Potential Scan Rate Research Articles

Effect of lanthanum, ce- rium, praseodymium on corrosion-electrochemical behavior of aluminum conductor alloy AlTi0.1 in NaCl electrolyte

The article presents the results of studying the effect of lanthanum, cerium and praseodymium additives (0–1.0 wt.%) as structure modifiers on the anodic behavior of the aluminum conductive alloy AlTi0.1 in the NaCl electrolyte medium. The studies were carried out using the potentiostatic method with a potential scan rate of 2 mV/s. It was found that over time, the free corrosion potential of the alloys shifts to the positive side and acquires a positive value with an increase in the modifier concentration (lanthanum, cerium, praseodymium) in the aluminum conductive alloy. The addition of lanthanum to the aluminum conductive alloy AlTi0.1 by 12–23%, cerium by 20–30% and praseodymium by 25–35% increases its corrosion resistance. An increase in the corrosion rate of the alloys with an increase in the NaCl concentration in the solution, regardless of their composition, was noted. An increase in the concentration of chloride ion in the NaCl electrolyte leads to a decrease in the potentials of free corrosion, repassivation and pitting of alloys.

Scan-Rate-Dependent Ion Current Rectification in Bipolar Interfacial Nanopores.

This study presents a theoretical investigation into the voltammetric behavior of bipolar interfacial nanopores due to the effect of potential scan rate (1-1000 V/s). Finite element method (FEM) is utilized to explore the current-voltage (I-V) properties of bipolar interfacial nanopores at different bulk salt concentrations. The results demonstrate a strong impact of the scan rate on the I-V response of bipolar interfacial nanopores, particularly at relatively low concentrations. Hysteresis loops are observed in bipolar interfacial nanopores under specific scan rates and potential ranges and divided by a cross-point potential that remains unaffected by the scan rate employed. This indicates that the current in bipolar interfacial nanopores is not just reliant on the bias potential that is imposed but also on the previous conditions within the nanopore, exhibiting history-dependent or memory effects. This scan-rate-dependent current-voltage response is found to be significantly influenced by the length of the nanopore (membrane thickness). Thicker membranes exhibit a more pronounced scan-rate-dependent phenomenon, as the mass transfer of ionic species is slower relative to the potential scan rate. Additionally, unlike conventional bipolar nanopores, the ion current passing through bipolar interfacial nanopores is minimally affected by the membrane thickness, making it easier to detect.

Electrochemical reduction behavior of PO43– ions in molten CaCl2

This work focuses on the electrochemical reduction behavior of PO43– ions in molten CaCl2 at 1123 K, aiming to develop a next-generation process for producing white phosphorus (P4) through electrolysis of dissolved PO43–. Results from cyclic voltammetry indicate a shift for the electrochemical reduction of PO43– from a reversible reaction to a quasi-reversible one as the potential scan rate increases. The detachment rate of P4 gas was found to be higher at the graphite electrode compared to Mo and W electrodes. The apparent diffusion coefficient of PO43–, determined from chronoamperometry and chronopotentiometry at a graphite electrode, ranges from 1.43 to 2.26 × 10–4 cm2 s–1. Additionally, an increase in the concentration of O2– was found to decrease the detachment rate of P4 gas, likely due to changes in the melt's physical properties. However, the increase in O2– up to 0.30 mol% does not significantly affect the diffusion of PO43–. This study provides valuable insights into the electrochemistry of PO43– in molten CaCl2 and offers a theoretical guidance for the technology development of P4 production through electrolysis.

