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Scanning electrochemical probe microscopy (SEPM) maps and investigates the chemical and physical properties of surfaces and interfaces using a micro- or nanoscale electrochemical probe, e.g., a microelectrode or a nanopipette, positioned close to an interface of interest. SEPMs share a common general architecture but are distinct from each other through the choice of probe and in the different physicochemical properties of the sample that can be investigated, including, among others, interfacial charge transfer rates, topography, permeability, or surface charge. Thus, a single instrument, with an appropriately flexible control system, can facilitate widespread access to the family of SEPM techniques - scanning electrochemical microscopy (SECM), scanning ion conductance microscopy (SICM), scanning electrochemical cell microscopy (SECCM), the scanning micropipette contact method (SMCM), and hybrid varieties of these techniques. Herein, we describe in detail a flexible open-source SEPM instrument that can perform common and widely applicable SEPM techniques and experimenter-defined methodologies, with minimal programming from the user. The instrument makes use of a field programmable gate array (FPGA)-based data acquisition card, and this contribution further illustrates the benefits of adopting FPGA architecture generally in electrochemical instrumentation. We describe the software and hardware for the instrument, using examples from the literature to illustrate how common SEPM operation modes and hyphenated techniques are readily implemented. Additionally, to demonstrate the application of custom-developed scanning protocols, we briefly present some further experimental examples. This Tutorial seeks to serve the needs of expert users of SEPMs and encourage new entrants alike.  To this end, to encourage those who are interested in either setting up their own instruments or making optimal use of commercially available instruments, we also briefly include some more basic and general information on SEPM techniques and uses, to put the more advanced work and instrumental aspects in context. # Data from: A look inside a flexible open-source scanning electrochemical probe microscope Dataset DOI: [10.5061/dryad.9p8cz8wx3](https://doi.org/10.5061/dryad.9p8cz8wx3) ## Description of the data and file structure Comma-separated text file representing SICM imaging of topography and BH~4~^-^ electrooxidation on a Au nanocluster (AuNC) in 30 mM NaOH (pH 12.5) aqueous solution with 3 mM NaBH~4~. Figures and tables refer to the associated primary article. ### Files and variables * ScanHopping.tsv Columns represent: | Data Channel Name | Units | Description | Breakout Box Connector | | :---------------- | :----------------------- | :---------------------------------------------------------------------------------------------------------- | :--------------------- | | X | µm | Measured X Piezo Position | AI-0 | | Y | µm | Measured Y Piezo Position | AI-1 | | Z | µm | Measured Z Piezo Position | AI-2 | | V1 | volts | Voltage 1 | AO-3 | | V2 | volts | Voltage 2 | AO-4 | | Current1 | amperes | Current 1 | AI-3 | | Current2 | amperes | Current 2 | AI-4 | | Current3 | amperes | Current 3 | AI-6 | | Feedback Type | integer | Feedback type for z-piezo control. See Table S2 details. |   | | Line Number | integer | Indicates the waypoint number being approached (starts = 1 and increments by 1 as each waypoint is reached) |   | | Lock-in Amplitude | amperes[^\[1\]^](#_ftn1) | Oscillation amplitude (rms/peak-to-peak depending on the lock-in model) | AI-5 | | Lock-in phase | degrees | Oscillation phase vs the reference phase (from lock-in amplifier). | AI-7 | | δ*t*~data~ | seconds | Time between data point and the preceding data point (see above for definition) |   |   --- [\[1\]](#_ftnref1) This presupposes that the current is being fed into the lock-in amplifier; a common setup that is shown in Figure S8. If other inputs are fed to the lock-in units will be different. 

Not AvailableScanning electrochemical cell microscopy (SECCM) produces nanoscale-resolution electrochemical maps of electrode surfaces using the meniscus at the tip of an electrolyte-filled nanopipette as a mobile electrochemical cell. While the use and range of applications of SECCM have grown rapidly since its introduction, the pathway to performing SECCM measurements can be daunting to those without direct access to expert users. This work fills this expertise gap by providing a step-by-step guide to performing one’s first SECCM experiments, including troubleshooting strategies, videos/images, suggested parameters and experimental systems, and representative data (of both successful experiments and common problems). No background in SECCM is assumed and fundamentals are clearly explained at each stage with a rationale for the experimental steps provided. This work provides an entry point for the uninitiated to understand and use this powerful nanoscale electrochemical characterization technique. 

