Planar Electrodes Research Articles

Second-Harmonic Nonlinear Electrochemical Impedance Spectroscopy: Part I. Analytical Theory and Equivalent Circuit Representations for Planar and Porous Electrodes

Analytical theory for second harmonic nonlinear electrochemical impedance spectroscopy (2nd-NLEIS) of planar and porous electrodes is developed for interfaces governed by Butler-Volmer kinetics, a Helmholtz (mainly) or Gouy-Chapman (introduced) double layer, and transport by ion migration and diffusion. A continuum of analytical EIS and 2nd-NLEIS models is presented, from nonlinear Randles circuits with or without diffusion impedances to nonlinear macrohomogeneous porous electrode theory that is shown to be analogous to a nonlinear transmission-line model. EIS and 2nd-NLEIS for planar electrodes share classic charge transfer RC and diffusion time-scales, whereas porous electrode EIS and 2nd-NLEIS share three characteristic time constants. In both cases, the magnitude of 2nd-NLEIS is proportional to nonlinear charge transfer asymmetry and thermodynamic curvature parameters. The phase behavior of 2nd-NLEIS is more complex and model-sensitive than in EIS, with half-cell NLEIS spectra potentially traversing all four quadrants of a Nyquist plot. We explore the power of simultaneously analyzing the linear EIS and 2nd-NLEIS spectra for two-electrode configurations, where the full-cell linear EIS signal arises from the sum of the half-cell spectra, while the 2nd-NLEIS signal arises from their difference.

Electrochemical fabrication and characterizations of Ag/AgCl pseudo-reference electrode: a preliminary study

In this work Ag/AgCl planar pseudo-reference electrodes (pREs) were fabricated and studied. The pRE was derived from typical copper-cladded flame retardant 4 (FR4) board, with layers of Ni, Au, and Ag electrochemically deposited sequentially. Lastly, the AgCl layer was obtained through electro-chlorination process. The morphology and Open Circuit Potential (OCP) of the samples were obtained from characterizations. It was revealed that the Au layer consisted of finer grains compare to that of Ag having larger granular structure. There was also morphological difference between as-prepared AgCl and post OCP run AgCl, where the later show signs of degradation. Based on the potential-transient curve of electro-chlorination, chlorination process took place on the surface of Ag, subsequently diffused into the bulk layer. Sample chlorinated for 1 min shows better stability in OCP test where the potential exhibit minimum changes. The duration of the sample being stable during electrochemical process was 10 minutes.

Surface and Conductivity Characterization of Layered Organic Ionic Plastic Crystal (OIPC)-Polymer Films.

Organic ionic plastic crystals (OIPCs) are attractive solid electrolyte materials for advanced energy storage systems owing to their inherent advantages (e.g., high plasticity, thermal stability, and moderate ionic conductivity), which can be further improved/deteriorated by the addition of polymer or metal oxide nanoparticles. The role of the nanoparticle/OIPC combinations on the resultant interphase structure and transport properties, however, is still unclear due to the complexity within the composite structures. Herein, we demonstrate a systematic approach to specifically interrogating the interphase region by fabricating layered OIPC/polymer thin films via spin coating and correlating variation in the ionic conductivity of the OIPC with their microscopic structures. In-plane interdigitated electrodes have been employed to obtain electrochemical impedance spectroscopy (EIS) spectra on both OIPC and layered OIPC/polymer thin films. The thin-film EIS measurements were evaluated with conventional bulk EIS measurements on the OIPC pressed pellets and compared with EIS obtained from the OIPC-polymer composites. Interactions between the OIPC and polymer films as well as the morphology of the film surfaces have been characterized through multiple microscopic analysis tools, including scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, and optical profilometry. The combination of EIS analysis with the microscopic visualization of these unique layered OIPC/polymer thin films has confirmed the impact of the OIPC-polymer interphase region on the overall ionic conductivity of bulk OIPC-polymer composites. By changing the chemistry of the polymer substrate (i.e., PMMA, PVDF, and PVDF-HFP), the importance of compatibility between the components in the interphase region is clearly observed. The methods developed here can be used to screen and further understand the interactions among composite components for enhanced compatibility and conductivity.