Improving the electrochemical performance of nickel-cobalt organic framework by hybridizing with carbon quantum dots

To improve the electrochemical properties of nickel-cobalt metal-organic skeleton materials, two carbon quantum dots (CQDs), namely, CQD-CA and N-doped CQD-CAn, were prepared by using citric acid as carbon source and then introduced into NiCo-MOF to prepare CQDs/NiCo-MOF composites. Through the application of physical characterization and electrochemical analysis methods, such as SEM, TEM, XRD, XPS and BET, it was found that NiCo-MOF@CA and NiCo-MOF@CAn exhibited a nano thinner lamellar structure, higher specific surface area, larger pore structure, and excellent electron transport ability. Especially, by introducing CQDs, the charge could transfer from oxygen to Ni and Co, and there was some higher electron cloud density around active metals Ni and Co in NiCo-MOF@CAn than in NiCo-MOF, effectively activating the metal center Ni and Co. As the result, the specific capacitance of NiCo-MOF@CAn reached 1917.7 F·g−1 at the potential scan rate 5 mV·s−1, significantly higher than that of NiCo-MOF (1173.4 F·g−1) and NiCo-MOF@CA (1489.3 F·g−1). The method might provide an alternative strategy for modulating the morphology, porous structure and the partial electron structure of the target materials by introducing various CQDs.

Quantitative Interpretation of Potentiodynamic Polarization Curves Obtained at High Scan Rates in Scanning Electrochemical Cell Microscopy.

Scanning electrochemical cell microscopy is becoming the tool of choice for the investigation of localized metal corrosion. Typically, potentiodynamic polarization measurements in scanning electrochemical cell microscopy are performed at high potential scan rates. However, Tafel extrapolation applied to high-scan-rate potentiodynamic polarization curves would yield inaccurate corrosion kinetics due to the interference of double-layer charging current or mass transport of species in the metal oxide. Instead, the high field model was used to simulate the potentiodynamic polarization curves of pure aluminum at 25, 50, 100, and 200 mV/s in neutral and acidic phosphate solutions, thus enabling quantitative analysis of local corrosion kinetics by fitting the potentiodynamic polarization curve.

Performance evaluation of microbial fuel cells for bioelectricity generation: influence of potential scan-rate and real-time external load

AbstractThe electrochemical performance of microbial fuel cells is conventionally assessed through linear sweep voltammetry at predefined potential scan rates. Nevertheless, this approach frequently falls short in representing the long-term behavior of microbial fuel cells under actual external loads, highlighting the need for a standardized evaluation method incorporating both linear sweep voltammetry and external loads. To address this gap, this study evaluates the performance of single-chamber microbial fuel cells under different loads and scan rates. The MFCs were tested with external loads of 1200, 470, and 270 Ω, derived from maximum power points of polarization sweeps at scan rates of 0.1, 0.5, and 1 mV/s at two operational phases. Power estimates at these scan rates were 61.96, 87.88, and 166.68 mW/m2 at current densities of 116.5, 229.6, and 403 mA/m2, respectively. In the initial two hours, average power densities with 1200, 470, and 270 Ω were 73 ± 16.7, 36.3 ± 42, and 88.5 ± 120.1 mW/m2, respectively. Over the long term, the fuel cells under constant loading with resistance estimated at 0.1 mV/s showed average power 73.7% and 89.1% higher than those with resistances estimated at 0.5 mV/s and 1 mV/s, respectively, indicating that higher scan rates lead to overestimation of power. Although initially underestimated, the 0.1 mV/s scan rate more accurately reflected the true long-term performance of the fuel cells. This study emphasizes the importance of using appropriate scan rates for linear sweep voltammetry to obtain realistic long-term performance estimates of microbial fuel cells under real-time loads.

