This work was supported by the Korea Institute of Energy Technology Evaluation and Planning (KETEP) and the Ministry of Trade, Industry &#38; Energy (MOTIE) of the Republic of Korea (No. 20214000000280), and the Chung-Ang University Graduate Research Scholarship 2021.

1. Fabrication of electrode and supercapacitor (Figure 1)
<ol>
	<li>Prepare the electrodes prior to the electrochemical analysis by combining 80 weight (wt)% of the electrode active material (0.8 g activated carbon), 10 wt% of the conductive material (0.1 g carbon black), and 10 wt% of the binder (0.1 g polytetrafluoroethylene (PTFE)).
	<ol>
		<li>Drop isopropanol (IPA; 0.1-0.2 mL) into the above-mentioned mixture, then spread the mixture thinly into a dough with a roller.</li>
	</ol>
	</li>
	<li>Before attaching the electrode to stainless steel (SUS) mesh, cut the SUS mesh to dimensions of 1.5 cm (width) &#215; 5 cm (length). After weighing the SUS mesh, coat the electrode (1 cm2) with a thickness of 0.1-0.2 mm on a SUS mesh and compress it with an electrode pressing machine. Here, the mass range of the electrode was 0.001-0.003 g.</li>
	<li>Dry the assembled supercapacitor electrode in an oven at 80 &#176;C for about 1 day to evaporate the IPA.</li>
	<li>Weigh the SUS mesh to obtain the weight of the electrode and then immerse the mesh in the electrolyte (2 M H2SO4 aqueous solution).</li>
	<li>Place the SUS mesh in a desiccator to remove air bubbles at the surface of the supercapacitor electrode.</li>
</ol>
2. Preparation of sequence file for electrochemical analysis
<ol>
	<li>CV sequence settings to obtain the analysis results.
	<ol>
		<li>Run the potentiostat measurement program to set the measurement experiment sequence file (Figure 2A).</li>
		<li>Click the Experiment button in the toolbar and go to Sequence File Editor &#62; New or click the New Sequence button (Figure 2B). Click the Add button to add a sequence step (Figure 3A).</li>
		<li>In every step, set Control as Sweep, Configuration as PSTAT, Mode as CYCLIC, and Range as Auto. Set the Reference for Initial(V) and Middle(V) as Eref and put -200e-3 in the Value. Set the Reference for Final(V) as Eref and put 800e-3 in the Value.</li>
		<li>The voltage scan rate is set as the desired value&#160;by&#160;the user. Here, the scan rate&#160;was&#160;set to 10&#160;mV/s. Put the value in Scanrate(V/s) as 10.0000e-3. Copy step-1 and click Paste[Dn] to paste it to step-2~5. Change the value of Scanrate(V/s) to either 20.000e-3, 30.000e-3, 50.000e-3, and 100.00e-3 respectively.</li>
		<li>Set Quiet time(s) as 0 and Segments as the number 2n+1 where n is the number of cycles. Here, 21 was applied for 10 cycles.</li>
		<li>Set Cut Off Condition as follows: for Condition-1 set Item as Step End and Go Next as Next.</li>
		<li>In the Controlling Miscellaneous Setting section, in the Sampling tab, set Item as Times(s), OP as &#62;=, and DeltaValue as 0.333333 (step-1), 0.166666 (step-2), 0.111111 (step-3), 0.06667 (step-4), and 0.03333&#160;(step-5) for each scan rate. This is the time interval for recording the data.</li>
		<li>Click Save As to save the CV analysis sequence file in any folder of the computer.</li>
	</ol>
	</li>
	<li>GCD sequence settings to obtain the analysis results
	<ol>
		<li>Run the potentiostat measurement program to set the measurement experiment sequence file (Figure 2A).</li>
		<li>Click the Experiment button in the toolbar and go to Sequence File Editor &#62; New or click the New Sequence button (Figure 2B). Click the Add button to add a sequence step (Figure 4A,B).</li>
		<li>In Step-1, set Control as CONSTANT, Configuration as GSTAT, Mode as NORMAL, and Range as Auto. Set the Reference for Current(A) as ZERO. When the mass of the electrode is 0.00235 g, set Value as 1.8618e-3 which means the current density is 1 A/g.</li>
		<li>Set Cut Off Condition as follow: for Condition-1 set Item as Voltage, OP as &#62;=, DeltaValue as 800e-3, and Go Next as Next.</li>
		<li>Set the following in the Controlling Miscellaneous setting section: in the Sampling tab, set Item as Times(s), OP as &#62;=, and DeltaValue as 0.1.</li>
		<li>In Step-2, each set is the same as in Step-1, except set value of Current(A) as the negative value of Step-1 (-1.8618e-3). Set Condition-1 as follows: Item as Voltage, OP as &#60;=, DeltaValue as -200e-3, and Go Next as Next.</li>
		<li>In Step-3, set Control as LOOP, Configuration as CYCLE, and set List-1 in Condition-1 of Cut Off Condition as Loop Next, Go Next as Step-1, and set List-2 as Step End, and Go Next as Next. Set the Iteration value as 10 which is the number of repeating cycles.</li>
