemical conversion of CO2. The capabilities of SEPMs are showcased, and the possibility of coupling other techniques to SEPMs is presented. Emphasis is given to scanning electrochemical microscopy (SECM), scanning ion conductance microscopy (SICM), electrochemical scanning tunneling microscopy (EC-STM), and scanning electrochemical cell microscopy (SECCM).
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Abstract A novel and cost-efficient probe fabrication method yielding probes for performing simultaneous scanning electrochemical microscopy (SECM) and scanning ion conductance microscopy (SICM) is presented. Coupling both techniques allows distinguishing topographical and electrochemical activity information obtained by SECM. Probes were prepared by deposition of photoresist onto platinum-coated, pulled fused silica capillaries, which resulted in a pipette probe with an integrated ring ultramicroelectrode. The fabricated probes were characterized by means of cyclic voltammetry and scanning electron microscopy. The applicability of probes was demonstrated by measuring and distinguishing topography and electrochemical activity of a model substrate. In addition, porous boron-doped diamond samples were investigated via simultaneously performed SECM and SICM. Graphic abstract
Scanning Electrochemical Microscopy
Ultramicroelectrode
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Photoresist
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Abstract Scanning electrochemical microscopy (SECM) is one of a number of scanned probe microscopy (SPM) techniques invented following the demonstration of the scanning tunneling microscope. The use of an electrochemical process for image formation defines SECM. In most applications of the method, an ultramicroelectrode (UME) is used as the probe and the probe signal is the Faradic current arising from the electrolysis of solution species. In other cases, the use of an ion‐selective electrode (ISE) as the probe provides a probe signal proportional to the logarithm of the activity of an ion in solution (eg., pH). In SECM, the primary interaction between probe tip and sample is mediated by diffusion of solution species between the sample and the tip of the probe, which distinguishes SECM from other SPM methods that may use an electrochemically active probe. An electrochemically active probe permits a versatile range of experiments, an essential aspect of which is chemical sensitivity or control of chemical processes occurring at a substrate surface. Forming an image in an SPM technique requires that the probe signal be perturbed in a reproducible fashion by some aspect of the imaged substrate. There are two principal image‐forming modes in SECM: feedback and generation/collection (GC). The feedback mode uses the Faradaic current that flows from electrolysis of an intentionally‐added or naturally present mediator species at an UME probe. Imaging in the feedback mode provides topographic images of blocking or conducting surfaces. Images of many types of surfaces have been obtained in the feedback mode; examples include images of electrodes, polymer films, and immiscible liquid interfaces. It is possible to manipulate the SECM imaging conditions to produce images that representing chemical and electrochemical activity. The generation/collection (GC) mode uses the probe to detect changes in the concentration of a chemical species at the surface of the imaged material. Ideally, the probe acts as a passive sensor to produce concentration maps of a particular chemical species near the substrate surface. GC mode imaging is described further by the type of sensing probe used. In amperometric GC imaging, the probe is an UME, which detects species by electrolysis. First reported as a method to map electrochemically active areas on electrodes, amperometric GC is used to make high‐resolution chemical concentration maps of corroding metal surfaces, biological materials, and polymeric materials. In addition, measurements of ion fluxes through porous materials, such as skin and dental material, are useful applications. In potentiometric GC imaging, the probe is an ISE, which has the advantage of increased sensitivity to nonelectroactive ions and improved selectivity for imaging a desired ion concentration.
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Scanning Probe Microscopy
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Chemical Imaging
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Due to their exceptional sensitivity, scanning probe microscopes enable detailed interrogation of surfaces and interfaces. When correlating spatial information to additional scanning probe surface measurements (such as force, electrical potential or conductivity, impedance, thermal mapping, viscoelastic parameters, redox activity, and more), spatial resolution is often limited. In this work, we present the development and demonstrate the utility of an electrochemical assembly (probe, potentiostat, and sample cell) for use with a high-resolution, fast scanning Cypher atomic force microscope that enables measurements of highly-localized electrochemical signals. These measurements bear on various metrologies such as electrochemical scanning tunneling microscopy (EC-STM), scanning electrochemical microscopy (SECM), and electrochemical strain microscopy (ECSM), and relevant results will be presented. Figure 1. The first-generation electrochemical cell for use with a lower-resolution scanning probe microscope. Figure 1
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Abstract Spatially resolved characterization of electrode surfaces or electrode–electrolyte interfaces is of fundamental interest in battery research to unravel the complex underlying physicochemical processes. Scanning probe microscopy (SPM) techniques and derived methods have recently gained importance in in situ or operando studies of battery electrodes. This minireview provides an overview on well‐established and advanced SPM methods such as scanning electrochemical cell microscopy (SECCM) and hybrid atomic force microscopy–scanning electrochemical microscopy (AFM‐SECM) and their future potential for in situ/operando studies providing correlated structure/reactivity information. Although, most studies so far are focusing on lithium (Li)‐ion batteries, the potential for post‐Li battery chemistries is clearly evident. Future approaches for rapid performance assessment using scanning droplet cell electrochemistry in combination with advanced scanning probe microscopy are proposed and contrasted with the emerging challenges in the characterization of novel battery chemistries, as SPM methods have not yet been much used in this research area.
