![]() ![]() 1 is specially designed to carry out imaging with CLPs thanks to the integration of a programmable, high precision rotational positioner that rotates the sample stage in between line scan measurements. A key difference is that the SECM instrument in Fig. 5,26,27 The common SECM components include X, Y, and Z positioners for precise control over the probe position and a bipotentiostat to control the applied potential of the probe and substrate. The overall design and many of the key components of this microscope share many similarities with the conventional SECM instruments, which have been described in detail in previous publications. DESIGN AND OPERATING PRINCIPLES OF CLP-SECMįigure 1 contains a simple block diagram showing the key components of our microscope and how they are configured with respect to each other. Subsequently, the communication and control of the hardware is explained and example measurements from the instrument are presented. Herein, we first describe the procedures for fabricating and characterizing the CLP used in this study before detailing the system design and key microscope components. The advantages of this new instrument include its ability to perform programmable rotational movements with simple hardware and probe design, allowing for streamlined data acquisition of electrochemical data. In this paper, we describe a custom-built programmable scanning electrochemical microscope setup for CLP-SECM imaging that can overcome these limitations. 22 Specifically, those first demonstrations involved tedious probe positioning, sample rotation, probe cleaning, and data acquisition procedures that increased imaging times and introduced unnecessary human errors into the measurement scheme. Our previous study described the basic principles of CLP-SECM imaging with CS image reconstruction, but the quality and areal imaging rates demonstrated in that work were limited by the CLPs and the microscope setup employed in that study. Additionally, fabrication of these probes is nontrivial, and more complex electronics (e.g., multiplexer or multichannel potentiostat) are required to record the signals from the individually addressable electroactive elements. 13,14,25 Yet, the resolution of these probes remains limited by the lateral spacing between the point probes embedded within the array. combined the idea of using a linear array of microelectrodes with polymeric thin films to create soft, flexible probes capable of imaging large sample areas, even for tilted and curved surfaces. 13,14,22–24 For example, multiple studies have demonstrated the use of individually addressable submicrometer electrodes for large area imaging. 2,3,19–21 Alongside instrument development, the use of innovative probe configurations and geometries has emerged as a promising approach to increase SECM imaging rates. 13,15–18 For example, the development of scanning droplet cells for scanning electrochemical cell microscopy (SECCM), combined with the use of more efficient spiral scan patterns, has resulted in substantial increases in areal imaging rates, thanks to their ability to utilize high scan rates without being limited by convection. Previous research efforts have attempted to overcome the trade-off between resolution and areal imaging rates through a variety of approaches that have involved modifications to SECM hardware, 1,8–12 the use of advanced probe geometries, 13–16 and/or post-measurement image processing to correct for blurriness and artifacts associated with fast scan speeds. These exemplary measurements illustrate methods for calibrating the positioning system, positioning and cleaning the CLP, and verifying proper positioning/probe sensitivity along its length. In order to illustrate the basic operating procedures for the microscope, line scans and images measured in the substrate generation-probe-collection mode for flat samples containing platinum disk electrodes are presented. Herein, we provide detailed descriptions of CLP fabrication, microscope design, and the procedures used to carry out scanning electrochemical microscopy imaging with CLPs. A combination of linear and rotational motors allows for CLP scanning at different angles over areas up to 25 cm 2 to generate the raw signal necessary to reconstruct the desired electrochemical image using CS signal analysis algorithms. The CLP is a nonlocal probe consisting of a band electrode, where the achievable spatial resolution is set by the thickness of the band and the achievable imaging rate is largely determined by its width. This article describes a home-built scanning electrochemical microscope capable of achieving high areal imaging rates through the use of continuous line probes (CLPs) and compressed sensing (CS) image reconstruction. ![]()
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