		<li>Step-1, step-2, and step-3 form a single loop. Copy and paste them after step-4 and change the value of Current (A) to either 3.7236e-3, 5.5855e-3, 9.3091e-3, or 18.618e-3, calculated for various current densities of 2,3,5, and 10 A/g.</li>
		<li>Click Save As to save the GCD analysis sequence file in any folder of the computer.</li>
	</ol>
	</li>
	<li>EIS sequence settings to obtain the analysis results
	<ol>
		<li>Run the potentiostat measurement program to set the measurement experiment sequence file (Figure 2A).</li>
		<li>Click the Experiment button in the toolbar and go to Sequence File Editor &#62; New or click the New Sequence button (Figure 2B). Click the Add button to add a sequence step (Figure 5A,B).</li>
		<li>In Step-1, set Control as CONSTANT, Configuration as PSTAT, Mode as TIMER STOP, and Range as Auto. Set the Reference for Voltage(V) as Eref and Value as 500e-3 which is half of the size of the voltage range.</li>
		<li>Set cut-off condition as follows: for Condition-1 set Item as Step Time, OP as &#62;=, DeltaValue as 3:00, and Go Next as Next. This is the process for stabilizing the potentiostat device.</li>
		<li>In Step-2, set Control as EIS, Configuration as PSTAT, Mode as LOG, and Range as Auto. Set Speed of Initial (Hz) as Normal and value of Initial (Hz) and Middle (Hz) as 1.0000e+6 which is the high-frequency value and Final (Hz) as 10.000e-6, which is the low-frequency value.</li>
		<li>Set the Reference for Bias(V) as Eref and Value as 500e-3. To get a linear response result, set the amplitude (Vrms) as 10.000e-3. Set Density as 10 and Iteration as 1.</li>
		<li>Click Save as to save the EIS analysis sequence file in any folder of the computer.</li>
	</ol>
	</li>
</ol>
3. Electrochemical analysis
<ol>
	<li>Operate the potentiostat device and run the measurement program to perform the CV, GCD, and EIS analyses. Fill 100 mL of 2 M H2SO4 aqueous electrolyte in a glass container (a beaker-shaped glass container was used).</li>
	<li>Before starting the measurement, in the potentiostat, connect the three types of lines: the working electrode (L-WE), the reference electrode (L-RE), and the counter electrode (L-CE), to the SUS mesh, reference electrode (Ag/AgCl), and counter electrode (Pt wire), respectively (Figure 6). Connect the fourth line, the working sensor (L-WS) to the L-WE.</li>
	<li>Cover the glass container with a cap, and immerse the three electrodes in the electrolyte through a perforation in the cap. Position the electrodes so that the WE is maintained at a constant distance between the CE and RE.</li>
	<li>Run the measurement program and open the prepared sequence. Click Apply to CH to insert the sequence to the potentiostat&#39;s channel. Start the measurement by clicking the Start button.</li>
</ol>
4. Data analysis
<ol>
	<li>CV data analysis for fitting the graph
	<ol>
		<li>Open raw measurement data in the convert program to obtain the results in spreadsheet format. Click the File button and open the raw data. Select all cycles and click Export ASCII on the toolbar. Check the Cycle, Voltage, and Current in Columns to Export on the right side of the program.</li>
		<li>Click Create Directory and then click Export to convert raw data to spreadsheet format.</li>
		<li>Open the spreadsheet file and extract the voltage and current values of cycles 10, 20, 30, 40, and 50, which are the last cycles at each scan rate.</li>
		<li>Plot the CV graph with the voltage as the X-axis and specific current density as the Y-axis.</li>
	</ol>
	</li>
	<li>GCD data analysis for fitting the graph
	<ol>
		<li>Open raw measurement data in the convert program to obtain the results in spreadsheet format. Click the File button and open the raw data. Select all cycles and click Export ASCII on the toolbar. Check the Cycle, Voltage, and CycleTime in Columns to Export on the right side of the program.</li>
		<li>Click Create Directory and then click Export to convert raw data to spreadsheet format.</li>
		<li>Open the spreadsheet file and extract the voltage and CycleTime values for cycles 10, 20, 30, 40, and 50, which are the last cycles at each current density.</li>
		<li>Plot the GCD graph with the cycle time as the X-axis and voltage as the Y-axis.</li>
	</ol>
	</li>
	<li>EIS data analysis for fitting the graph
	<ol>
		<li>Open raw measurement data in EIS program. Click the Open file icon and open raw data and click the file name that was applied to see the detailed data.</li>
		<li>Extract Z&#39; [Ohm] as the X value and Z&#39;&#39; [Ohm] as the Y value and plot the EIS graph.</li>
	</ol>
	 </li>
</ol>