Gallium Nitride Electrodeposition at Indium Tin Oxide and Fluorine Tin Oxide Electrodes in Ammonium Nitrate and Gallium Nitrate Aqueous Solution

The potential of gallium nitride thin films in semiconductor technology and devices has garnered interest. This study aims to develop an effective GaN electrodeposition technique that will function on both Earth and microgravity situations and may be applied to any kind of needed application, such as in photovoltaic devices. To determine the optimal electrodeposition conditions, e.g. applied potential, cyclic voltammetry (CV) was done on a boron-doped diamond electrode at 0.01 mV/s potential scan rate and at 0.8 V vs. Ag/AgCl (Saturated KCl) constant applied potential. In the CV study, a well-defined peak formed at -1.75 V vs. Ag/AgCl (Saturated KCl). To start examining all the features of the electrodeposition of a thin film on Indium Tin Oxide (ITO) and Fluorine Tin Oxide (FTO) Electrodes, chronoamperometry (CA) measurements were done at different time scales, ranging from 3600s to 14400s and at a constant applied potential of -1.7 V vs. Ag/AgCl (Saturated KCl). The characterization methods used to examine the materials' topography, elemental contrast, crystal structure, and electrodeposition weight percentages included scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive spectroscopy (EDS). Longer electrodeposition times produced the best grain formation, promoting dendritic structure at the electrode surface. Furthermore, the optimal weight electrodeposition percentage of Ga and N was 10% and 35 % at 3600s, respectively, although the electrodeposited electrode surface was heterogeneous. The surface topographies at 3600s showed less grains definition and dendritic structures. At higher electrodeposition times, e.g. 14400s, more grain definitions and dendritic structures were found. For the 3600s electrodeposition time, XRD peaks were found at 33o, 37o and 46o, which are characteristics of GaN wurtzite structure according to literature.

Enhancing corrosion resistance of 316L stainless steel through electrochemical deposition of polyaniline coatings in acidic environments

Stainless steel is widely used because of its excellent corrosion resistance in typical environments. However, it is susceptible to corrosion in acidic media, therefore, to address this issue, the electrochemical deposition of polyaniline coatings on 316L stainless steel was investigated using cyclic voltammetry at different potential windows and scan rates. The successful polymerization and surface morphology were analyzed using Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM), respectively. Moreover, thermal stability of the PANI coating was assessed through thermo gravimetric analysis while the corrosion behavior of bare and coated steels immersed in 1M H2SO4 was studied using electrochemical impedance spectroscopy (EIS). Based on the Nyquist plots obtained from the EIS revealed that the corrosion resistance of the PANI coating improved significantly with a decrease in scan rate and by limiting the upper potential, especially during longer exposure times up to 72 h. Results suggest that controlling the deposition parameters and optimizing the electrochemical conditions can lead to even greater improvements in the corrosion resistance of the stainless steel. These findings offer valuable insights for researchers and engineers in the field of materials science and corrosion protection, enabling them to develop more precise and efficient strategies for enhancing the durability and performance of stainless steel in acidic environments.

Electrochemical sensor based on mesoporous g-C3N4/N-CNO/gold nanoparticles for measuring oxycodone

Oxycodone, often used as an analgesic, is a potent opioid. While its effectiveness has been proven in the control of moderate to acute pain, excessive use of oxycodone imposes heart failure, heart palpitations, reduction of red blood cells, bone pain, and even death. Therefore, monitoring the oxycodone concentration in blood is vital for emergency care. For this purpose, a novel electrochemical sensor was designed based on a glassy carbon electrode modified with mesoporous g-C3N4 (M-C3N4), carbon nano-onions doped with nitrogen (N-CNO), and gold nanoparticles. At first, the SEM and XRD techniques were employed to characterize prepared M-C3N4 and N-CNO samples. The electro-oxidation behavior of the oxycodone was evaluated by cyclic and differential pulse voltammetric methods. Based on the influence of the potential scanning rate and solution pH on the voltammetric response of oxycodone oxidation, a redox mechanism was proposed. A 16 nM detection limit was acquired for the oxycodone analysis with a linear response in the 0.05–150 µM range. This sensor showed a remarkable ability for oxycodone detection in plasma samples. The long-term stability, superior selectivity, and reproducibility of this sensor prove its ability to measure oxycodone accurately and precisely in authentic spices.