{"Abstract":["Scanning electrochemical cell microscopy (SECCM) produces\n nanoscale-resolution electrochemical maps of electrode surfaces using the\n meniscus at the tip of an electrolyte-filled nanopipette as a mobile\n electrochemical cell. While the use and range of applications of SECCM\n have grown rapidly since its introduction, the pathway to performing SECCM\n measurements can be challenging for those without direct access to expert\n users. This work fills this gap by providing a step-by-step guide to\n performing SECCM experiments, including troubleshooting strategies,\n videos/images, suggested parameters and experimental systems, and\n representative data (of both successful experiments and common problems).\n This work provides an entry point for the uninitiated to make use of this\n powerful nanoscale electrochemical characterization technique."],"TechnicalInfo":["# Data from: A tutorial for scanning electrochemical cell microscopy\n (SECCM) measurements: Step-by-Step instructions, visual resources, and\n guidance for first experiments Dataset DOI:\n [10.5061/dryad.3j9kd51v4](10.5061/dryad.3j9kd51v4) ## Description of the\n data and file structure This file contains the data presented in "A\n Tutorial for Scanning Electrochemical Cell Microscopy (SECCM)\n Measurements: Step-by-Step Instructions, Visual Resources, and Guidance\n for First Experiments". ### Files and variables #### File:\n Capacitive\\_current\\_vs\\_scan\\_rate\\_FigS5.txt **Description:** Data for\n Figure S5 Capacitive current vs scan rate ##### Variables * Scan rate\n (V/s): * Capacitive Current (pA): #### File: Clean\\_Detachment\\_Fig17.txt\n **Description: Data for Fig 17 clean detachment**  ##### Variables * z\n (micrometers) * Current (pA) #### File: CV\\_Fig\\_2iA.txt\n **Description:** CV data for Figure 2iA ##### Variables * Potential (mV) *\n Current (pA) #### File: CV\\_Fig\\_2iB.txt **Description:** CV data for\n Figure 2iB ##### Variables * Potential (mV) * Current (pA) #### File:\n CV\\_Fig\\_2iC.txt **Description:** CV data for Figure 2iC ##### Variables *\n Potential (mV) * Current (pA) #### File: CV\\_Fig\\_16A.txt\n **Description:** CV data for Figure 16A ##### Variables * Potential (mV) *\n Current (pA) #### File: CV\\_Fig156.txt **Description:** CV data for Figure\n 16B ##### Variables * Potential (mV) * Current (pA) #### File:\n Electrical\\_Characterization\\_CV\\_Fig12.txt **Description:** CV data for\n Figure 12 ##### Variables * Potential (V) * Current (nA) #### File:\n Electrical\\_Characterization\\_i\\_t\\_Fig11.txt **Description:** Current vs\n time data for figure 11 ##### Variables * Time (s) * Current (nA) ####\n File: OC\\_1Vpers\\_CV\\_Fig5B.txt **Description:** Open circuit 1 V/s CV\n data for figure 5B ##### Variables * Potential (mV) * Current (pA) ####\n File: OC\\_5Vpers\\_CV\\_Fig5B.txt **Description:** Open circuit 5 V/s CV\n data for figure 5B ##### Variables * Potential (mV) * Current (pA) ####\n File: OC\\_Fig\\_5A\\_NoisyOffset.txt **Description:** Open circuit Current\n vs time data for Noisy and offset data in Figure 5A ##### Variables * Time\n (s) * Current (pA) #### File: OC\\_10Vpers\\_CV\\_FigS5.txt\n **Description:** Open circuit 10 V/s CV data for figure S5 ##### Variables\n * Potential (mV) * Current (pA) #### File: OC\\_FigS4\\_DDPCA\n **Description:** Open circuit data DDPCA amplifier Figure S4 #####\n Variables * Potential (V) * Current (pA) #### File: OC\\_Fig5A\\_Desired.txt\n **Description:** Open circuit Current vs time data for desired data in\n Figure 5A ##### Variables * Time (s) * Current (pA) #### File:\n Extended\\_Adhesion\\_Fig17.txt **Description:** Extended adhesion data in\n Figure 17 ##### Variables * Z (micrometers): * Current (nA) #### File:\n OC\\_0.1Vpers\\_CV\\_Fig5B.txt **Description:** Open circuit 0.1 V/s CV data\n for figure 5B ##### Variables * Potential (mV) * Current (pA) #### File:\n SECCM\\_imap\\_Fig2ii.txt **Description:** SECCM Current Map Data Figure 2ii\n ##### Variables * x coordinate (micrometers) * y coordinate (micrometers)\n * Current (pA) #### File: OC\\_FigS4\\_DLPCA **Description:** Open circuit\n data DLPCA amplifier Figure S4 ##### Variables * Potential (V) * Current\n (pA) #### File: SECCM\\_imap\\_Fig16.txt **Description:** SECCM Current map\n data Figure 16 ##### Variables * X (micrometers) * Y (micrometers) *\n Current (pA) #### File: SECCM\\_Z\\_height\\_map\\_FigS15.txt\n **Description:** SECCM topography map data Figure S15 ##### Variables * X\n (micrometers) * Y (micrometers) * Z (micrometers) #### File:\n Resistor\\_Fig6\\_Flatline.tsv **Description:** Flatline response data\n Figure 6 ##### Variables  * Potential (V) * Current (nA) #### File:\n Undesirable\\_CV\\_FigS13B.txt **Description:** Undesirable CV data Figure\n S13B ##### Variables * Potential (mV) * Current (nA) #### File:\n Undesirable\\_CV\\_FigS13A.txt **Description:** Undesirable CV Figure S13A\n ##### Variables * Potential (mV) * Current (nA) #### File:\n SECCM\\_z\\_height\\_map\\_Fig2iii.txt **Description:** SECCM topography map\n data Figure 2iii ##### Variables * x coordinate (micrometers) * y\n coordinate (micrometers) * z height (micrometers) #### File:\n Resistor\\_Fig6\\_Offset.txt **Description:** Offset response data Figure 6\n ##### Variables * Potential (V) * Current (nA) #### File:\n Resistor\\_Fig6\\_Desired.tsv **Description:** Desired resistor response\n data Figure 6 ##### Variables: * Potential (V) * Current (nA) #### File:\n Resistor\\_Fig6\\_Lim\\_current\\_range.tsv **Description:** Limited current\n range data Figure 6 ##### Variables * Potential (V) * Current (nA)"]}