The authors have nothing to disclose.

This study provides a protocol for various analyses using a three-electrode system with a potentiostat device. This system is widely used to evaluate the electrochemical performance of supercapacitors. A suitable sequence for each analysis (CV, GCD, and EIS) is important for obtaining optimized electrochemical data. Compared with the two-electrode system having a simple setup, the three-electrode system is specialized for analyzing supercapacitors at the material level15. However, the selection of...

Supercapacitors have attracted enormous attention as suitable power sources for a variety of applications such as microelectronic devices, electric vehicles (EVs), and stationary energy storage systems. In EV applications, supercapacitors can be used for rapid acceleration and can enable the storage of regenerative energy during the deceleration and braking processes. In renewable energy fields, such as solar power generation1 and wind power generation2, supercapacitors can be used as stationary energy storage systems3,4. Renewable energy generation is limited by the fluctuating and intermittent nature of these energy supplies; therefore, an energy storage system that can respond immediately during irregular power generation is required5. Supercapacitors, which store energy via mechanisms that differ from those of lithium-ion batteries, exhibit a high power density, stable cycle performance, and fast charging-discharging6. Depending on the storage mechanism, supercapacitors can be distinguished into double-layer capacitors (EDLCs) and pseudocapacitors7. EDLCs accumulate electrostatic charge at the electrode surface. Therefore, the capacitance is determined by the amount of charge, which is affected by the surface area and porous structure of the electrode materials. By contrast, pseudocapacitors, which consist of conducting polymers and metal oxide materials, store charge through a Faradaic reaction process. The various electrochemical properties of supercapacitors are related to the electrode materials, and developing new electrode materials is the main issue in improving the performance of supercapacitors8. Hence, evaluating the electrochemical properties of these new materials or systems is important in the progress of research and further applications in real life. In this regard, electrochemical evaluation using a three-electrode system is the most basic and widely utilized method in lab-scale research of energy storage systems9,10,11,12,13.
The three-electrode system is a simple and reliable approach for evaluating the electrochemical properties, such as the specific capacitance, resistance, conductivity, and cycle life of supercapacitors14. The system offers the benefit of enabling analysis of the electrochemical characteristics of single materials15, which is in contrast to the two-electrode system, where the characteristics can be studied through the analysis of the given material. The two-electrode system just gives information about the reaction between two electrodes. It is suitable for analyzing the electrochemical properties of the entire energy storage system. The potential of the electrode is not fixed. Therefore, it is not known at what voltage the reaction takes place. However, three-electrode system analyzes only one electrode with fixing potential which can perform a detailed analysis of the single electrode. Therefore, the system is targeted toward analyzing the specific performance at the material level. The three-electrode system consists of a working electrode (WE), reference electrode (RE), and counter electrode (CE)16,17. The WE is the target of research, assessment as it performs the electrochemical reaction of interest18 and is composed of a redox material that is of potential interest. In the case of EDLCs, utilizing high surface area materials is the main issue. Therefore, porous materials with a high surface