Tailoring a facile electronic and ionic pathway to boost the storage performance of Fe3O4 nanowires as negative electrode for supercapacitor application

Today, high-energy applications are devoted to boosting the storage performance of asymmetric supercapacitors. Importantly, boosting the storage performance of the negative electrodes is a crucial topic. Fe3O4-based active materials display a promising theoretical storage performance as a negative electrode. Thus, to get a high storage performance of Fe3O4, it must be tailored to have a higher ionic and electronic conductivity and outstanding stability. Functionalized graphite felt (GF) is an excellent candidate for tailoring Fe3O4 with a facile ionic and electronic pathway. However, the steps of the functionalization of GF are complex and time-consuming as well as the energy loss during this step. Thus, the in-situ functionalization of the GF surface throughout the synthesis of Fe3O4 active materials is proposed herein. Fe3O4 is electrodeposited at the in-situ functionalized GF surface with the crystalline nanowires-like structure as revealed from the various analyses; SEM, TEM, Mapping EDX, XPS, XRD, wettability test, and Raman analysis. Advantageously, the synthetic approach introduces full homogeneous and uniform coverage of the large surface area of the GF. Thus, Fe3O4 nanowires with high ionic and electronic conductivity are characterized by a higher storage performance. Interestingly, Fe3O4/GF possesses a high specific capacity of 1418 mC cm−2 at a potential scan rate of 10 mV s−1 and this value retained to 54% at a potential scan rate of 50 mV s−1 at an extended potential window of 1.45 V. Remarkably, the diffusion-controlled reaction is the main contributor of the storage of Fe3O4/GF electrode as revealed by the mechanistic studies.

Genuine differential voltammetry

A novel form of differential voltammetry is proposed, developed through the implicit anodic and cathodic current components of the experimentally accessible conventional net current measured in a voltammetric experiment. By employing basic mathematical modelling of an electrode reaction of a dissolved redox couple at a conventional, macroscopic electrode within the framework of the Butler-Volmer electrode kinetic model, the implicit anodic and cathodic current components of the net conventional current are clearly defined and can be estimated. Consequently, a novel form of differential current, calculated as the difference between anodic and cathodic implicit current components associated with a single potential of the voltammetric experiment, can be established. This differential current demonstrates remarkable characteristics in terms of electrode kinetics and analytical performance, particularly in cases involving fast, seemingly electrochemically reversible electrode processes. It holds promise to be analytically superior to the best-known differential voltammetric techniques so far (e.g., square-wave voltammetry), as well as provides a means for estimating the rate constants of very fast, apparently reversible electrode processes at macroscopic electrodes under mild experimental conditions (i.e., studied at slow potential scan rates). The practical implication of the novel methodology is significant: a simple linear sweep voltammogram of a quasi-reversible electrode reaction with unknown electrode kinetic parameters can be readily transformed into the novel type of differential voltammogram through a convolution procedure of the conventional net current, paving a new way for studying electrode processes by voltammetry.

Bridging Pharma and Sustainability: Green Electrochemical Analysis of Antiparkinsonian Drug in Pharmaceuticals and Plasma, Aligned with United Nations Goals via the NQS Index

This study presents a sustainable electrochemical investigation of pramipexole (PRA) in pharmaceuticals and human plasma, using cyclic and differential pulse voltammetry. Key parameters, including potential range, buffer pH, accumulation period, and scan rate were optimized, establishing efficient voltammetric methods for PRA analysis. The analytical range was 0.60–12.00 μg ml−1, with a detection limit of 0.14 μg ml−1 and a correlation coefficient of 0.9998. Recovery rates for PRA ranged from 98.60 ± 0.26% to 101.33 ± 0.38%, validating the methodology’s applicability in human plasma with an average recovery of 99.25 ± 0.45%. The study highlights the environmental sustainability of the developed voltammetric electrode, evaluated through SWOT analysis, and assesses the greenness impact using tools like Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical greenness (AGREE) and Analytical greenness for sample preparation (AGREEprep). Significantly, this work aligns with numerous United Nations Sustainable Development Goals (UN-SDGs), specifically goals 3, 4, 5, 7, 9, 11, 12, 13, 14, 15, and 17, illustrating our commitment to sustainable pharmaceutical research. The sustainability of the method was further quantified using the newly introduced Need, Quality, Sustainability (NQS) index, demonstrating significant alignment with sustainable analytical practices.