Circularly Polarized Ultra-Wideband Antenna for Uni-Traveling-Carrier Photodiode Terahertz Source

This paper proposes a circularly polarized ultra-wideband (UWB) antenna for a Uni-Traveling-Carrier Photodiode (UTC-PD) to meet the growing demand for bandwidth and polarization diversity in terahertz (THz) communication. In the design of the UTC-PD integrated antenna, the planar electrodes of the chip are directly integrated with the antenna to simplify the integration process. However, this integration introduces new problems, such as asymmetry inside the spiral antenna, which leads to a deterioration in the corresponding high-frequency performance. To address this issue, the antenna’s structure is optimized, and a lens is integrated to enhance directivity and eliminate surface waves. As a result, the proposed antenna achieves a 100–1500 GHz (175%) impedance bandwidth and a 150–720 GHz (131%) axial ratio bandwidth for the UTC-PD. The maximum gain of the antenna is 21.05 dBi at 1 THz.

High-redox-capacity solid contact based on ferrocenyl self-assembled monolayer functionalized macroporous gold for an all-solid-state carbonate-selective electrode

Solid-contact ion-selective electrodes (ISEs) are a promising tool for direct detection of CO32– activity/concentration in seawater. Herein, a stable solid-contact CO32–-ISE was fabricated based on ferrocenyl self-assembled monolayer (SAM) functionalized macroporous gold (m-PG). Instead of the commonly used planar electrode, the m-PG film, prepared by using an electrochemical self-templating method involving the gold electrodeposition and hydrogen bubbling generation, is used as the conductive substrate. The redox capacity of the ferrocenyl SAM on the m-PG film is much larger than that on the planar Au electrode, due to the high surface area and good conductivity of m-PG. The solid-contact CO32–-ISE based on ferrocenyl SAM modified m-PG shows a Nernstian potential response in the activity range from 2.6 × 10-5 to 5.3 × 10-4 M with a slope of 28.3 ± 0.4 mV/dec and a detection limit of 1.1 × 10-5 M. The proposed electrode also exhibits a good electrode-to-electrode reproducibility with a standard variation of the standard potential (E0) of 1.5 mV (n = 7), an improved potential stability and a long lifetime up to at least 120 days. The strategy for electrode substrate transformation from planar gold substrate to porous gold substrate provides an alternative way to improve the redox capacities of ferrocenyl SAMs for preparing the stable and reliable solid-contact ISEs.

Treatment of landfill leachate nanofiltration concentrate by a three-dimensional electrochemical technology with waste aluminum scraps as particle electrodes: Efficacy, mechanisms, and enhancement effect of subsequent electrocoagulation

Landfill leachate nanofiltration concentrate is a kind of wastewater containing high concentrations of color and refractory organics. Herein, we proposed a novel three-dimensional electrochemical technology (3DET) with waste aluminum scraps as particle electrodes for its treatment. The planar and particle electrodes were first optimized. Ti/RuO2 and graphite were used as anodes in the two-dimensional electrochemical technology (2DET). In the light of contaminant removal (color, UV254, COD, and TOC), chlorine reduction, and energy consumption, graphite was selected as planar anodes and cathodes. Moreover, 3DET with Al particle electrodes (Al 3DET) outperformed that with conventional granular activated carbon electrodes, 2DET, and Al particles. At 120 min, the removal efficiencies of color, UV254, COD, and TOC using Al 3DET were 98.94 %, 84.72 %, 51.93 %, and 67.46 %, respectively. UV–vis and EEM spectroscopy, and GC–MS analyses indicate that macromolecular organic matter such as humic-like substances could be effectively degraded and simultaneously removed. Reactive species identification tests including free radical quenching and EPR spectra were conducted. The results indicate that in addition to anodic direct oxidation, indirect oxidation by oxidative species (H2O2, •OH, and RCS) and flocculation by Al species also played a vital role in contaminant removal. Continuous-flow experiments show that Fe EC as a post-treatment step of Al 3DET could effectively provide a neutralization effect for the 3DET effluent and enhance the removal efficiency of contaminants. The total operating cost of combined process was 1.307 USD/m3. This study shows that the Al 3DET-Fe EC process is a promising technology for the treatment of nanofiltration concentrate.