area and micropores, such as porous carbon, graphene, and nanotubes, are preferred19,20. Activated carbon is the most common material for EDLCs because of its high specific area (&#62;1000 m2/g) and many micropores. Pseudocapacitors are fabricated with materials that can undergo a Faradaic reaction21. Metal oxides (RuOx, MnOx, etc.) and conducting polymers (PANI, PPy, etc.) are commonly used22. The RE and CE are used to analyze the electrochemical properties of the WE. The RE serves as a reference for measuring and controlling the potential of the system; the normal hydrogen electrode (NHE) and Ag/AgCl (saturated KCl) are generally chosen as the RE23. The CE is paired with the WE and completes the electrical circuit to allow charge transfer. For the CE, electrochemically inert materials are used, such as platinum (Pt) and gold (Au)24. All components of the three-electrode system are connected to a potentiostat device, which controls the potential of the entire circuit.
Cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) are typical analytical methods that use a three-electrode system. Various electrochemical characteristics of supercapacitors can be assessed using these methods. CV is the basic electrochemical method used to investigate the electrochemical behavior (electron transfer coefficient, reversible or irreversible, etc.) and capacitive properties of material during repeated redox processes14,24. The CV plot shows redox peaks related to the reduction and oxidation of the material. Through this information, researchers can evaluate the electrode performance and determine the potential where the material is reduced and oxidized. Furthermore, through CV analysis, it is possible to determine the amount of charge that material or electrode can store. The total charge is a function of the potential, and the capacitance can be easily calculated6,18. Capacitance is the main issue in supercapacitors. A higher capacitance represents the ability to store more charge. EDLCs give rise to rectangular CV patterns with linear lines so that the capacitance of the electrode can be calculated easily. Pseudocapacitors present redox peaks in rectangular plots. Based on this information, researchers can assess the electrochemical properties of materials using CV measurements18.
GCD is a commonly employed method for identifying the cycle stability of an electrode. For long-term use, the cycle stability should be verified at a constant current density. Each cycle consists of charge-discharge steps14. Researchers can determine the cycle stability through variations in the charge-discharge graph, specific capacitance retention, and Coulombic efficiency. EDLCs give rise to a linear pattern; thus, the specific capacitance of the electrode can be calculated easily using the slope of the discharge curve6. However, pseudocapacitors exhibit a nonlinear pattern. The discharge slope varies during the discharging process7. Furthermore, the internal resistance can be analyzed through the current-resistance (IR) drop, which is the potential drop owing to the resistance6,25.
EIS is a useful method for identifying the impedance of energy storage systems without destruction of the sample26. The impedance can be calculated by applying a sinusoidal voltage and determining the phase angle14. The impedance is also a function of the frequency. Therefore, the EIS spectrum is acquired over a range of frequencies. At high frequencies, kinetic factors such as the internal resistance and charge transfer are operative24,27. At low frequencies, the diffusion factor and Warburg impedance can be detected, which are related to mass transfer and thermodynamics24,27. EIS is a powerful tool for analyzing the kinetic and thermodynamic properties of a material at the same time28. This study describes the analysis protocols for evaluating the electrochemical performance of supercapacitors using a three-electrode system.