A Flexible Na‐Ion Supercapacitor/Battery Hybrid Device

AbstractA hybrid supercapacitor/battery device is proposed by integrating Na3V2(PO4)2F3 and multi‐walled carbon nanotubes as the battery electrode and carbon nanofiber as a supercapacitor electrode. The device made via the slurry casting of electrode material on foldable thin nickel foils leads to a robust, mechanically flexible sodium‐ion capacitor/battery (supercapattery) as a hybrid energy storage system. The device exhibits a specific capacitance of 136 F g−1 with a corresponding specific capacity of 95 C g−1 at a potential scan rate of 1 mV s−1, a maximum working voltage of 0.70 V, and a power density of 15 kW kg−1 at 2.50 Wh kg−1. Mechanical flexibility tests show practically unperturbed electrochemical properties at significant bending angles of up to 160°, indicating excellent robustness during large‐scale device deformation. The current study offers new avenues to develop energy storage systems for next‐generation portable and wearable energy storage devices that can be integrated into a variety of platforms.

Ferulic acid detection in honey using carbon paste electrode modified by C-C3N4/Li2CoMn3O8 nanocomposite

Honey is regarded as a valuable food commodity which has many and varied components, including phenolic compounds. Ferulic acid (FA) is one of these compounds, which possesses activities such as antioxidant, anti-inflammatory, anti-diabetic, haemolytic, antiviral, anti-cancer, etc. In view of these unique characteristics, a quick, sensitive, simple and inexpensive method for FA identification is required. This research developed a novel electrochemical sensor for measuring FA in honey samples. The sensor utilizes a C-C3N4/Li2CoMn3O8 nanocomposite modified carbon paste electrode (C-C3N4/LCMO/CPE) to enhance the sensitivity and detection. The synthesized nanocomposite exhibits remarkable properties, featuring an abundance of electrochemically active sites and enhanced electron transfer rates, making it ideal for developing advanced electrochemical sensors. The XRD, SEM and EDX analysis were used to examine and look like the synthesised nanocomposite structure. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods were used to evaluate the electrochemical behavior of C-C3N4/LCMO/CPE sensor for FA detection and optimized by adjusting pH, and potential scan rate. FA was measured in a phosphate buffered saline (PBS; 0.1 M, pH 4.0) by DPV with the detection limit of 3.6 nM and quantitative limit of 0.009 µM in the linear response ranges of 0.009–3.000 and 5.00–100 µM. Chronoamperometry was utilized to calculate the diffusion coefficient of FA (D = 3.45 (±0.11) × 10−6 cm2.s−1) on the surface of the C-C3N4/LCMO/CPE, as well as the electron transfer coefficient (α = 0.68). The sensor’s high sensitivity for accurately assessing FA in real samples was demonstrated by recovery values ranging from 96.96 to 102.36 %.

Gallium Nitride Electrodeposition at Indium Tin Oxide and Fluorine Tin Oxide Electrodes in Ammonium Nitrate and Gallium Nitrate Aqueous Solution

Gallium nitride thin films in semiconductor technology have garnered interest. This study aims to develop an effective GaN electrodeposition technique applicable where needed. To determine the optimal conditions, cyclic voltammetry (CV) was done on a boron-doped diamond electrode at 0.01 mV/s potential scan rate and at 0.8 V vs. Ag/AgCl (Saturated KCl) constant applied potential. In the CV study, a well-defined peak formed at -1.75 V vs. Ag/Ag/Cl (Saturated KCl). To start examining thin film features on Indium Tin Oxide (ITO) and Fluorine Tin Oxide (FTO) electrodes, chronoamperometry (CA) measurements were done at time scales ranging from 3600s to 14,000s and at a constant applied potential of -1.7 V vs. Ag/AgCl (Saturated KCl). The characterization methods used to examine the samples included SEM and EDS. The optimal weight electrodeposition percentages of Ga and N on ITO were 10.3% and 27.2% and 47.3% and 12.7% on FTO respectively.