Analyzing the electrochemical reduction of CO and CO2 as reactants to C1 and C2 products on copper-based flow-through gas diffusion electrodes

Electrochemical CO2 reduction (eCO2R) into useful chemicals and fuels is extensively studied, but it faces challenges such as high activation energy, carbonation, lower reaction rate, and unstable operation in alkaline conditions. In contrast, electrochemical CO reduction (eCOR) can efficiently produce C2+ products through a two-step conversion process without requiring high activation energy and involving complex reaction routes like CO2 electroreduction. Therefore, Converting CO2 to CO and then to C2+ products can be a strategic approach to enhance activity, selectivity, and economic viability. However, eCOR demonstrates lower reaction rates and sluggish kinetic with planar electrodes due to its lower solubility and poor mass transport to the electrode surface, therefore, industrially relevant current densities are still far to reach. Flow-through gas diffusion electrodes (FTGDEs) can potentially solve the issue of poor mass transport due to their abundant surface area, porous structure, and improved triple-phase interface. Herein, electrochemical CO reduction to C2+ products is investigated using Cu-based FTGDEs. A comparison of eCOR with eCO2R is also carried out to study the catalytic activity, selectivity, and stability. To demonstrate the influence of particle size, FTGDEs are designed using varying Cu particle sizes i.e. 10 nm, 100 nm, and 10 µm. The eCOR produced C2+ products with ethylene being the main product achieving 474 mA/cm2 current density and 72% faradaic efficiency at − 0.9 V vs. RHE, while eCO2R yielded more C1 products with lower catalytic activity and selectivity. Compared to gas diffusion configuration, the poor catalytic activity and selectivity of eCOR are observed in non-gas diffusion configuration which signifies that, due to higher local CO concentration and improved triple-phase generation, higher performance of FTGDEs can be obtained from gas diffusion configuration. Finally, the stable operation of Cu electrodes during eCOR highlights its promise as a highly suitable candidate for enhancing eCOR towards higher carbon products.

Planar Patch Clamp and Techniques of Patch-Clamp Spectroscopy in Antimicrobial Therapy

Planar patch-clamp is an effective screening tool in pharmacology, institutionalized in molecular microbiology over 15 years ago [1]. The creation of planar polymer patch-clamp electrodes and silicon substrates in the 2000s [2,3] and the creation of microfluidic chips and perfusable chambers corresponding to this pharmacological screening technology, although works on the development of microfluidic chips for planar patch-clamp were already being published in the early to mid-2000s, and the first "benchmark study" of a chip for planar patch-clamp dates back to 2003 [4,5]. At the moment, there are automated and robotic schemes for planar patch-clamp, including those available for sale and maintenance [6-8]. In the CIS, this method is not widespread, however, devices such as the "Patchliner" with planar patch-clamp, capable of recording up to 8 cells synchronously, are available [9-11]. Patch-clamp tools can be used in the development of drugs and antimicrobial agents, screening of which can be performed on E. coli, etc. [12-14]. The response of the organism mediated by lysosomes can also be the subject of using this method, as lysosomal ion currents can also be measured in planar patch-clamp systems [PMID: 21139138].

Multiscale modelling of species transport in hydrophilic Nafion®-coated Cu catalysts for CO2 electro-reduction

Ionomers such as Nafion are being used for engineering the microenvironment of the CO2RR towards selectivity to higher hydrocarbons. Their cationic exchange qualities mitigate homogeneous bicarbonate reactions, providing favourable conditions for production of C2-C3 products. The proximity of Nafion® layers to the negatively charged electrode surface results in complex effects that have yet to be explored computationally. We combine mass transport equations and density functional theory (DFT) calculations to model the hydrophilic moieties in Nafion® layer on a 1D planar copper electrode. We vary the Nafion® layer thickness in the thick film regime (200–1100 nm), the ionic strength of supporting aqueous electrolyte and the applied voltage to investigate the concentration profile of participating species within the Nafion® layer. We find that the bicarbonate ion concentration and local pH decrease with decreasing thickness which makes thinner films better at mitigating bicarbonates at the cost of a relatively lower pH. We observe the breakdown of Donnan exclusion effects with higher ionic strength electrolytes which allows diffusion of both co-ions and counter-ions, promoting the bicarbonate reactions. Further, we find that the pKa of Nafion® generally increases as the local dielectric constant of the reaction medium decreases. This is primarily due to the accumulation of K+ and production of low dielectric constant products such as ethanol, albeit their concentrations are low on planar Cu electrodes. The lower permittivity of the reaction medium weakens the exclusion forces and changes the morphology of Nafion® which ultimately impacts its ability to mitigate homogeneous bicarbonate reactions.