<table><tbody><tr><td>Activated carbon</td><td>GS</td><td></td><td>Active material</td></tr><tr><td>Ag/AgCl electrode</td><td>BASi</td><td>RE-5B</td><td>Reference electrode</td></tr><tr><td>Carbon black</td><td>Hyundai</td><td></td><td>Conductive material</td></tr><tr><td>Desicator</td><td>Navimro</td><td></td><td></td></tr><tr><td>Electrode pressing machine</td><td>Rotech</td><td></td><td></td></tr><tr><td>Extractor</td><td>WonA Tech</td><td></td><td>Convert program (raw data to excel form)</td></tr><tr><td>Isopropanol(IPA)</td><td>Samchun</td><td>I0346</td><td>Solvent to melt the binder</td></tr><tr><td>Polytetrafluoroethylene(PTFE)</td><td>Hyundai</td><td></td><td>Binder</td></tr><tr><td>Potentiostat</td><td>WonA Tech</td><td>Zive SP1</td><td></td></tr><tr><td>Pt electrode</td><td>BASi</td><td>MW-018122017</td><td>Counter electrode</td></tr><tr><td>Reaction flask</td><td>Duran</td><td></td><td>Container for electrolyte</td></tr><tr><td>SM6</td><td>WonA Tech</td><td></td><td>Program of setting sequence and measuring electrochemical result</td></tr><tr><td>Sulfuric acid</td><td>Samshun</td><td>S1423</td><td>Electrolyte</td></tr><tr><td>SUS mesh</td><td>Navimro</td><td></td><td>Current collector</td></tr><tr><td>Teflon cap</td><td>WonA Tech</td><td></td><td>Cap of the electrolyte continer</td></tr><tr><td>Zman</td><td>WonA Tech</td><td></td><td>EIS program</td></tr></tbody></table>

evaluating the electrochemical properties of supercapacitors using the three-electrode system

The three-electrode system is a basic and general analytical platform for investigating the electrochemical performance and characteristics of energy storage systems at the material level. Supercapacitors are one of the most important emergent energy storage systems developed in the past decade. Here, the electrochemical performance of a supercapacitor was evaluated using a three-electrode system with a potentiostat device. The three-electrode system consisted of a working electrode (WE), reference electrode (RE), and counter electrode (CE). The WE is the electrode where the potential is controlled and the current is measured, and it is the target of research. The RE acts as a reference for measuring and controlling the potential of the system, and the CE is used to complete the closed circuit to enable electrochemical measurements. This system provides accurate analytical results for evaluating electrochemical parameters such as the specific capacitance, stability, and impedance through cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS). Several experimental design protocols are proposed by controlling the parameter values of the sequence when using a three-electrode system with a potentiostat device to evaluate the electrochemical performance of supercapacitors. Through these protocols, the researcher can set up a three-electrode system to obtain reasonable electrochemical results for assessing the performance of supercapacitors.

The electrodes were manufactured according to protocol step 1 (Figure 1). Thin and homogeneous electrodes were attached to SUS mesh with a size of 1 cm2 and 0.1-0.2 mm thickness. After drying, the weight of the pure electrode was obtained. The electrode was immersed in a 2 M H2SO4 aqueous electrolyte, and the electrolyte was allowed to sufficiently permeate the electrode before the electrochemical analyses. The production sequence and system setting for the e...

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Evaluating the Electrochemical Properties of Supercapacitors using the Three-Electrode System

The protocol describes the evaluation of various electrochemical properties of supercapacitors using a three-electrode system with a potentiostat device.