Development of cobalt-carbon-based potentiometric phosphate sensors using cyclic voltammetry with potential scan rate variations

Phosphate sensor development is still needed because there are not many available in the field offering fast detection on environment, medicine, and agriculture. Herein, this study reported the potentiometric sensing of phosphate ions using a cobalt-carbon electrode. Cobalt was electrodeposited in the surface of carbon-producing cobalt-carbon electrodes using cyclic voltammetry at various scan-rate using Ag|AgCl as reference electrode and assisted by ionic strength adjustor 0.0025 M at pH 4. The electrode was characterized based on morphology and crystallinity. Then, the potentiometric sensing performance was evaluated using a Cobalt carbon electrode as a working electrode for phosphate ions in various concentrations. The results showed the homogeneous particle size observed at a scan rate of 5 mV/s. Besides, all the scan-rate variations produced an amorphous structure. The greatest potentiometric slope was −34.2 mV/decade on the electrode produced at a scan rate of 1 mV/s. The electrode reproducibility test produced the highest coefficient of variation value of 0.77 %.

Breaking boundaries in Electrochemistry: Unveiling a new dimensionless number to tackle convective transfer effect on the voltamperometric answer

This study introduces the Theokane number (Tk) as a groundbreaking dimensionless number in Electrochemistry. Tk enables the determination of the operating state of an electrochemical (EC) system—indicating whether it is in a transient state (characteristic of cyclic voltammetry) or a steady state (typical of linear sweep voltammetry)—based on a given combination of potential scan rate and residence time. It aims to bridge the gap between various voltamperometric methods. Tk uniquely compares the duration of the potential scan applied to an EC system to the residence time of the reaction mixture at the electrode. This comparison is pertinent in environments ranging from microfluidic setups to macroscale reactors, including stirred vessels.Tk is particularly crucial for understanding the ‘continuous answer’ of an EC system subjected to voltamperometric polarization across a spectrum of potential scan and stirring rates. Voltammograms recorded in a micro-reactor under varying conditions highlight the influence of operating parameters on EC responses. The approach introduced in this study accomplish three key objectives: i) it validates the Tk number through the comparison of experimental and simulation data, ii) it proposes a range for its applicability; and iii) it opens a new mode for analyzing EC responses. It is important to note that Tk is applicable to both quasi-reversible and irreversible systems.

Enhanced corrosion protection of the ionic liquid doped-polypyrrole/MWCNT composite coating on stainless steel

Composite coatings were deposited on type of 430 stainless steel (SS) by one-step electrochemical process by adding Tetra Butyl Phosphonium Bromide (TBPB) ionic liquid and Multi-Walled Carbon Nanotube (MWCNT) to the sulfuric acid-polypyrrole medium. The coating conditions were optimised by changing potential range, scan rate and number of cycles. The protectivity of all polypyrrole/TBPB and polypyrrole/TBPB-MWCNT composite coatings was investigated in NaCl (3.5%) and 0.5 M sulfuric acid solution. The composite electrode prepared in 0.02 M TBPB and 5.0 mg MWCNT medium was found to be the best protective coating. Electrochemical measurements were performed by using potentiodynamic polarization (PDP) and electrochemical-impedance-spectroscopy (EIS) techniques. Althougt the corrosion protection efficiency of the coating was higher than its initial value in both media during long-term immersion until 504 h, the steel coated with the polypyrrole/TBPB/MWCNT composite was represented more protective efficiency in H2SO4 compared to NaCl solution.

