Influence of electrode size and geometry on electrochemical experiments with combined SECM–SFM probes
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Gold electrodes integrated into silicon scanning force microscopy (SFM) probes allow the acquisition of spatially correlated data for sample morphology (via SFM) and local electrochemical reactivity via scanning electrochemical microscopy (SECM). The lateral resolution of both techniques is controlled by different properties of the integrated probes. The topographic tracking provided by the SFM mechanism allows the realization of very small working distances for the SECM measurements. Microfabrication technology was used in order to reduce the size of the active electrode area of the tip into the sub-100 nm regime. The functionality of the probes was tested using electrochemical methods. Experiments revealed that the response could be quantitatively compared to numerical simulation. The low working distance, in combination with the small size of the active electrode area, allows for high lateral resolution in the SECM images. This is illustrated with different model substrates that cover a range of different rate constants and illustrate the dependence of the SECM contrast on the local kinetics of the sample in the sub-micrometre size range.Keywords:
Scanning Electrochemical Microscopy
Scanning Probe Microscopy
As the development of scanning probe microscopy (SPM) continues, the spatial resolution and sensitivity for various material properties steadily improve. Therefore, SPM images morphological features as well as electrical, mechanical, magnetic, and chemical properties with a nanoscale resolution. Among the various SPM techniques, pipette-based SPM offers new possibilities and insights into the sample’s electrochemical properties. Since the invention of scanning electrochemical microscopy (SECM), the first-generation pipette-based SPM for electrochemical measurement, it has been extensively used in many research fields, e.g. for visualizing chemical reactions at surfaces and interfaces. However, the difficult distance control between the pipette probe and the sample surface limits the application of SECM. Here, we introduce scanning electrochemical cell microscopy (SECCM): a latest pipette-based SPM method, which investigates electrochemical responses on target materials in a point-by-point approach using the ionic current for distance control. We present experimental and theoretical data on contributing factors to the electrochemical response, including pipette configuration, redox species, scan rate and choice of substrate. A variety of pipette inner diameters (range from ~150 nm to ~ 1 μm), buffer concentrations, and voltammetric sweep rates are reviewed using well-defined conductive substrates and electrodes. Based on our results, we propose optimized experimental parameters for various measurement conditions. We believe that SECCM has great potential in providing new insights to electrochemical properties of surfaces and interfaces required for research on chemical energy storage, among others. Figure 1
Scanning Electrochemical Microscopy
Pipette
Scanning Probe Microscopy
Horizontal scan rate
Electrochemical cell
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The combination of scanning electrochemical microscopy (SECM) With atomic force microscopy (AFM) requires a combined scanning probe tip. In order to add the functionality of SECM, submicro- and nanoelectrodes have been integrated into AFM tips, using focused ion beam (FIB) based microfabrication techniques. Meeting the requirements for SECM measurements, needs to integrate the electroactive area within a certain working distance recessed form the apex of the AFM tip. Furthermore, a pinhole-free insulating layer is a major prerequisite for simultaneous topographical and electrochemical imaging applications. Parylene C was successfully applied for the insulation of the combined scanning probe tips. Cyclovoltarnmetry was performed, in order to characterize the electrochemical properties. Furthermore, FIB microfabrication procedures benefit from the advantageous properties of Parylene towards manufacturing integrated nanoelectrodes.
Scanning Electrochemical Microscopy
Parylene
Scanning Probe Microscopy
Pinhole (optics)
Characterization
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There has been tremendous development on microscopy techniques based on the scanning tunneling and atomic force microscopes over the last decades. The aim of this book chapter is to provide introductory concepts, basic operating principles and recent advances on seventeen selected techniques in this field. The focus is on applications of each technique in key areas of nanoscience and nanotechnology. The characterization of local functionalities ranges from physical and chemical properties of diverse materials including semiconductors, metals, oxides, polymers and biological systems. The topics include scanning electrochemical microscopy (SECM), electrochemical scanning tunneling microscopy (ECSTM), scanning ion conduction microscopy (SICM), scanning gate microscopy (SGM), scanning capacitance microscopy (SCM), near-field scanning optical microscopy (NSOM), force modulation microscopy (FMM), photo scanning tunneling microscopy (PSTM), scanning spread resistance microscopy (SSRM), scanning thermal microscopy (SThM), conductive atomic force microscopy (CAFM), scanning Hall probe microscopy (SHPM), Kelvin probe force microscopy (KPFM), piezoresponse force microscopy (PFM), scanning electrostatic force microscopy (SEFM), synchrotron X-ray scanning tunneling microscopy (SXSTM) and scanning voltage microscopy (SVM).
Keywords:
scanning probe microscopy;
scanning electrochemical microscopy;
scanning ion conduction microscopy;
scanning capacitance microscopy;
scanning spread resistance microscopy;
conductive atomic force microscopy;
scanning voltage microscopy
Scanning Probe Microscopy
Scanning Electrochemical Microscopy
Scanning thermal microscopy
Scanning gate microscopy
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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).
Scanning Electrochemical Microscopy
Scanning Probe Microscopy
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Scanning Electrochemical Microscopy
Scanning Probe Microscopy
Electrochemical energy conversion
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Scanning Electrochemical Microscopy
Ultramicroelectrode
Scanning Probe Microscopy
Micrometer
Chemical Imaging
Characterization
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The application of scanning tunnelling microscopy (STM) and scanning electrochemical microscopy (SECM) to studies of the liquid/solid interface, especially electrode surfaces, is reviewed. Some general principles describing features of the images obtained by these techniques are proposed and illustrated by examples taken from recent work in the authors' laboratory.
Scanning Electrochemical Microscopy
Scanning Probe Microscopy
Interface (matter)
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Three main electrochemical scanning probe microscopy(EC SPM) techniques for micro and nano fabrication are reviewed. The mechanism and different approaches of micro/nanofabrication about scanning tunneling microscope (STM), atomic force microscope (AFM) and scanning electrochemical microscope (SECM) are discussed in detail. The advantage and disadvantage of each technique are compared and analyzed.
Scanning Probe Microscopy
Scanning Electrochemical 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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In the past 20 years the characterization of electroactive surfaces and electrode reactions by scanning probe techniques has advanced significantly, benefiting from instrumental and methodological developments in the field. Electrochemical and electrical analysis instruments are attractive tools for identifying regions of different electrochemical properties and chemical reactivity and contribute to the advancement of molecular electronics. Besides their function as a surface analytical device, they have proved to be unique tools for local synthesis of polymers, metal depots, clusters, etc. This review will focus primarily on progress made by use of scanning electrochemical microscopy (SECM), conductive AFM (C-AFM), electrochemical scanning tunneling microscopy (EC-STM), and surface potential measurements, for example Kelvin probe force microscopy (KFM), for multidimensional imaging of potential-dependent processes on metals and electrified surfaces modified with polymers and self assembled monolayers.
Scanning Electrochemical Microscopy
Characterization
Scanning Probe Microscopy
Self-assembled monolayer
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