The three-electrode system is a basic and general analytical platform for investigating the electrochemical performance and characteristics of energy ...

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11.7K Views.  Chung-Ang University. The protocol describes the evaluation of various electrochemical properties of supercapacitors using a three-electrode system with a potentiostat device.

Video: Evaluating the Electrochemical Properties of Supercapacitors using the Three-Electrode System

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Scanning electrochemical microscopy (SECM) is used to measure the local electrochemical behavior of liquid/solid, liquid/gas and liquid/liquid interfaces. Atomic force microscopy (AFM) is a versatile tool to characterize micro- and nanostructure in terms of topography and mechanical properties. However, conventional SECM or AFM provides limited laterally resolved information on electrical or electrochemical properties at nanoscale. For instance, the activity of a nanomaterial surface at crystal facet levels is difficult to resolve by conventional electrochemistry methods. This paper reports the application of a combination of AFM and SECM, namely, AFM-SECM, to probe nanoscale surface electrochemical activity while acquiring high-resolution topographical data. Such measurements are critical to understanding the relationship between nanostructure and reaction activity, which is relevant to a wide range of applications in material science, life science and chemical processes. The versatility of the combined AFM-SECM is demonstrated by mapping topographical and electrochemical properties of faceted nanoparticles (NPs) and nanobubbles (NBs), respectively. Compared to previously reported SECM imaging of nanostructures, this AFM-SECM enables quantitative assessment of local surface activity or reactivity with higher resolution of surface mapping.

Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope AFM-SECM

Atomic force microscopy (AFM) combined with scanning electrochemical microscopy (SECM), namely, AFM-SECM, can be used to simultaneously acquire high-resolution topographical and electrochemical information on material surfaces at nanoscale. Such information is critical to understanding heterogeneous properties (e.g., reactivity, defects, and reaction sites) on local surfaces of nanomaterials, electrodes and biomaterials.

Scanning electrochemical microscopy (SECM) is used to measure the local electrochemical behavior of liquid/solid, liquid/gas and liquid/liquid interfaces. ...

Synthesizing a Gel Polymer Electrolyte for Supercapacitors, Assembling a Supercapacitor Using a Coin Cell, and Measuring Gel Electrolyte Performance

Supercapacitors (SC) have attracted attention as energy storage devices due to their high density and long cycle performance. SCs used in devices operating in stretchable systems require stretchable electrolytes. Gel polymer electrolytes (GPEs) are an ideal replacement for liquid electrolytes. Polyvinyl alcohol (PVA) and polyvinylidene fluoride-co-hexafluoropropylene (PVDF-HFP) have been widely applied as a polymer-matrix-based electrolytes for supercapacitors because of their low cost, chemically stable, wide operating temperature range, and high ionic conductivities. Herein, we describe the procedures for (1) synthesizing a gel polymer electrolyte with PVA and PVDF-HFP, (2) measuring the electrochemical stability of the gel polymer electrolytes by cyclic voltammetry (CV), (3) measuring the ionic conductivity of the gel polymer electrolytes by electrochemical impedance spectroscopy (EIS), (4) assembling symmetric coin cells using activated carbon (AC) electrodes with the PVA- and PVDF-HFP-based gel polymer electrolytes, and (5) evaluating the electrochemical performance using galvanostatic charge-discharge analysis (GCD) and CV at 25 &#176;C. Additionally, we describe the challenges and insights gained from these experiments.

We present a protocol to test the electrochemical and physical properties of a supercapacitor gel polymer electrolyte using a coin cell.

Supercapacitors (SC) have attracted attention as energy storage devices due to their high density and long cycle performance. SCs used in devices ...