Cleaner extraction of white phosphorus from phosphate rock through molten salt electrolysis

White phosphorus (P4) is an essential raw material for the production of phosphorus chemicals. The conventional carbothermal reduction process used to extract P4 from phosphate rock is known as energy intensive and environmentally polluting, posing obstacles to meeting the urgent global demands for clean production and carbon neutrality. Moreover, the low product purity restricts its application in high-value industries. This paper presents an original approach that is both simple and coke-free for extracting high-purity P4. The method involves electrolyzing dissolved phosphate rock in molten CaCl2 at a mild temperature. We undertake an in-depth investigation into the dissolution behavior of phosphate rock in molten CaCl2 and the electrolysis behavior of the melt. The experiments demonstrate the rapid dissolution of phosphate in the rock when exposed to molten CaCl2, reaching saturation within a short time (e.g., within 10 min at 850 °C). The dissolution of phosphate shows a preference over silicates present in the phosphate rock. The electrochemical reduction of PO43− in molten CaCl2 is electrochemically reversible, as observed at potential scan rates not exceeding 0.20 V s−1. The obtained P4 product through electrolysis is of higher purity compared to the industrial-grade commercial product produced via carbothermal reduction. The implementation of pre-electrolysis can further improve the purity of the product and the current efficiency of the electrolysis process. The theoretical electricity and carbon consumption in the electrolysis method are estimated to be 9.12 kWh and 0.53 kg, respectively, for every 1 kg of P4 produced. These values are lower than the conventional carbothermal reduction process. This cutting-edge electrolysis method represents a paradigm shift towards a more sustainable development of the phosphorus chemical industry, thereby showcasing its potential for revolutionizing the field.

Corrosion Electrochemistry at Micro/Nano-Scale

A fundamental understanding of corrosion mechanisms is the key to developing suitable corrosion protection approaches for metallic structures and new corrosion resistant alloys for emerging technologies. However, corrosion testing methods such as mass loss and conventional electrochemical testing average over large areas and thus often mask the underlying mechanisms, due to either low sensitivity, low resolution, and/or a lack of element-resolved information. Recent advances in electron microscopy have led to development of liquid-cell transmission electron microscopy (LC-TEM) that allows in-situ monitoring of morphological and even compositional evolution in materials at high spatial resolution during interactions of surfaces with aqueous environments. However, electrochemical testing in such restricted volume with a very thin (~ 500 nm) electrolyte layer places stringent demands not only for a reference electrode, but also for a comprehensive understanding of the factors affecting electrochemical kinetics at the nano-scale1.In order to solve the need for a micro-reference electrode, we recently proposed the concept of metallic Luggin-Haber probe2. The metallic Luggin-Haber probe is a metal wire that serves as a bridge between the test solution and the reference electrode that was in a physically-distinct container. In standard-scale electrochemical cells, it was found that the metal bridge (MB) provides a means of making potential measurements that are identical to those made using a direct reference electrode or using a salt bridge.The MB is shown to be compatible with a wide range of electrochemical techniques including cyclic potentiodynamic polarization and electrochemical impedance spectroscopy. The present work explores the compatibility of the MB for electrochemistry in LC-TEM using Pt as working electrode. The work includes the effect of radiolysis of electrolyte, electrolyte flow rate, pH and potential scan rate on electrochemical kinetics when using LC-TEM, in a detailed comparison with results obtained using a standard-scale electrochemical cell. Present work is a discrete effort towards developing advanced methodologies for electrochemical measurement in situations involving restricted electrolyte volume including thin electrolyte layers, droplets, localized corrosion sites, batteries and fuel cells. References A. Kosari, H. Zandbergen, F. Tichelaar, P. Visser, H. Terryn, and A. Mol, Corrosion, 76, 4–17 (2020).S. Choudhary, K. Marusak, T. Eldred, and R. G. Kelly, J. Electrochem. Soc., 169, 111505 (2022).