Highly Stable Vertically Oriented 2H‐NbS2 Nanosheets on Carbon Nanotube Films toward Superior Electrocatalytic Activity

Abstract2D metallic transition‐metal dichalcogenides (MTMDCs) have attracted widespread research interest in the exploration of fundamental physical issues and energy‐related fields. Although relatively high catalytic activity has been predicted theoretically in the new type MTMDCs‐based electrocatalysts, their hydrogen evolution reaction (HER) performance is severely hampered by the insufficient catalytic stability due to structural degradation during long‐time use and limited active sites in planar electrode structures. Herein, the scalable synthesis of vertically‐oriented 2H‐NbS2 nanosheets is reported on low‐cost carbon nanotube (CNT) film substrates by a facile chemical vapor deposition route. The 3D vertically‐oriented 2H‐NbS2 nanosheets present abundant edge active sites and strong interface coupling with CNT thus possessing exceptional mechanical stability. These features impart the 3D nanosheets catalysts with remarkably low overpotentials of ≈55 mV at 10 mA cm−2 and ultra‐high exchange current density of ≈1445 µA cm−2, and negligible performance degradation after 200 h operation at the large current density, which are superior to those of other TMDCs‐based catalysts. This work hereby provides novel perspectives for the batch synthesis and application of 3D MTMDCs‐based electrocatalysts with greatly improved electrocatalytic performance and stability that are needed for practical applications.

The discharge characteristics and benzene degradation performance of a three-electrode DBD reactor powered by dual AC power generators

A three-electrode hybrid volume/surface dielectric barrier discharge (V-SDBD) configuration with two plane electrodes and six grounded strips electrode was designed for enhancing the generation of discharge plasma to degrade gaseous benzene. Two plane electrodes were separately powered by a 5 kHz AC generator and a 50 Hz AC generator, respectively. Compared with the typical two-electrode volume DBD (VDBD) reactor excited by 50 Hz AC generator, the hybrid V-SDBD reactor has lower onset discharge voltage and better discharge homogeneity, and the benzene degradation efficiency of V-SDBD was 1.12 times higher than that of VDBD at a similar energy efficiency. Moreover, an increase in the voltage on HVE-II promoted benzene degradation, but decreased the energy efficiency of benzene degradation.

Supersonic Flow past a Sharp Plate with Surface Anomalous Glow Discharge in a Magnetic Field

The electrodynamic structure of an anomalous glow discharge between two plane electrodes located on the surface of a sharp plate in supersonic flow of molecular nitrogen is studied numerically in a wide range of Mach numbers using a modified ambipolar model of quasi-neutral electric-discharge plasma. The ambipolar diffusion coefficient and the effective ionization rate are modified while taking into account the external magnetic field. The problem is solved in the two-dimensional x–y formulation, when the external magnetic field strength is directed in the positive or negative direction of the z axis. The parameters of anomalous glow discharge are numerically studied in the pressure range p = 0.14–5 Torr and the voltage drops on the quasineutral current column of discharge plasma V = 30–320 V. The main problem parameters which make it possible to obtain a reasonable agreement with the available experimental data are determined.

Fabrication of Ni-Cr-FeOx ceramic supercapacitor electrodes and devices by one-step electric discharge ablation

This investigation addresses the need in the development of a facile, low-cost and computer-aided design method to fabricate ceramic supercapacitors, based on patterned metal oxide films. It is motivated by the promising advantages of planar electrode arrangement for the fabrication of ceramic supercapacitors operating at extremely high charge-discharge rates. Herein, one-step electric discharge ablation (EDA) technique is developed for fabricating Ni-Cr-FeOx electrodes using commercial 304 stainless steel current collectors for the first time. The binder-free, noble materials-free, toxic chemical-free and conductive additives-free Ni-Cr-FeOx based in-plane microsupercapacitors (IMSC) are fabricated by the EDA technique. The obtained IMSC delivers a high areal capacitance of 38.3 mF cm−2 at 1 mV s−1 and shows superior capacitive behavior at an ultrahigh scan rate of 152,000 mV s−1, which is >760 times higher than the reported values for ceramic metal oxide based electrodes in the literature. This one-step, low-cost, environmental friendly, and automatic fabrication method is promising for the scale-up synthesis of various ceramic metal oxides and fabrication of supercapacitor devices.

Electric field bridging-effect in electrified microfibrils' scaffolds.