Chronoamperometry Analysis of EET in Lactiplantibacillus plantarum with DHNA

Characterizing Mediated Extracellular Electron Transfer in Lactic Acid Bacteria with a Three-Electrode, Two-Chamber Bioelectrochemical System

Many bacteria perform extracellular electron transfer (EET), whereby electrons are transferred from the cell to an extracellular terminal electron acceptor. This electron acceptor can be an electrode and electrons can be delivered indirectly via a redox-active mediator molecule. Here, we present a protocol to study mediated EET in Lactiplantibacillus plantarum, a probiotic lactic acid bacterium widely used in the food industry, using a bioelectrochemical system. We detail how to assemble a three-electrode, two-chambered bioelectrochemical system and provide guidance on characterizing EET in the presence of a soluble mediator using chronoamperometry and cyclic voltammetry techniques. We use representative data from 1,4-dihydroxy-2-naphthoic acid (DHNA)-mediated EET experiments with L. plantarum to demonstrate data analysis and interpretation. The techniques described in this protocol can open new opportunities for electro-fermentation and bioelectrocatalysis. Recent applications of this electrochemical technique with L. plantarum demonstrated an acceleration of metabolic flux towards producing fermentation end-products, which are critical flavor components in food fermentation. As such, this system has the potential to be further developed to alter flavors in food production or produce valuable chemicals.

Here we present a protocol for characterizing mediated extracellular electron transfer (EET) in lactic acid bacteria using a three-electrode, two-chamber bioelectrochemical system. We illustrate this method with Lactiplantibacillus plantarum and the redox mediator 1,4-dihydroxy-2-naphthoic acid and provide a thorough description of the electrochemical techniques used to evaluate mediated EET.

Many bacteria perform extracellular electron transfer (EET), whereby electrons are transferred from the cell to an extracellular terminal electron ...

Biochemistry

Electrochemical Measurements of Supported Catalysts Using a Potentiostat/Galvanostat

Source: Laboratory of Dr. Yuriy Rom&#225;n &#8212; Massachusetts Institute of Technology
A potentiostat/galvanostat (often referred to as simply a potentiostat) is an instrument that measures current at an applied potential (potentiostatic operation) or measures potential at an applied current (galvanostatic operation) (Figure 1). It is the most commonly used instrument in the electrochemical characterization of anode and cathode materials for fuel cells, electrolyzers, batteries, and supercapacitors.
Conventionally, these anode and cathode materials are interfaced with a potentiostat via a three-electrode electrochemical cell. The electrode leads from the potentiostat are connected to the reference electrode, the counter electrode (often called the auxiliary electrode), and the working electrode (which contains the test material of interest). The electrochemical cell is then filled with a high ionic strength electrolyte solution, such as an acidic, alkaline, or salt solution. The media for this high ionic strength solution is typically aqueous; however, for applications necessitating higher operating cell potential windows, such as batteries and supercapacitors, non-aqueous media is often used. The cell media is degassed with an inert gas (to prevent unwanted side reactions) or with a test gas (if the test reaction involves a gas at one of the electrodes).
Alternatively, a salt bridge or membrane is employed to maintain ionic contact if the two half cells are to be measured in different electrolytes. In heterogeneous electrocatalysis, this type of &#34;two compartment&#34; cell is often used if the test molecule at the working electrode is also reactive at the counterelectrode. This happens frequently as the counterelectrode typically employed is platinum, which is a highly active catalyst for many reactions. Here, single compartment cells will be used, where all three electrodes are in the same media.
This video will explain the process of polishing a working electrode, preparing a catalyst ink, mounting the catalyst ink onto the working electrode, preparing the electrochemical cell, and then performing electrochemical measurements. The measurements that are performed include: cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronopotentiometry (CP), and chronoamperometry (CA).
<img alt="Figure 1" src="/files/ftp_upload/5698/5698fig1.jpg" /> 
Figure 1. An example of a single compartment electrochemical cell. a.) Teflon cap, b.) glass cell, c.) Pt wire counter electrode, d.) working electrode, e.) Ag/AgCl reference electrode, f.) 0.5 M aqueous sulfuric acid electrolyte solution.