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Scanning probe microscopy (SPM) techniques have become indispensable tools for studying nano- and microscale materials and processes but suffer from a trade-off between resolution and areal scan rate that limits their utility for a number of applications and sample types. Here, we present a novel approach to SPM imaging based on combining nonlocal scanning line probes with compressed sensing (CS) signal analysis methods. Using scanning electrochemical microscopy (SECM) as an exemplar SPM technique, we demonstrate this approach using continuous microband electrodes, or line probes, which are used to perform chemical imaging of electrocatalytic Pt discs deposited on an inert substrate. These results demonstrate the potential to achieve high areal SPM imaging rates using nonlocal scanning probes and CS image reconstruction.
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Microscale chemistry
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Abstract Scanning electrochemical microscopy (SECM) is one of a number of scanning probe microscopy (SPM) techniques that arose out of the development of the scanning tunneling and atomic force microscopes. Scanning probe microscopes operate by scanning, or “rastering,” a small probe tip over the surface to be imaged. The SECM tip is electrochemically active, and imaging occurs in an electrolyte solution. In most cases, the SECM tip is an ultramicroelectrode (UME), and the tip signal is a Faradaic current from electrolysis of solution species. Some SECM experiments use an ion‐selective electrode (ISE) as a tip. In this case, the tip signal is usually a voltage proportional to the logarithm of the ion activity in solution. The use of an electrochemically active tip allows an extremely versatile set of experiments, with chemical sensitivity to processes occurring at a substrate surface as an essential aspect. A requirement of SPM techniques is that the signal from the tip must be perturbed in some reproducible fashion by the presence of the surface. One of the two methods used in SECM to provide this signal change is known as the “feedback” mode. Feedback can provide topographic images of either electronically insulating or conducting surfaces. A unique advantage of SECM is the ability to design experiments in which the mediator interacts with the substrate surface to provide chemical and electrochemical activity maps at micrometer and submicrometer resolution.
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Abstract : This conference dealt with an array of scanning probe and other microscopy techniques based on various physical and chemical properties. Some of them are: Scanning Tunneling Microscopy STM, Scanning Electrochemical Microscopy SEM, Scanning Capacitance Microscopy SCM, Scanning Force Microscopy SFM, Atomic Force Microscopy AFM, Magnetic Force Microscopy, Photon STM, Ballistic Electronic Microscopy, Photo Tunneling Microscopy, Evanescent Field Optical Microscopy.
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Scanning electrochemical microscopy (SECM) is a method of local probe microscopy based on the displacement of an ultramicroelectrode (UME) in the vicinity of an interface. The UME has at least one dimension in the micrometer range. It is extremely useful in modern electroanalysis for the characterization of surfaces by imaging electroactive and non-electroactive materials or for obtaining quantitative data on specific analytes or processes by studying the reactions occurring on the surface of a substrate. It operates through several modes (feedback, generation/collection, penetration etc…) and allows evaluating kinetics of chemical reactions, studying biological cells, achieving localized surface modifications or imaging surfaces. More recently, scanning electrochemical cell microscopy (SECCM) was developed to allow obtaining high spatial resolution images. SECCM is derived from SECM and consists of a probe which is a sharp double barrel capillary (nanopipette), with both compartments containing a quasi-reference electrode or quasi-reference counter electrode (QRCE) and filled with an electrolytic solution.
Scanning Electrochemical Microscopy
Ultramicroelectrode
Scanning Probe Microscopy
Chemical Imaging
Micrometer
Characterization
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Scanning Electrochemical Microscopy
Scanning Probe Microscopy
Biomolecule
Nanometre
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