Introduction: The use of biocompatible scaffolds combined with the implantation of neural stem cells, is increasingly being investigated to promote the regeneration of damaged neural tissue, for instance, after a Spinal Cord Injury (SCI). In particular, aligned Polylactic Acid (PLA) microfibrils' scaffolds are capable of supporting cells, promoting their survival and guiding their differentiation in neural lineage to repair the lesion. Despite its biocompatible nature, PLA is an electrically insulating material and thus it could be detrimental for increasingly common scaffolds' electric functionalization, aimed at accelerating the cellular processes. In this context, the European RISEUP project aims to combine high intense microseconds pulses and DC stimulation with neurogenesis, supported by a PLA microfibrils' scaffold. Methods: In this paper a numerical study on the effect of microfibrils' scaffolds on the E-field distribution, in planar interdigitated electrodes, is presented. Realistic microfibrils' 3D CAD models have been built to carry out a numerical dosimetry study, through Comsol Multiphysics software. Results: Under a voltage of 10V, microfibrils redistribute the E-field values focalizing the field streamlines in the spaces between the fibers, allowing the field to pass and reach maximum values up to 100kV/m and values comparable with the bare electrodes' device (without fibers). Discussion: Globally the median E-field inside the scaffolded electrodes is the 90% of the nominal field, allowing an adequate cells' exposure.

Development of a Method for Multisensory Stripping Voltammetry in the Analysis of Medical Preparations.

For the effective dosage of newly developed ophthalmic drugs, an assessment of the dynamics of their concentration in lacrimal fluid over time is required. To express the detection and identification of drugs, new methods are needed that must meet numerous requirements, not the least of which are selectivity, speed, the absence of false-negative results, and cost-effectiveness. The possibility of identifying anesthetics (sevoflurane) in lacrimal fluid has been studied using a new electrochemical method of multisensory inversion voltammetry in the electronic tongue and electronic nose format. The measurements were performed on a planar electrode, which is a three-electrode structure. The solution of the test system consisted of 0.05 M KCl, which contained the metal cations Zn2+, Cd2+, Pb2+, Co2+, and Hg2+ at a concentration of 5 × 10-5 M. It is shown that this method is effective for the determination of anesthetics, and the dynamics of changes in their concentration over time are examined. This study aimed to research the behavioral pharmacokinetics in the lacrimal fluid of the opioid drug sevoflurane in pediatric ophthalmology using multisensory stripping voltammetry in patients during strabismus correction surgery. The dynamics of changes in their concentrations over time were examined. After the instillation of the anesthetics in patients, their concentrations in the tear fluid remained unchanged within 10 min. The list of organic substances that can be determined by multisensory stripping voltammetry has been extended. The class of organic substances determined by the method of multisensory inversion voltammetry has been expanded.

Enhancing polarization retention in BiFeO3 domain wall nanodevices through controlled space charge redistribution

Ferroelectric thin films with binary switchable polarization offer promising applications in domain wall (DW) memory. However, achieving reliable polarization retention in size-reduced devices remains challenging. In this study, we present a planar ferroelectric BiFeO3 DW nanodevice demonstrating stable polarization retention through electrical cycling. By precisely controlling the device size, including the width and gap of planar Pt electrodes, we observed a back-switching process in switched polarization within 20 min, as characterized by ex-situ piezoresponse force microscopy (PFM). To overcome this issue, long-time alternating voltage pulse cycling effectively suppressed the back-switching behavior, leading to symmetrized polarization coercive voltages of the device. PFM characterization further confirmed the persistence of the artificially created DW between the electrode pair. This improved polarization retention was attributed to the migration of mobile charged defects, such as oxygen vacancies, at the domain boundary. The presence of these defects generated a local built-in field, which screened the net polarization induced by the charged DW. Upon erasing the DW, the local built-in field gradually dissipated during opposite voltage poling, resulting in restored poor polarization retention and asymmetric coercive voltage in the nanodevices. This work presents a promising approach to utilize defect redistribution for stabilizing the switched polarization in the development of high-density ferroelectric DW memory.

Low-cost, interdigitated capacitive sensor using laser-written graphene foam for touch, proximity, and liquid level detection

Flexible capacitive sensors are gaining popularity in place of sophisticated optical sensing or bulky mechanical designs for specific applications such as proximity/gesture detection and liquid level sensing. So, here, we propose Laser Induced Graphene Foam (LIGF) based planar capacitive sensors, which are flexible, highly sensitive, energy-efficient, and cost-effective, making them accessible for various applications. The working of these sensors involves the interdigitated planar electrode configuration and the fringing effect, influencing capacitance when the permittivity or the electric charge of the surrounding medium changes. LIGF planar capacitive elements were produced on a commercially availed polymer polyimide by using direct laser writing technique employing a low-cost diode laser. The developed LIGF-based planar capacitive touch sensor showed an average touch response (|ΔC/Co|) of more than 49%; moreover, when used for proximity sensing, this sensor could detect the presence of human hand up to a maximum distance of 170 mm from the sensor surface. An extended design of the sensor has demonstrated liquid level sensing with an accuracy of 0.97 mm. As a result of its ability to sense dielectric materials, contactless operation, long-range sensing, cost-effectiveness, low-power consumption, and environmental friendliness, the LIGF electrode-based capacitive sensor can be incorporated into a variety of modern technology and devices.

Dielectrophoretic profiling of erythrocytes to study the impacts of metabolic stress, temperature, and storage duration utilizing a point-and-planar microdevice

Dielectrophoresis (DEP) is widely utilized for trapping and sorting various types of cells, including live and dead cells and healthy and infected cells. This article focuses on the dielectric characterization of erythrocytes (red blood cells or RBCs) by quantifying DEP crossover frequency using a novel point-and-planar microwell device platform. Numerical simulations using COMSOL Multiphysics software demonstrate that the distribution of the DEP force is influenced by factors such as the shape of the point electrode, spacing between the point and planar electrodes, and the type of bioparticle being investigated. The dependency on electrode spacing is experimentally evaluated by analyzing the DEP crossover response of erythrocytes. Furthermore, the results are validated against the traditional electrical characterization technique called electrorotation, which typically requires laborious fabrication and operation using quadrupole electrodes. Other significant factors, including erythrocyte storage age and the changes in cell properties over time since collection, osmolarity, and temperature, are also assessed to determine the optimal conditions for erythrocyte characterization. The findings indicate a significant difference between fresh and stored erythrocyte samples (up to 4 days), highlighting the importance of maintaining an isotonic medium for cell storage.

Steady-state currents of planar interdigitated electrode arrays in shallow cells

Analytical equations for the steady-state current at shallow electrochemical cells with embedded interdigitated electrode (IDE) arrays were found by solving the diffusion equation in steady state using conformal transformations. These equations consider the cases where the IDE is used with an external counter electrode (four-electrode configuration) and where one of its arrays is used as internal counter electrode (three- and two-electrode configuration). Since the expressions for the current depend on Jacobian elliptic functions, we found approximations which depend only on trigonometric and hyperbolic functions which can ease the calculations at the expense of an error below 5%. Additionally, we provide expressions for steady-state voltammograms for the case of Nernstian (reversible) electrode reactions. The obtained theoretical results agree with theoretical and simulation results from the literature and with our own experiments. These results can be useful as criteria for designing electrochemical cells based on IDEs, and as benchmarks for assessing their performance, especially for polymer- or paper-based microfluidics.

Fabrication of nanofibrous PbO2 electrode embedded with Pt for decomposition of organic chelating agents

A new fabrication method of nanofibrous metal oxide electrode comprising Pt nanofiber (Pt–NF) covered with PbO2 on a Ti substrate was proposed. Pt–NF was obtained by performing sputtering deposition of Pt on the surface of electrospun poly(vinyl alcohol) (PVA) nanofiber on a Ti substrate, in which PVA was then removed by calcination (Ti/Pt–NF). Subsequently, by introducing PbO2 to the Ti/Pt–NF using the electrodeposition method, a nanofibrous Ti/Pt–NF/PbO2 electrode was finally obtained. Because the Ti substrate was covered by nanofibrous Pt, it had no environmental exposure and thus, was not oxidized during calcination. The crystal structure of the PbO2 mainly consisted of β-form rather than α-form; the β-form was suitable for electrochemical decomposition and remained stable even after 20 h of use. The nanofibrous Ti/Pt–NF/PbO2 electrodes showed 10% lower anode potential, 1.6 times higher current density at water decomposition potential, lower electrical resistance in the ion charge transfer resistance, and 2.27 times higher electrochemically active surface area than those of a planar-type Ti/Pt/PbO2 electrode, and demonstrated excellent electrochemical performance. As a result, compared with the planar electrode, the Ti/Pt–NF/PbO2 electrode showed more effective electrochemical decomposition toward nitrilotriacetic acid (80%) and ethylenediaminetetraacetic acid (83%), which are commonly used as chelating agents in nuclear decontamination.